CN115448292A - Insulating assembly, device for preparing fullerene and method for preparing fullerene - Google Patents

Insulating assembly, device for preparing fullerene and method for preparing fullerene Download PDF

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Publication number
CN115448292A
CN115448292A CN202211020117.7A CN202211020117A CN115448292A CN 115448292 A CN115448292 A CN 115448292A CN 202211020117 A CN202211020117 A CN 202211020117A CN 115448292 A CN115448292 A CN 115448292A
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China
Prior art keywords
sleeve
section
gasification furnace
fullerene
gas
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CN202211020117.7A
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Chinese (zh)
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纪崇甲
高树国
王兴立
姚文辉
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Beijing Three Arc Technology Co ltd
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Beijing Three Arc Technology Co ltd
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Priority to CN202211020117.7A priority Critical patent/CN115448292A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/152Fullerenes
    • C01B32/154Preparation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The application relates to an insulating assembly, a device for preparing fullerene and a method for preparing fullerene, wherein the insulating assembly is connected with a gasification furnace and comprises: the purging flange comprises a flange body and a gas channel, the gas channel is arranged in the flange body, and a gas inlet of the gas channel is arranged on the outer wall surface of the purging flange; the insulating sleeve is arranged between the purging flange and the gasification furnace, and the gas outlet of the gas channel is arranged on one side, facing the insulating sleeve, of the purging flange; the electrode sleeve can penetrate through the purging flange and the insulating sleeve and extend into the gasification furnace, and a gas outlet of the gas channel is provided with a purging channel from the gasification furnace. The technical scheme of this application has solved the problem of the insulation failure between electrode and gasifier among the prior art effectively.

Description

Insulating assembly, device for preparing fullerene and method for preparing fullerene
Technical Field
The application relates to the technical field of fullerene preparation, in particular to an insulation component, a device for preparing fullerene and a method for preparing fullerene.
Background
At present, with the development of the technology for preparing fullerene, a plurality of methods for preparing fullerene exist, and the arc discharge method is simple to operate and low in cost, so that the method is widely applied at present. The preparation of fullerene by the arc process is to synthesize carbon dust containing fullerene by consuming graphite rods through arc discharge by using two graphite rods as electrodes. Two different electrodes are insulated by an insulating material, and since the temperature in the synthesis furnace (gasification furnace) is high, a ceramic insulating material having high temperature resistance is generally used.
When fullerene is produced by the arc method, one electrode is connected to a synthesis furnace through an insulating member, parts having an insulating function are connected to the synthesis furnace so that the electrode is not electrically connected to the synthesis furnace, the other electrode is connected to the synthesis furnace, and a graphite rod as an electrode and the insulating member are both contained in the closed synthesis furnace. The prior art insulator can have the condition that the insulating property does not meet the requirement after being used for a period of time.
Disclosure of Invention
The application provides an insulating assembly, a device and a method for preparing fullerene, which are used for solving the problem of insulation failure between an electrode and a gasification furnace in the prior art.
In order to solve the above problem, the application provides an insulating assembly, and insulating assembly links to each other with the gasifier, and insulating assembly includes: the purging flange comprises a flange body and a gas channel, the gas channel is arranged in the flange body, and a gas inlet of the gas channel is arranged on the outer wall surface of the purging flange; the insulating sleeve is arranged between the purging flange and the gasification furnace, and the gas outlet of the gas channel is arranged on one side, facing the insulating sleeve, of the purging flange; wherein the electrode sleeve can pass through the purging flange and the insulating sleeve and extend into the gasification furnace, and a gas outlet of the gas channel has a purging channel from the gasification furnace.
Further, the flange body includes a first body section and a second body section, the inner diameters of the first body section and the second body section are the same, the outer diameter of the first body section is larger than the outer diameter of the second body section, and the gas outlet of the gas passage is disposed circumferentially outside the second body section.
Furthermore, the gas channel has a plurality of gas outlets which are arranged at the joint of the first body section and the second body section at intervals.
Further, insulating cover includes integrated into one piece's first sleeve section and second sleeve section, and the internal diameter of first sleeve section is greater than the internal diameter of second sleeve section, and the side of first sleeve section orientation sweeping flange links to each other with the side seal of first body section orientation insulating cover.
Further, a first gap is formed between the inner wall of the first sleeve section and the outer wall of the second body section, a second gap is formed between one side, facing the second body section, of the second sleeve section and the side face, facing the second sleeve section, of the second body section, a third gap is formed between the inner wall of the second sleeve section and the outer wall of the electrode sleeve, and the first gap, the second gap and the third gap form a purging channel.
Further, the width of the second gap is larger than or equal to the width of the first gap, and the width of the third gap is larger than the width of the second gap.
Further, the width of the first gap is between 2mm and 5mm, the width of the second gap is between 2mm and 7mm, and the width of the third gap is between 5mm and 10 mm.
Further, the circumferential outer side of the insulating sleeve has an annular groove.
Further, the insulating sleeve is made of insulating ceramic or polytetrafluoroethylene.
The application also provides a device for preparing fullerene, the device for preparing fullerene comprises a gasification furnace module and a fullerene recovery module, the fullerene recovery module is connected with the gasification furnace module, the gasification furnace module comprises an insulating component, and the insulating component is the insulating component.
The application also provides a method for preparing fullerene, which adopts the device for preparing fullerene, and the method comprises the following steps: and detecting the conductivity coefficient of the insulating sleeve.
Compared with the prior art, the technical scheme provided by the application has the following advantages:
according to the technical scheme, the gas channel is arranged in the flange body of the blowing flange, the gas outlet of the gas channel faces the insulating sleeve, so that attached substances such as carbon dust, carbon powder and fullerene on the insulating sleeve can be blown off, and the insulating property of the insulating sleeve is further guaranteed. The gas outlet of the gas channel is provided with a blowing channel to the gasification furnace, so that the attached substances can be blown into the gasification furnace, the waste of the substances is avoided, and the environment pollution is caused. The technical scheme of this application has solved the problem of the insulation failure between electrode and gasifier among the prior art effectively.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.
FIG. 1 shows a schematic view of the mounting structure of the insulation assembly of the present application;
FIG. 2 shows a schematic view of the internal structure of the insulation assembly of FIG. 1;
FIG. 3 illustrates a schematic internal structural view of a gasifier assembly of the present application;
FIG. 4 shows a schematic partial cross-sectional view of the sparge pipe and heat exchanger of the gasifier assembly of FIG. 3;
FIG. 5 shows a schematic view of the internal structure of the heat exchanger of the gasifier assembly of FIG. 3;
FIG. 6 shows an overall schematic structural view of the gasifier assembly of FIG. 3;
FIG. 7 illustrates a schematic view of a reducing configuration of the gasifier assembly of FIG. 3;
FIG. 8 is a schematic structural view of a sleeve of the reducing structure of FIG. 7;
fig. 9 shows a schematic structural view of a collection assembly of an apparatus for producing fullerenes of the present application;
FIG. 10 shows a schematic view of the construction of the filtering collection canister body of the collection assembly of FIG. 9;
fig. 11 shows a schematic flow chart of a fullerene processing method of the present application.
