CN211522400U - Microwave heating carbon fiber precursor annealing-pre-oxidation treatment equipment - Google Patents
Microwave heating carbon fiber precursor annealing-pre-oxidation treatment equipment Download PDFInfo
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- CN211522400U CN211522400U CN201922295504.1U CN201922295504U CN211522400U CN 211522400 U CN211522400 U CN 211522400U CN 201922295504 U CN201922295504 U CN 201922295504U CN 211522400 U CN211522400 U CN 211522400U
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Abstract
The utility model relates to a microwave heating carbon fiber precursor annealing-pre-oxidation treatment device, which comprises an annealing treatment microwave oven, a pre-oxidation microwave oven, a rectangular quartz carrier tube, a gas distribution device, a thermocouple and a ventilation pipeline, wherein the rectangular quartz carrier tube, the gas distribution device, the thermocouple and the ventilation pipeline are respectively arranged in the two microwave ovens, and the pre-oxidation microwave oven is divided into three chambers by a heat insulation baffle; the carbon fiber precursor is sequentially subjected to annealing and pre-oxidation treatment through the traction assembly. The annealing treatment can well eliminate the acting stress among the molecules in the fiber, and is convenient for the full and uniform pre-oxidation treatment of the fiber; the pre-oxidation temperature gradient adjustment is helpful to eliminate the problem of uneven structure; the traction component can conveniently and flexibly adjust the magnitude of the fiber drafting tension; the equipment improves the heating efficiency and the energy utilization rate, greatly shortens the time required by the pre-oxidation of the carbon fiber precursors, and ensures that the prepared carbon fibers have perfect appearance and uniform structure and almost have no obvious skin-core structure, thereby laying a solid foundation for obtaining high-strength asphalt-based carbon fibers.
Description
Technical Field
The utility model belongs to the technical field of the carbon fiber preparation, a preoxidation technique of carbon fiber is related to, especially relate to a microwave heating carbon fiber precursor annealing-preoxidation treatment facility that helps improving carbon fiber performance.
Background
Pitch-based carbon fibers are generally carbon fibers having a certain tensile strength and elastic modulus, which are obtained by spinning, pre-oxidation and carbonization of coal tar pitch or petroleum pitch by means of a thermal polycondensation process, and generally have a carbon content of 95% or more, particularly 99% after graphitization. Due to the excellent high temperature resistance, corrosion resistance, fatigue resistance, radiation resistance, high electric conductivity and heat transfer performance, the composite material is widely applied to the advanced fields of aerospace, national defense and military and the like and the civil industries of advanced sports goods, medical appliances and the like. However, the process of carbon fiber preparation is complex, and especially, the pre-oxidation treatment is time-consuming and labor-consuming, and the condition of non-uniform fiber internal and external structures (skin-core structure) is also easily generated, so that the performance of the fiber is greatly influenced, and therefore how to improve the pre-oxidation rate and quality of the fiber becomes a key for restricting the development of the pitch-based carbon fiber.
The pitch-based carbon fiber pre-oxidation treatment is mainly to convert the fiber from thermoplasticity to thermosetting, and the melting phenomenon does not occur in the subsequent carbonization and graphitization treatment processes, and in the process, oxygen is usually utilized to react with active components in the fiber to form an oxygen-containing cross-linked structure, and meanwhile, small molecular gas is generated to achieve the purpose of non-melting. To traditional pre-oxidation oven, mainly adopt the heating of electric stove silk to produce the heat, reach the purpose of fibre pre-oxidation with the help of oxidizing atmosphere, the fibre mainly heats through heat conduction and thermal radiation's mode in this process, because the oxidation furnace chamber is great, each position temperature differs, produce the thermal convection phenomenon very easily, the inhomogeneity of furnace temperature has been aggravated to a certain extent, in addition pitch base carbon fiber precursor intensity ratio is lower, make this process very easily appear disconnected silk phenomenon, and traditional heating method heat is from the fibre surface to inside diffusion, easily make the skin-core structure appear in the fibre like this, traditional unilateral ventilation mode makes oxygen distribute inequality in the stove simultaneously, and the gas that produces in the pre-oxidation process is at the furnace enrichment easily.