Wherein the figures include the following reference numerals:
10. a gasifier component; 11. a gasification furnace; 12. a heat exchanger; 13. a heat exchanger support; 14. an air blowing pipe; 141. an air blowing port; 15. a diameter-variable structure; 151. a connecting flange; 152. a sleeve; 153. pressing a sleeve; 16. a diffusion bin; 17. the electric arc generating device is connected with the flange; 20. an electrode assembly; 30. an insulating assembly; 31. blowing the flange; 311. a flange body; 3111. a first body section; 3112. a second body section; 312. a gas channel; 32. an insulating sleeve; 321. a first sleeve section; 322. a second sleeve section; 33. a purge channel; 331. a first gap; 332. a second gap; 333. a third gap; 40. a collection assembly; 41. a collection reservoir structure; 411. a collection storage tank; 412. a first valve; 413. a buffer tank; 414. a second valve; 42. a transfer transport structure; 421. a filtering and collecting tank body; 4211. filtering and collecting the tank body; 4212. a filter screen; 422. a spiral rolling brush; 423. transferring the tank body; 424. transferring the rolling brush; 43. a negative pressure suction port; 100. a first space; 200. a second space.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Usually only one or a few graphite rod electrodes can be installed at a time as consumable graphite rod electrodes. During the operation, carbon dust containing fullerene is synthesized, and since the synthesis furnace (gasification furnace) is sealed, the carbon dust adheres to the inner wall of the synthesis furnace, the surface of the insulating member, and the like. As graphite is a conductive material, carbon powder attached to each part in the synthetic furnace is continuously increased along with the continuous increase of carbon ash, and the carbon powder attached to the surface of an insulating part (an insulating sleeve) is also continuously increased, so that the insulation failure is caused, and the equipment cannot normally run. Because the efficiency of preparing fullerene by an electric arc method is low, only one or a plurality of graphite rods can be consumed each time, the quantity of generated carbon powder is not large, the insulation failure time can be properly slowed down by increasing the surface area of an insulating part, increasing the isolation of labyrinth insulation and the like, but the insulation failure condition can occur after the quantity of the carbon powder is increased. When the insulation fails, the synthesis furnace needs to be disassembled, the insulation part and the synthesis furnace inside are cleaned, and after the cleaning is finished, the synthesis furnace is sealed again, vacuumized, filled with inert gas and the like, and then normal synthesis work can be carried out. The process can be carried out only after the temperature in the synthesis furnace reaches the room temperature, so that a large amount of time is wasted, the production efficiency is reduced, and the production cost is increased.
As shown in fig. 1 and 2, the insulation assembly 30 of the present embodiment is connected to the gasification furnace 11. The insulation assembly 30 includes: a purge flange 31 and an insulating sleeve 32. The purge flange 31 includes a flange body 311 and a gas passage 312, the gas passage 312 is provided in the flange body 311, and a gas inlet of the gas passage 312 is provided in an outer wall surface of the purge flange 31. The insulating sleeve 32 is disposed between the purge flange 31 and the gasification furnace 11, and the gas outlet of the gas passage 312 is disposed on the side of the purge flange 31 facing the insulating sleeve 32. Wherein, the electrode sleeve can pass through the purging flange 31 and the insulating sleeve 32 and extend into the gasification furnace 11, and the gas outlet of the gas channel 312 to the gasification furnace 11 is provided with a purging channel 33.
According to the technical scheme of the embodiment, the gas channel 312 is arranged in the flange body 311 of the blowing flange 31, and the gas outlet of the gas channel 312 faces the insulating sleeve 32, so that substances attached to the insulating sleeve 32, such as carbon dust, carbon powder and fullerene, can be blown off, and the insulating performance of the insulating sleeve 32 is further ensured. The gas channel 312 has a purge channel 33 from the gas outlet to the gasification furnace 11, so that the adhered substances can be purged into the gasification furnace, thereby avoiding the waste of the substances and polluting the environment. The technical scheme of this application has solved the problem of the insulation failure between electrode and gasifier among the prior art effectively.
As shown in fig. 2, in the solution of the present embodiment, the flange body 311 includes a first body section 3111 and a second body section 3112, inner diameters of the first body section 3111 and the second body section 3112 are the same, an outer diameter of the first body section 3111 is larger than an outer diameter of the second body section 3112, and the gas outlet of the gas passage 312 is disposed at a circumferential outer side of the second body section 3112. The gas outlet that sets up gas channel 312 has been made things convenient for in setting up of second body section 3112, and in addition, the processing burden can also be reduced in the setting of first body section 3111 and second body section 3112, for example, only is higher to the machining precision of first body section 3111 towards one side of insulating cover 32, and need not improve holistic machining precision.
As shown in fig. 1 and 2, in the solution of the present embodiment, the gas outlet of the gas channel 312 is multiple, and the multiple gas outlets are arranged at the connection position of the first body section 3111 and the second body section 3112 at intervals. The arrangement of the plurality of air outlets improves the purging area of the gas channel 312, and further ensures the insulation effect of the insulation sleeve 32. It should be noted that, in the technical solution of this embodiment, the gas channel 312 is a gas inlet, and a plurality of gas outlets are uniformly arranged at intervals along the circumferential direction of the flange body 311. Parameters such as flow and pressure of the gas can be adjusted according to the requirement to meet the requirement of purging.
As shown in fig. 2, in the solution of this embodiment, the insulating sleeve 32 includes a first sleeve section 321 and a second sleeve section 322 that are integrally formed, an inner diameter of the first sleeve section 321 is larger than an inner diameter of the second sleeve section 322, and a side of the first sleeve section 321 facing the purge flange 31 is connected to a side of the first body section 3111 facing the insulating sleeve 32 in a sealing manner. A sealing ring is arranged between the side of the first sleeve section 321 facing the purging flange 31 and the side of the first body section 3111 facing the insulating sleeve 32, and the sealing performance of the insulating assembly 30 is ensured by the structure. It should be noted that, the first body section 3111 and the second body section 3112 are matched with the first sleeve section 321 and the second sleeve section 322, so that not only can sealing be well achieved, but also smooth purging can be achieved. The insulating assembly 30 can be monitored in real time by arranging a sensor, and the start and stop of the purging can be controlled according to the monitored condition, for example, the purging is started when the insulating property of the insulating sleeve 32 is lower than a set threshold, and the purging is stopped when the insulating property of the insulating sleeve 32 is higher than the set threshold, and the purged gas is inert gas. Of course, a real-time, uninterrupted purge may also be performed.
As shown in fig. 2, in the solution of the present embodiment, a first gap 331 is formed between an inner wall of the first sleeve section 321 and an outer wall of the second body section 3112, a second gap 332 is formed between a side of the second sleeve section 322 facing the second body section 3112 and a side of the second body section 3112 facing the second sleeve section 322, a third gap 333 is formed between an inner wall of the second sleeve section 322 and an outer wall of the electrode sleeve, and the first gap 331, the second gap 332 and the third gap 333 form the purge channel 33. The structure is compact and reasonable, and the adhesion and accumulation of substances such as carbon dust and the like are not easy to occur. The inner diameter of the first sleeve section 321 is greater than the outer diameter of the second body section 3112, and the first sleeve section 321 is located circumferentially outward of the second body section 3112.
As shown in fig. 2, in the solution of the present embodiment, the width of the second gap 332 is greater than or equal to the width of the first gap 331, and the width of the third gap 333 is greater than the width of the second gap 332. The purge passage 33 having the above structure is not easily clogged, for example, the width of the purge passage 33 from the start end to the end increases, and the substances adhered to the wall surface of the insulating sheath 32 and the wall surface of the electrode sleeve are more easily blown off. Specifically, the width of the first gap 331 is between 2mm and 5mm, the width of the second gap 332 is between 2mm and 7mm, and the width of the third gap 333 is between 5mm and 10 mm.
As shown in fig. 1 and 2, in the solution of the present embodiment, the circumferential outer side of the insulating sheath 32 has an annular groove. The provision of the annular groove on the one hand reduces the weight and on the other hand allows a certain elastic deformation of the insulating sleeve 32.
As shown in fig. 1 and 2, in the solution of the present embodiment, the material of the insulating sheath 32 is insulating ceramic. The insulating ceramic is a material of the insulating sheath 32, and is not easily adhered with substances such as carbon dust. As another example, the material of the insulating sheath 32 may be teflon.
The gas channel 312 further includes a gas inlet section, a gas buffer section and a gas outlet section which are sequentially communicated with each other, the gas buffer section is located in the purging flange 31, and both the cross-sectional area of the gas inlet section and the cross-sectional area of the gas outlet section are smaller than the cross-sectional area of the gas buffer section. The structure ensures that the purging airflow is relatively stable.
The application also provides a device for preparing fullerene. The device for preparing fullerene comprises a gasification furnace module and a fullerene recovery module, wherein the fullerene recovery module is connected with the gasification furnace module, the gasification furnace module comprises an insulation component 30, and the insulation component 30 is the insulation component 30. The insulating assembly 30 of the device gasifier module for preparing fullerene is not easy to fail in insulation.
As shown in fig. 3 to 8, the gasification furnace module of the present application includes: a gasifier assembly 10 and an electrode assembly 20. The gasification furnace assembly 10 includes a gasification furnace 11 and a heat exchanger 12, the heat exchanger 12 is disposed in the gasification furnace 11 and divides the gasification furnace 11 into a first space 100 and a second space 200, and a passage communicating the first space 100 and the second space 200 is provided between the heat exchanger 12 and the gasification furnace 11. The electrode assembly 20 is at least partially disposed within the first space 100.
By applying the technical scheme of the embodiment, the electrode assembly 20 reacts in the first space 100, and the product generated by the reaction is rapidly cooled by the heat exchanger 12, so that the yield of the product can be improved. The heat exchanger 12 divides the inner space of the gasification furnace 11 into a first space 100 and a second space 200, and the temperature in the second space 200 is lower than that in the first space 100, so that the generated product can be cooled rapidly, and the yield of the product can be improved. The technical scheme of the application has solved the slower problem of product cooling speed in the gasifier among the prior art effectively.
It should be noted that the cooling function of the heat exchanger 12 is not only in the second space 200, but also the heat exchange temperature of the first space 100 that is subjected to the heat exchanger 12 is rapidly decreased.
As shown in fig. 3, in the solution of the present embodiment, the heat exchanger 12 is a plate-shaped structure that is disposed obliquely, and the angle between the surface of the heat exchanger 12 facing the electrode assembly 20 and the axis of the gasification furnace 11 is α,0 ° < α < 90 °. The structure is beneficial to falling of products, carbon powder and other substances, namely the carbon powder and the products can be attached to the surface of the heat exchanger 12 when entering the second space 200 from the first space 100, and the carbon powder and the products can more easily enter the second space 200 under the action of gravity and purging through the obliquely arranged heat exchanger 12. More specifically, in the present embodiment, the angle α is set between 20 ° and 70 °, and the above structure is compact, and the landing effect and other comprehensive factors are good.
As shown in fig. 3 and 4, in the solution of the present embodiment, the heat exchanger 12 has a fluid channel, an inlet of the fluid channel is located at a low point of the heat exchanger 12, and an outlet of the fluid channel is located at a high point of the heat exchanger 12. The heat exchanger 12 has better heat exchange effect, for example, the low point of the heat exchanger 12 has lower temperature than the high point of the heat exchanger 12, and the fluid flows from the low point of the low temperature to the high point of the high temperature, so that the heat exchange efficiency is higher. Specifically, the fluid channels are in an S shape with the ends communicating with each other, and the structure further improves the heat exchange efficiency of the heat exchanger 12.
As shown in fig. 3 and 4, in the solution of the present embodiment, the gasification furnace assembly 10 further includes a heat exchanger support 13, the heat exchanger support 13 is disposed on the inner wall of the gasification furnace 11, and the heat exchanger 12 is supported on the heat exchanger support 13. The arrangement of the heat exchanger support 13 prevents the heat exchanger 12 from being directly fixed on the inner wall of the gasification furnace 11, and the heat exchanger 12 is directly fixed on the inner wall of the gasification furnace 11 to damage the overall structure, stress strain and the like of the gasification furnace 11. The inclination angle of the heat exchanger 12 can be adjusted by the up-and-down movement of the heat exchanger support 13, such a structure is easy to set, for example, the heat exchanger support 13 is connected with the inner wall of the gasification furnace through a fastener, and the angle adjustment of the heat exchanger 12 can be realized by adjusting different heights of the connection of the heat exchanger support 13 on one side of the heat exchanger 12 and the gasification furnace 11.
As shown in fig. 3 and 4, in the solution of the present embodiment, the gasifier assembly 10 further includes a gas blowing structure, and the gas blowing structure is located in the first space 100. The blowing structure can blow off the attachments on the heat exchanger 12, and the product (fullerene) and carbon powder are prevented from being accumulated on the heat exchanger 12 due to the arrangement of the blowing structure. Substances such as fullerene enter the second space 200 from the first space 100, and the blowing structure is positioned in the first space 100 to be more beneficial to blowing off the fullerene.
As shown in fig. 3 and 4, in the solution of this embodiment, the blowing structure includes a blowing pipe 14, and the blowing pipe 14 is disposed at the high side of the heat exchanger 12. The structure is convenient to set, the processing cost is low, and the purging effect is good. A gap is formed between the outer edge of the heat exchanger 12 and the inner wall of the gasification furnace 11, and substances such as fullerene enter the second space 200 from the surface of the first space 100 or the heat exchanger 12 under the action of actions such as purging, negative pressure, gravity and the like.