The microwave heating has the characteristics of uniform heat, quickness, energy conservation, instant adjustment and the like, has obvious advantages when being applied to the carbon fiber pre-oxidation process, and becomes a research hotspot. Patent CN2018201826003 discloses a fiber pre-oxidation device, which applies a microwave focusing to a fiber yarn bundle passing continuously through a super-high speed pre-oxidation process, so as to quickly and effectively reduce the skin-core structure of oxidized fibers. Patent CN2018206432002 discloses a microwave heating polyacrylonitrile pre-oxidation device, wherein polyacrylonitrile horizontally moves through a traction mechanism and sequentially passes through three microwave ovens, and an oxidant is filled in a titration funnel, so that pre-oxidation treatment of gradient temperature rise is realized. However, most of the existing microwave pre-oxidation devices are only suitable for polyacrylonitrile carbon fibers and pitch-based carbon fibers, and the microwave heating devices for preparing the carbon fibers are not reported, but the requirements of different raw materials on equipment required for preparing the carbon fibers are quite different.
In addition, in the spinning process, due to the unique performance of the spinnable pitch, the spinning process has only one time of drafting opportunity, the shearing action and the rapid drafting at the spinneret plate enable large action stress to exist among macromolecules in the fiber, and if direct pre-oxidation treatment is carried out, more micro defects are likely to appear in the finally obtained carbon fiber. Therefore, it is of great practical and economic significance to design a microwave heating device suitable for pitch-based carbon fibers to improve the pre-oxidation rate and quality of the fibers.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to overcome prior art's defect, provide a microwave heating carbon fiber precursor annealing-pre-oxidation treatment facility that helps improving carbon fiber performance, this equipment adopts microwave heating and has increased fibre annealing device before the pre-oxidation, has improved heating efficiency and energy utilization, has shortened the required time of carbon fiber precursor pre-oxidation greatly, and the carbon fiber appearance that makes is perfect, the structure is even, does not have obvious skin core structure almost.
The utility model discloses a following technical scheme realizes:
the annealing-pre-oxidation treatment equipment for microwave heating of the carbon fiber precursor mainly comprises an annealing treatment microwave oven and a pre-oxidation microwave oven, wherein a carrier tube and a gas distribution device which are horizontally arranged along the axial direction of a furnace chamber, a thermocouple and a ventilation pipeline which are vertical to the axial direction are respectively arranged in the annealing treatment microwave oven and the pre-oxidation microwave oven.
Holes for gas to enter the furnace chamber are uniformly formed in the upper surface and the lower surface of the carrier tube, the gas distribution devices are arranged on the upper side and the lower side of the carrier tube, so that the atmosphere in the furnace chamber is uniformly distributed, the tail end of the thermocouple is positioned in the middle of the cavity of the carrier tube, the other end of the thermocouple is connected with the controller, and the temperature in the furnace is changed by adjusting the controller; the inlet of the ventilation pipeline is provided with a flow regulating valve for controlling the gas flow.
The carbon fiber precursor passes through the annealing treatment microwave oven and the pre-oxidation microwave oven in sequence through the traction assembly; the traction assembly is a rolling wheel externally connected with a power device.
Preferably, a rolling wheel is respectively arranged at the inlet of the annealing treatment microwave oven and the outlet of the pre-oxidation microwave oven, and three or more rolling wheels are arranged between the two microwave ovens.
Preferably, a rolling wheel in the traction assembly is provided with a torsion sensor, and the magnitude of the traction force can be set according to the fiber traction requirement; the drawing force is preferably 0.04 MPa.
Preferably, the carrier tube is a rectangular quartz carrier tube, and the quartz material can effectively prevent the powder generated by the heat insulation material on the inner wall of the hearth from polluting the fibers.
The atmosphere in the furnace may include gases having an oxidizing action such as oxygen, ozone, and air, and inert gases such as nitrogen, argon, and helium. Preferably, inert gas is introduced into the annealing treatment microwave oven, and the temperature is set to be 200 ℃; and introducing gas with an oxidizing effect into the pre-oxidation microwave oven, wherein the set temperature range is 100-300 ℃.
Further, as the utility model discloses preferred technical scheme, annealing treatment microwave oven is single chamber, divide into a plurality of cavities with it through setting up thermal-insulated baffle in the pre-oxidation microwave oven, every cavity is equipped with thermocouple and vent line alone, and the microwave generator of every cavity regulates and control alone, satisfies the demand of different stages pre-oxidation temperature.
Preferably, the pre-oxidation microwave oven has three chambers, and the temperature of each chamber is 100 ℃, 200 ℃ and 300 ℃ from left to right.
The carbon fiber precursor for the equipment treatment is pitch-based carbon fiber precursor, polyacrylonitrile-based carbon fiber precursor and viscose-based carbon fiber precursor.