As shown in fig. 3 and 4, in the solution of this embodiment, the air blowing pipe 14 includes an air inlet and an air blowing opening 141, the air blowing opening 141 faces the surface of the heat exchanger 12, the angle between the air blowing opening 141 and the surface of the heat exchanger 12 is β, and β is greater than 0 ° and less than 90 °. The air blowing port 141 is angled with respect to the surface of the heat exchanger 12, which is more advantageous for blowing off substances such as fullerene. In the technical scheme of this embodiment, the value range of angle β is between 10 ° to 40 °, and such angle setting sweeps the area bigger, and the effort is bigger, and the effect that sweeps is better.
As shown in fig. 3 and 4, in the technical solution of this embodiment, the cross section of the gasification furnace 11 is circular, the heat exchanger 12 is elliptical, the gas blowing pipe 14 is arc-shaped and is adapted to the edge of the heat exchanger 12, and the gas blowing port 141 is disposed on the side facing the axis of the gasification furnace 11. The structure further ensures the purging area, and the purging of the gas blowing pipe 14 can fully cover the surface of the heat exchanger 12.
As shown in fig. 3, in the technical solution of the present embodiment, the distance between the center of the heat exchanger 12 and the graphite rod of the electrode assembly 20 is H, and H is greater than or equal to 30mm and less than or equal to 150mm. The selection of the distance integrates the factors such as the production rate of the product, the cooling effect, the space distance and the like, and ensures that the finished product rate of the fullerene is higher.
As shown in fig. 6 and 7, in the present embodiment, the side wall of the gasification furnace 11 has a cooling jacket, and the cooling jacket of the gasification furnace 11 has a cooling medium inlet and a cooling medium outlet. The cooling jacket is more favorable for realizing rapid cooling, thereby ensuring that the finished product rate of the fullerene is higher.
As shown in fig. 7 and 8, in the technical solution of this embodiment, the gasification furnace assembly 10 further includes a reducing structure 15, the reducing structure 15 is disposed at the discharge port of the gasification furnace 11, an inner wall of the reducing structure 15 and an inner wall of the discharge port of the gasification furnace 11 are in smooth transition, and an inner diameter of the reducing structure 15 includes a contraction section, a stationary section and an expansion section disposed in a direction from the entrance to the exit. The arrangement of the reducing structure 15 is more beneficial to the substances such as fullerene, carbon powder and the like to enter the diffusion bin 16 from the gasification furnace 11 under the action of negative pressure, gravity and the like. The arrangement of the contraction section enables the air flow to be enhanced at the position of the reducing structure 15, so that the acting force on fullerene, carbon powder and the like can be enhanced, and further the fullerene and the carbon powder can be favorably separated from the gasification furnace 11.
As shown in fig. 7, in the technical solution of this embodiment, the bottom of the gasification furnace 11 is a tapered section that gradually shrinks, and the diameter of the large opening of the tapered section is the same as that of the outlet of the tapered section. The transition of 11 inner structure of gasifier has been guaranteed to above-mentioned structure, has avoided the inside of gasifier 11 to appear structures such as step, and the step structure can cause piling up of materials such as fullerene and carbon dust, and smooth transition has all been adopted to the inside and matched with structure of the gasifier 11 of the technical scheme of this embodiment, is difficult for causing piling up of fullerene and carbon dust.
As shown in fig. 7 and fig. 8, in the solution of the present embodiment, the reducing structure 15 includes a connecting flange 151, a sleeve 152, and a sleeve pressing block 153, the connecting flange 151 is detachably connected to the gasification furnace 11, the connecting flange 151 is at least partially embedded in the gasification furnace 11, the sleeve 152 is embedded in the connecting flange 151, and the sleeve pressing block 153 is connected to the connecting flange 151 and fixes the sleeve 152 in the connecting flange 151. The structure is convenient to disassemble and assemble and convenient to maintain. In addition, the arrangement of the reducing structure 15 can be adjusted according to the requirement, for example, the inner diameter d of the stable section can be adjusted according to the requirement by selecting a proper sleeve 152.
As shown in fig. 7 and 8, in the technical solution of this embodiment, the bottom of the gasification furnace 11 has a cylindrical section to form a discharge port of the gasification furnace 11, the connection flange 151 includes a connection section, a flange plate section and an installation section, the connection section protrudes from a first side of the flange plate section, the installation section protrudes from a second side of the flange plate section, an outer wall of the connection section is adapted to an inner wall of the discharge port of the gasification furnace 11, an inner wall of the connection section has the same inclination angle as an inner wall of the tapered section, an inner wall of the installation section is cylindrical, an outer wall of the sleeve 152 has a step, an outer diameter of a side of the sleeve 152 close to the gasification furnace 11 is larger than an outer diameter of a side of the sleeve 152 far away from the gasification furnace 11, the sleeve 152 includes a first sleeve section, a second sleeve section and a third sleeve section, an inner diameter of the first sleeve section gradually shrinks, an inner diameter of the second sleeve section is the same, an inner diameter of the third sleeve section gradually enlarges, an inclination angle of the inner wall of the first sleeve section is the same as the inclination angle of the inner wall of the connection section and is adjacent to the connection section. As can be seen from the above, the small holes in the technical solution of the present embodiment have a large pressure difference, which is beneficial to the rapid diffusion of carbon powder, fullerene and other substances, and the inert gas is supplemented through the gas inlet of the plasma of the electrode assembly 20; the conicity of the contraction section and the expansion section of the embodiment is between 30 degrees and 60 degrees, the smaller the conicity is, the smaller the resistance is, and if a plane is generated, the falling of substances such as fullerene is not facilitated.
As shown in fig. 6, in the technical solution of this embodiment, the gasification furnace module further includes a diffusion bin 16, the diffusion bin 16 is connected to the connection flange 151, the volume of the diffusion bin 16 is 60 times to 130 times of the volume of the gasification furnace 11, and the diameter of the inlet of the diffusion bin 16 is 6 times to 28 times of the diameter of the outlet of the reducing structure 15. The diffusion chamber 16 is arranged to quickly reduce the speed of the fullerene and other substances passing through the reducing structure 15, and the wall surface of the diffusion chamber 16 is provided with a cooling jacket, so that the fullerene and other substances can be ensured to have enough cooling time in the diffusion chamber 16.
As shown in fig. 6, in the solution of the present embodiment, the wall surface of the diffusion chamber 16 has a cooling channel. The wall surface of the diffusion bin 16 is set to be a jacket structure, so that the cooling effect of the diffusion bin 16 is ensured, and the diffusion bin 16 has no blocking structure or a structure which is easy to attach fullerene. Specifically, the diffusion bin 16 is further provided with a purging structure, and an outlet of the purging structure is arranged on the inner wall surface of the diffusion bin 16. This allows the fullerene adhering to the wall surface of the diffusion chamber 16 to be blown out. The diffusion chamber 16 comprises two sections: the upper diffusion bin and the lower diffusion bin are connected through flanges, the upper diffusion bin and the lower diffusion bin are both provided with cooling jackets, and the cooling jackets of the upper diffusion bin and the lower diffusion bin are independent respectively.
The following is detailed in terms of experimental conditions:
experiment one: the apparatus was operated without installing a quenching device (heat exchanger 12). And adjusting the parameters of the arc generating device, setting the current to be 300A, setting the voltage to be 70V and setting the running power of the equipment to be about 21KW. Run time 1 hour. And opening a vacuum pump to vacuumize the gasification furnace 11, introducing inert gas, and operating an arc generation device to synthesize fullerene. And after the equipment stops running, collecting the produced carbon dust for analysis, wherein the comprehensive yield of the fullerene in the carbon dust is 3.4%.
Experiment two: a quenching device is installed in a gasification furnace, the height H of the quenching device in the gasification furnace is adjusted to be 50mm, and the axial angle alpha between the quenching device and an arc generating device (the upper part of the gasification furnace) is 45 degrees. And meanwhile, the periphery of the quenching device is adjusted to form a uniform gap with the inner wall of the gasification furnace. And a cooling pipeline arranged in the gasification furnace is respectively connected with a cooling water inlet and a cooling water outlet arranged on the quenching device, so that the quenching device is introduced with cooling water. And after the installation is finished, sealing the gasification furnace. Adjusting the parameters of the arc generating device, setting the current to be 300A, the voltage to be 70V and the equipment running power to be about 21KW, and synthesizing the fullerene under the same conditions. The run time was 1 hour. And opening a vacuum pump to vacuumize the gasification furnace, introducing inert gas, and operating an electric arc generating device to synthesize fullerene. In the operation process, the quenching device is observed through the observation window, after moving to the surface of the quenching device, some carbon powder enters the cooling area (the second space 200) along with the airflow, some carbon powder can be attached to the surface of the quenching device, and the carbon powder attached to the surface of the quenching device is continuously increased along with the increase of the generated carbon powder. And after the equipment stops running, collecting the generated carbon dust for analysis, wherein the comprehensive yield of the fullerene in the carbon dust is 6.2%. After several repeated experiments under the same conditions, the yield of the fullerene does not greatly fluctuate by about 0.5%.
Experiment three: a quenching device is installed in the gasification furnace, the height H of the quenching device in the gasification furnace 1 is adjusted to be 50mm, and the axial angle alpha between the quenching device and the arc generating device is 45 degrees. And meanwhile, the periphery of the quenching device is adjusted to form a uniform gap with the inner wall of the gasification furnace. And a cooling pipeline arranged in the gasification furnace is respectively connected with a cooling water inlet and a cooling water outlet arranged on the quenching device, so that the quenching device is introduced with cooling water. And a cold air purging device is installed and connected with an air inlet arranged on the cold air purging device through a gas pipeline. And after the installation is finished, sealing the gasification furnace. The parameters of the whole arc generating device are that the current is set to be 300A, the voltage is 70V, the equipment running power is about 21KW, and the fullerene is synthesized under the same conditions. The run time was 1 hour. And opening a vacuum pump to vacuumize the gasification furnace, introducing inert gas, and operating an electric arc generating device to synthesize fullerene. During synthesis, a valve loaded on a pipeline of the cold air purging device is opened, so that the cold air purging device is filled with gas. The gas is blown to the surface of the quenching device through a plurality of blowing holes which are arranged on the cold gas blowing device and form an angle beta with the quenching device. In the operation process, the quenching device is observed through the observation window, along with the work of the cold air blowing device, carbon powder rapidly enters a cooling area on the surface of the quenching device along with air flow, a small amount of carbon dust can be attached to the edge of the quenching device, and along with the operation of equipment, the attached carbon dust is not obviously increased. And after the equipment stops running, collecting the generated carbon dust for analysis, wherein the comprehensive yield of the fullerene in the obtained carbon dust is 8.3%. After several repeated experiments under the same conditions, the yield of the fullerene does not change greatly.
As demonstrated by the above examples, the cooling effect is increased after the addition of the quenching device, and a part of the soot enters the cooling zone. And a part of the carbon powder is attached to the surface of the quenching device and stays in the high-temperature area, and the fullerene in the carbon powder has secondary reaction in the high-temperature environment. The fullerene in the carbon powder entering the cooling area is preserved. So that the fullerene content in the carbon dust is increased to a certain extent. After the quenching device and the cold air blowing device are simultaneously installed, the carbon dust which is rapidly cooled quickly leaves the high-temperature area and enters the cooling area, and most of fullerene in the carbon dust is stored. Thus, the yield of the fullerene is improved.
Fig. 6 is an assembly diagram of a gasification furnace, which mainly includes a lower conical section (lower diffusion chamber) of the diffusion cooling chamber, an upper section (upper diffusion chamber) of the diffusion cooling chamber, the gasification furnace 11, a carbon rod guide structure of the electrode assembly 20, a reducing air-extracting block (sleeve 152), a reducing block pressing cover (sleeve pressing block 153), a vacuum valve, and the like. The diffusion cooling bin consists of a lower conical section of the diffusion cooling bin and an upper section of the diffusion cooling bin, and the middle of the diffusion cooling bin is connected through a flange. The diffusion cooling bin lower cone section and the diffusion cooling bin upper section are of double-layer structures, and a plurality of cooling water inlets and cooling water outlets are formed in the diffusion cooling bin lower cone section and the diffusion cooling bin upper section and used for introducing cooling water into the interlayer. The lower conical section of the diffusion cooling bin is connected with a vacuum valve so as to be connected with equipment such as a vacuum pump. The top flange of the upper section of the diffusion cooling bin is connected with the gasification gasifier, so that the gasification gasifier and the diffusion cooling bin are integrated. The gasification furnace has a double-layer structure and is provided with a plurality of cooling water inlets and outlets (not shown in the figure) for introducing cooling water into the interlayer. The top of the gasification furnace is provided with an electric arc generating device connecting flange 17 for connecting an electric arc generating device. The gasifier is provided with carbon-point guide structure and is used for installing the graphite rod. The gasification furnace is provided with an observation window for observing the synthesis condition in the gasification furnace. Vacuum pressure detection ports are arranged on the gasification furnace and the diffusion cooling bin (the diffusion bin 16) and are respectively used for connecting a pressure sensor of the diffusion cooling bin and a pressure sensor of the gasification furnace. The lower end equipment of the gasification furnace is provided with a reducing air pumping block which is fixed on the gasification furnace through a reducing block gland. The reducing air extraction block is provided with a small hole with the diameter of d, and the gasification furnace and the diffusion cooling bin are separated into two spaces through the reducing air extraction block. The space volume of the gasification furnace is relatively small, and the sum of the internal space volume of the diffusion cooling bin (diffusion bin 16) and the internal space of other accessory equipment is about 100 times of the internal space of the gasification furnace. The inner diameter of the upper diffusion bin is about 1000 mm.
Before the equipment runs, the electric arc generating device is arranged at the connecting flange 17 of the electric arc generating device, a graphite rod guide rod connecting flange arranged on the gasification furnace is connected with an upper carbon rod guide device (carbon rod guide structure) and a transmission mechanism of a graphite rod, and the graphite rod is arranged. And the vacuum valve connected with the air exhaust connecting flange at the lower end of the diffusion cooling bin is connected to a vacuum pump through a vacuum pipeline so as to filter the collecting device.
When the equipment is operated, the graphite rods are gasified by the electric arc generating device in the gasification furnace to synthesize carbon dust containing fullerene, and the carbon dust enters the diffusion cooling bin through the small holes arranged on the reducing air extraction block to be cooled. Because the space of the gasification furnace is smaller than the volume in the diffusion cooling bin, the data detected by the pressure sensor of the diffusion cooling bin and the pressure sensor of the gasification furnace shows that the pressure in the gasification furnace is higher than the pressure in the diffusion cooling bin, so that the airflow containing carbon powder in the gasification furnace can quickly enter the diffusion cooling bin. The diffusion cooling bin is isolated from the gasification furnace through the reducing air pumping block, and a high-temperature region taking the electric arc as the center cannot enter the diffusion cooling bin, so that the cooling effect in the diffusion cooling bin is ensured. The interior of the diffusion cooling bin is in a vacuum state, and the pressure is lower than the pressure in the gasification furnace. After the gas containing the carbon dust enters the diffusion cooling bin, the gas can be rapidly diffused for cooling. This provides an effect of accelerating the rapid exit of the toner and rapid cooling, thereby better preserving the fullerene after the formation. The diameter of the middle hole of the variable diameter air extraction block is increased by adjusting the pressure in the gasification furnace and the pressure in the diffusion cooling bin, so that the resistance of the middle hole to the carbon powder is reduced while the pressure difference of two spaces exists. Wherein, the diameter of the middle hole of the reducing air extraction block 5 is more than 5mm.
As shown in fig. 10 and 11, the apparatus for producing fullerene according to the present embodiment includes: a gasifier assembly 10 and a collection assembly 40. The gasifier component 10 has a discharge port and a gas replenishment port. The collection assembly 40 includes a collection tank structure 41 and a transfer structure 42, the transfer structure 42 is communicated between the gasifier assembly 10 and the collection tank structure 41, and the transfer structure 42 has a negative pressure suction interface.
The technical scheme of this embodiment, produce the product in the gasifier subassembly 10, collect subassembly 40 through the mechanical structure of transporting transport structure 42, the effort and the gravity etc. of negative pressure, collect foretell product in collecting storage tank structure 41, avoided cleaning through the manual work adoption brush like this, scrape, shovel etc. the method collects the product that generates, manpower and materials have been saved to above-mentioned structure, have improved work efficiency, avoid the harm to operation personnel and environment. The technical scheme of the embodiment effectively solves the problems that the preparation of fullerene in the prior art wastes time and labor during collection and pollutes the environment.
The gas replenishment port is filled with an inert gas.
As shown in fig. 10, in the technical solution of this embodiment, the transferring and conveying structure 42 includes a filtering and collecting tank 421 and a spiral rolling brush 422, the filtering and collecting tank 421 is a cylindrical structure, the spiral rolling brush 422 is installed on the filtering and collecting tank 421 through a first end of the filtering and collecting tank 421, and a second end of the filtering and collecting tank 421 is communicated with the collecting tank structure 41. The separation of gas and product can be realized well to the collection jar body 421 of filtering, and material such as adnexed product can be swept away in spiral round brush 422's setting, and then has guaranteed the collection of material such as carbon dust, carbon dust and fullerene.
As shown in fig. 10 and fig. 11, in the technical solution of this embodiment, the filtration collection tank 421 includes a filtration collection tank body 4211 and a filter screen 4212, the filter screen 4212 is disposed on a side wall of the filtration collection tank body 4211, the negative pressure suction port 43 is located on the side wall of the filtration collection tank body 4211, the length of the spiral rolling brush 422 is greater than the length of the filter screen 4212, and the negative pressure suction port 43 is located on a side of the filter screen 4212 away from the spiral rolling brush 422. The structure is easy to sweep off substances such as carbon dust, carbon powder and fullerene attached to the filter screen. It should be noted that the mesh number of the filter screen 4212 is smaller than the diameter of the product particles, and the filter screen 4212 is convenient to set and is beneficial to separating the product particles. It should be noted that the negative pressure suction port is provided with a valve.
As shown in fig. 10, in the technical solution of this embodiment, the sidewall of the filtering and collecting tank 421 is further provided with a first blowing opening, and the first blowing opening is located on one side of the filter screen far away from the spiral rolling brush 422. The structure further ensures the separation of products, and is beneficial to blowing off the products attached to the filter screen 4212 and the filtering and collecting tank body 4211. It should be noted that the first purge port is provided with a valve.
As shown in fig. 10, in the technical solution of this embodiment, the spiral rolling brush 422 includes a first motor, a first rolling shaft, and a first rolling brush, the first motor is installed on the filtration and collection tank 421, an output shaft of the first motor is connected to the first rolling brush, the first rolling brush is spirally disposed on an outer side of the first rolling shaft in a circumferential direction, and an end of the first rolling brush cleans a side wall of the filtration and collection tank 421. The structure has lower processing cost and convenient operation. It should be noted that the length of the filter screen 4212 refers to the length along the axial direction of the filtration collection tank 421, and the filter screen 4212 forms a part of the side wall of the partial filtration collection tank 421. In this embodiment, the filtering and collecting tank 421 is vertically disposed.
As shown in fig. 10, in the technical solution of this embodiment, the transferring and conveying structure 42 further includes a transferring tank 423 and a transferring roller brush 424, the transferring tank 423 is connected between the filtering and collecting tank 421 and the collecting assembly 40, and the transferring roller brush 424 is disposed on the transferring tank 423 to clean the inner wall of the transferring tank 423. The transfer conveyor structure 42 facilitates the positioning of the collection tank 411, such as for space issues, height issues, etc.
As shown in fig. 10, in the technical solution of this embodiment, the transfer tank 423 has a cylindrical structure, the transfer brush 424 is mounted on the transfer tank 423 through the first end of the transfer tank 423, the inlet of the transfer tank 423 and the outlet of the transfer tank 423 are both disposed on the side wall of the transfer tank 423, the inlet of the transfer tank 423 is close to the first end of the transfer tank 423, and the outlet of the transfer tank 423 is close to the second end of the transfer tank 423. Therefore, the products can be guaranteed to move and be collected according to the preset track as much as possible.
As shown in fig. 10, in the technical solution of this embodiment, the transfer roller 424 includes a second motor, a second roller and a second roller, the second motor is installed on the transfer tank 423, an output shaft of the second motor is connected to the second roller, the second roller is spirally disposed on the outer side of the second roller in the circumferential direction, and an end of the second roller cleans the side wall of the transfer tank 423. The structure has the advantages of low processing cost and convenient operation. It should be noted that the axis of the spiral rolling brush 422 is vertically arranged, the axis of the transfer rolling brush 424 is horizontally arranged, the brush of the spiral rolling brush 422 and the brush of the transfer rolling brush 424 are both spirally arranged, and the spiral direction is to push the products and other substances to move towards the outlet direction when cleaning.
As shown in fig. 10, in the solution of the present embodiment, the collecting tank structure 41 includes a collecting tank 411 and a first valve 412, and the collecting tank 411 is connected to the transferring and transporting structure 42 through the first valve 412. The first valve 412 is arranged to cut off the communication, and the structure has two collecting methods, so that the collecting tank 411 can be removed after the collection; alternatively, the valve and the collecting tank 411 may be transferred together after the collection is completed, so that the substance in the collecting tank 411 does not escape to the outside of the collecting tank 411, and the external substance does not enter the collecting tank 411 to contaminate the substance in the collecting tank 411.
As shown in fig. 10, in the technical solution of this embodiment, the collecting storage tank structure 41 further includes a buffer tank 413 and a second valve 414, the buffer tank 413 is a cylindrical structure, a first end of the buffer tank 413 is connected to the first valve 412, and a second end of the buffer tank 413 is connected to the transferring and transporting structure 42 through the second valve 414. The above structure can realize the function of buffer collection, for example, when the collection tank 411 finishes collecting and there is product, the buffer tank 413 can perform temporary collection. The buffer tank 413 is provided with a purge port, and the purge port is provided with a valve.
As can be seen from fig. 10, one end of the air inlet valve is connected to the filtering and collecting tank 421, and the other end of the air inlet valve is connected to the gasification furnace through a pipeline. One end of the air outlet valve is connected with the filtering and collecting tank 421, and the other end of the air outlet valve (the negative pressure suction port 43) is connected with a vacuum pump through a pipeline to perform air suction. Through the pumping of the vacuum pump, the carbon dust with the fullerene in the gasification furnace enters the filtering and collecting tank body through the air inlet valve along with the flowing of the gas, and the gas is discharged from the air outlet valve after entering the vacuum pump through the pipeline after passing through the filter screen. Wherein, the filtering precision of the filter screen is less than 1 μm, and the material of the filter screen is nickel-chromium alloy or titanium alloy, and can also be other filtering materials. The remaining carbon dust remains on the inner walls of the filter screen and the filter collection tank 421. The magnetic fluid is driven by the first motor to drive the spiral rolling brush (the first rolling brush) to rotate in a sealing transmission mode, carbon dust attached to the inner wall of the filtering and collecting tank body and the filter screen is cleaned, and the cleaned carbon dust falls into the transferring and conveying structure 42. Through the transport spiral round brush (second round brush) in carbon powder transport mechanism (transport structure 42), transport carbon powder buffer storage jar (buffer tank 413) to the carbon powder, through vacuum valve B (first valve 412), the carbon powder falls into carbon powder storage jar (collection storage tank 411). During operation, the direction of gas flow is in the direction of the arrows. During operation, both vacuum valve A (second valve 414) and vacuum valve B (first valve 412) are open so that toner falls into the toner reservoir. The filter screen is installed in filtering the collection tank body, seals through the sealing washer, prevents that the carbon dust from entering into in the exhaust duct through the filter core. The inlet and the outlet of the filtering and collecting tank body are provided with vacuum pressure detection interfaces, and the blocking degree of the filter screen and the amount of carbon powder in the gas are detected through the pressure difference between the gas outlet pressure sensor and the gas inlet pressure sensor which are arranged on the filtering and collecting tank body. After the pressure difference is greater than the set value, open a plurality of admission valves of setting on filtering the collection jar body, let in inert gas and clear up the filter screen. The vacuum valve a of the inlet valve needs to be closed before the inlet valve is opened. The gas inlet valve is closed to prevent the carbon dust from returning to the gasification furnace through gas flow and entering the high-temperature reaction area, so that the produced fullerene can carry out secondary reaction, and the yield is reduced. And closing the vacuum valve A to prevent the carbon dust in the buffer storage tank and the carbon powder storage tank from entering the filtering and collecting tank body again.
Since the filtering and collecting processes are performed in a vacuum negative pressure environment, the sealing performance of the device needs to be ensured, and meanwhile, the inert gas atmosphere in the sealed environment cannot be destroyed. There are two methods for collecting and transporting the collected carbon powder without destroying the inert gas atmosphere:
the method comprises the following steps: when the carbon dust in the carbon dust storage tank needs to be transferred after reaching a certain amount, the vacuum valve B is closed, and the carbon dust is transferred through the carbon dust transfer mechanismThe carbon dust can fall into the buffer storage tank, and can not continuously enter the carbon powder storage tank through the carbon powder buffer storage tank. The inert gas is filled into the carbon powder storage tank to normal pressure through an inert gas inlet arranged on the carbon powder storage tank, the carbon powder storage tank is disassembled after carbon ash in the carbon powder storage tank is stable for a period of time, an outlet of the carbon powder storage tank is rapidly sealed, and the carbon powder storage tank filled with the carbon powder is transferred away after the sealing is finished. While a toner storage tank without toner is installed. After the installation is finished, the vacuum valve K2 is connected with a vacuum pump to vacuumize the carbon powder storage tank, and when the pressure in the carbon powder storage tank is less than 1 multiplied by 10 -3 And after Pa, stopping air extraction. And filling inert gas into the carbon powder storage tank through an inert gas inlet arranged on the carbon powder storage tank, and stopping filling gas when the pressure value is consistent with the pressure sensor of the gas inlet. And opening the vacuum valve B, so that the carbon dust in the buffer storage tank can fall into the carbon powder storage tank.
The second method comprises the following steps: when carbon dust in the carbon dust storage tank reaches the time of just needing to shift away after a certain amount, at this moment close vacuum valve A, the carbon dust of transferring through carbon dust transport mechanism will fall into with carbon dust transport mechanism and vacuum valve A middle pipeline in, can not continue to enter into in the carbon dust storage tank through the buffer storage tank. And closing the vacuum valve B, filling inert gas into the buffer storage tank to normal pressure through an inert gas inlet arranged on the buffer storage tank, detaching the joint between the buffer storage tank and the vacuum valve B after the carbon ash in the buffer storage tank is stable for a period of time, connecting the carbon powder storage tank with the vacuum valve B, and enabling the vacuum valve B to be in a closed state. In the process of disassembly, a dust suction device needs to be installed to quickly suck away carbon powder floating out of the pipeline, so that the injury to personnel is prevented. Keeping the vacuum state in the carbon powder storage tank, and transporting away the carbon powder storage tank filled with the carbon powder and the vacuum valve B in a closed state. Therefore, the negative pressure transfer of the collected carbon powder is realized, and the carbon powder is prevented from flying out to cause harm to human bodies and the environment while the carbon powder is prevented from contacting with air. When the carbon powder is transferred, a carbon powder storage tank without carbon powder and a vacuum valve B are arranged. After the installation is finished, vacuumThe valve B is in an open state, and is connected with a vacuum pump through a vacuum valve K1 arranged on the buffer storage tank to vacuumize the carbon powder storage tank and the buffer storage tank, and when the vacuum pressure in the carbon powder storage tank and the buffer storage tank is less than 1 multiplied by 10 -3 And after Pa, stopping air extraction. And filling inert gas into the carbon powder storage tank and the buffer storage tank through an inert gas inlet arranged on the buffer storage tank, and stopping filling gas when the pressure value is consistent with the pressure sensor of the gas inlet. And opening the vacuum valve A, and allowing carbon dust in the carbon dust transfer mechanism to fall into the carbon dust storage tank which is replaced again through the buffer storage tank.
The application also provides a method for preparing fullerene. The method for preparing the fullerene adopts the device for preparing the fullerene, and comprises the following steps: the conductivity of the insulating sheath 32 is measured.
As shown in fig. 1, the method for processing fullerene according to the present embodiment includes: s10, vacuumizing the fullerene preparation device to a preset value. And S20, introducing working gas into the fullerene preparation device in the step S10. S30, the carbon soot containing fullerene is obtained by high-temperature gasification of the graphite rod in the gasification furnace in step 20. And S40, pumping the carbon powder out of the gasification furnace through negative pressure pumping, and feeding the carbon powder into a collection storage tank.
According to the technical scheme, firstly, a fullerene preparation device is vacuumized to a preset value, then working gas is introduced into the fullerene preparation device, a graphite rod in a gasification furnace is gasified at high temperature to obtain carbon dust containing fullerene, and finally the carbon dust is extracted from the gasification furnace through negative pressure extraction and enters a collection storage tank. Therefore, the fullerene is produced and collected by the device through a process flow method, so that the time and labor can be saved, and the pollution to the environment can be reduced. The technical scheme of this embodiment has solved when preparing fullerene among the prior art effectively, and the product is collected and is wasted time and energy and the problem of polluted environment.
In the embodiment of the present invention, the soot containing fullerene produced in step S30 is rapidly cooled. This can improve the yield of fullerene.
In the technical solution of this embodiment, a heat exchanger is provided in the gasification furnace in step S30, and a wall surface of the gasification furnace has a cooling water jacket. The arrangement of the heat exchanger and the cooling water jacket further improves the cooling effect, the heat exchanger can realize that the cooling speed in the gasification furnace is high, and the heat exchanger divides the gasification furnace into two spaces.
In the technical solution of the present embodiment, in step S30, the method further includes purging the gasification furnace. The heat exchanger is easy to accumulate products on the heat exchanger, and the products attached to the heat exchanger can be blown down by blowing, so that the yield and the heat exchange efficiency are improved.
In the technical solution of this embodiment, the step S40 further includes separating carbon powder from the air flow, and collecting the separated carbon powder to a collecting storage tank. The above separation can reduce the amount of the collecting storage tank, and specifically, the fullerene processing method of the present embodiment requires negative pressure pumping and continuous working gas introduction, so as to separate the product from the gas, and only collect the product into the collecting storage tank.
In the technical solution of this embodiment, after step S40, the method further includes transferring the collected collection tank. This completes the process from production to collection. Specifically, the collected patent collecting tank can adopt the following two ways: the import on the collection storage tank is provided with first valve, can shift for collection storage tank and first valve together when shifting the collection storage tank, also can only dismantle the collection storage tank from first valve and shift.
In the technical solution of this embodiment, the fullerene processing method further includes detecting an insulating property of an insulating member on the gasification furnace assembly. Thus, the fullerene production can be ensured to be smoothly carried out. Specifically, when the insulation performance of the insulation member is detected to be unsatisfactory, purging is performed.
It is noted that, in this document, relational terms such as "first" and "second," and the like, may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising a … …" does not exclude the presence of another identical element in a process, method, article, or apparatus that comprises the element.
The above description is merely illustrative of particular embodiments of the invention that enable those skilled in the art to understand or practice the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (11)

1. An insulation assembly, characterized in that the insulation assembly (30) is connected to a gasification furnace (11), the insulation assembly (30) comprising:
the purging flange (31), wherein the purging flange (31) comprises a flange body (311) and a gas channel (312), the gas channel (312) is arranged in the flange body (311), and a gas inlet of the gas channel (312) is arranged on the outer wall surface of the purging flange (31);
an insulating sleeve (32), wherein the insulating sleeve (32) is arranged between the purging flange (31) and the gasification furnace (11), and the gas outlet of the gas channel (312) is arranged on the side of the purging flange (31) facing the insulating sleeve (32); wherein
The electrode sleeve can extend into the gasification furnace (11) through the purging flange (31) and the insulating sleeve (32), and a purging channel (33) is formed between the gas outlet of the gas channel (312) and the gasification furnace (11).
2. The insulation assembly of claim 1, wherein the flange body (311) includes a first body section (3111) and a second body section (3112), inner diameters of the first body section (3111) and the second body section (3112) being the same, an outer diameter of the first body section (3111) being larger than an outer diameter of the second body section (3112), and gas outlets of the gas passages (312) being disposed circumferentially outside of the second body section (3112).
3. The insulation assembly of claim 2, wherein the gas outlet of the gas channel (312) is a plurality of gas outlets, the plurality of gas outlets being arranged at intervals at a junction of the first body segment (3111) and the second body segment (3112).
4. An insulation assembly according to claim 2, characterized in that the insulation sleeve (32) comprises a first sleeve section (321) and a second sleeve section (322) which are integrally formed, the inner diameter of the first sleeve section (321) being larger than the inner diameter of the second sleeve section (322), the side of the first sleeve section (321) facing the purge flange (31) being sealingly connected to the side of the first body section (3111) facing the insulation sleeve (32).
5. An insulation assembly according to claim 4, characterized in that the inner wall of the first sleeve section (321) and the outer wall of the second body section (3112) have a first gap (331), that the second sleeve section (322) has a second gap (332) between the side of the second body section (3112) facing the second sleeve section (3112) and the side of the second body section (3112) facing the second sleeve section (322), that the inner wall of the second sleeve section (322) and the outer wall of the electrode sleeve have a third gap (333), and that the first gap (331), the second gap (332) and the third gap (333) form the purge channel (33).
6. The insulating assembly according to claim 5, characterized in that the width of the second gap (332) is greater than or equal to the width of the first gap (331), and the width of the third gap (333) is greater than the width of the second gap (332).
7. The insulation assembly according to claim 5, wherein the width of the first gap (331) is between 2mm and 5mm, the width of the second gap (332) is between 2mm and 7mm, and the width of the third gap (333) is between 5mm and 10 mm.
8. Insulation assembly according to claim 1, characterized in that the circumferential outer side of the insulation sleeve (32) has an annular groove.
9. Insulation assembly according to claim 1, characterized in that the material of the insulating sheath (32) is insulating ceramic or polytetrafluoroethylene.
10. An apparatus for producing fullerenes, comprising a gasifier module and a fullerene recovery module, the fullerene recovery module being connected to the gasifier module, the gasifier module comprising an insulating assembly (30), the insulating assembly (30) being an insulating assembly (30) according to any one of claims 1 to 9.
11. A method for producing a fullerene, characterized in that the method for producing a fullerene employs the apparatus for producing a fullerene according to claim 10, the method comprising:
the conductivity of the insulating sleeve (32) is detected.
CN202211020117.7A 2022-08-24 2022-08-24 Insulating assembly, device for preparing fullerene and method for preparing fullerene Pending CN115448292A (en)

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