The working process of the microwave heating carbon fiber precursor annealing-pre-oxidation treatment equipment is as follows:
the carbon fiber precursor enters the annealing treatment microwave oven with specific temperature and specific atmosphere through a rolling wheel at the inlet of the annealing treatment microwave oven for annealing treatment, then enters the multi-cavity pre-oxidation microwave oven through the rolling wheel, each cavity of the pre-oxidation microwave oven keeps oxidizing atmosphere, but the temperature is raised from left to right in sequence, and finally the annealed and pre-oxidized carbon fiber precursor is discharged from a filament outlet through the rolling wheel.
The utility model discloses in, carbon fiber precursor gets into annealing treatment microwave oven at first and carries out annealing treatment, eliminates the intermolecular stress that produces because of distortion, shearing, draft between the macromolecule lamella that the fibre exists inside, makes the fibre easily oxygen molecule's diffusion in the following pre-oxidation treatment process, reduces the probability that fibre skin-core structure produced, especially for mesophase pitch base carbon fiber, annealing treatment not only eliminates intermolecular stress, still increases the stacking height of molecule lamella, makes the orientation of microcosmic fiber bundle stronger; the fibre after annealing process loops through the different pre-oxidation microwave ovens of power under the effect of pulling the subassembly, because the radiant intensity of microwave is different, make the interior temperature of stove produce the ladder change, in addition pre-oxidation belongs to the molecule diffusion control process, if the intensification is too fast, probably arouse the macromolecule to take place the schizolysis reaction, thereby cause the fibre hole structure to appear, the while intensification is too fast still can make the fibre surface take place excessive oxidation and form the oxide layer that the one deck is fine and close, prevent oxygen molecule to its inside diffusion, make the skin-core structure appear in the fibre, and multi-chamber pre-oxidation microwave oven, through regulation and control microwave intensity, the fibrous rate of rise of temperature of control that can be fine, reach ideal pre-oxidation.
Compared with the prior art, the beneficial effects of the utility model are as follows: the device has compact structure, reliable principle and easy operation; the microwave heating mode fully utilizes the advantages of uniform microwave heating, high speed and instantaneous controllability, and overcomes a plurality of defects of the traditional pre-oxidation furnace; two microwave ovens of annealing treatment and pre-oxidation treatment are sequentially arranged, so that the heating efficiency and the energy utilization rate are improved, and the time required by pre-oxidation of the carbon fiber precursor is greatly shortened; firstly, the carbon fiber protofilament is annealed, so that the acting stress among partial molecules in the fiber can be well eliminated, the diffusion of oxygen molecules is easy, the skin-core structure is eliminated, the orientation of a microscopic fiber bundle is enhanced, the subsequent sufficient and uniform preoxidation treatment of the fiber is facilitated, and the occurrence of microscopic defects in the carbon fiber caused by direct preoxidation is avoided; the pre-oxidation microwave oven adopts a multi-cavity design, realizes independent regulation of pre-oxidation temperature and atmosphere, can meet pre-oxidation requirements of different stages, and is beneficial to eliminating the problem of uneven pre-oxidation of fibers because the temperature and the heating rate in the oven generate step change along with the fiber oxidation process; and the gas distribution device enables the atmosphere in the furnace cavity to be uniformly distributed, the torsion sensor arranged on the traction assembly is convenient and flexible to adjust the drafting tension of the fibers, the prepared carbon fibers are perfect in appearance and uniform in structure, almost have no obvious skin-core structure, and a solid foundation is laid for obtaining the high-strength asphalt-based carbon fibers.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
FIG. 1 is a schematic structural diagram of an embodiment of the present invention,
in the figure: 1-thermocouple, 2-ventilation pipeline, 3-annealing treatment microwave oven, 4-gas distribution device, 5-carrier tube, 6-carbon fiber precursor, 7-rolling wheel at inlet of microwave oven, 8,9, 10-rolling wheel, 11-rolling wheel at outlet of microwave oven, 12-pre-oxidation microwave oven and 13-heat-insulating baffle.
Detailed Description
In order to more clearly explain the overall concept of the present invention, the following detailed description is given by way of example in conjunction with the accompanying drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application, however, the present application may be practiced in other ways than those described herein, and therefore the scope of the present application is not limited by the specific embodiments disclosed below.
Example 1
The embodiment provides annealing-pre-oxidation treatment equipment for microwave heating carbon fiber precursors, which comprises an annealing treatment microwave oven (3), a pre-oxidation microwave oven (12), rectangular quartz carrier tubes (5) respectively arranged in the two microwave ovens, a gas distribution device (4), a thermocouple (1) and a ventilation pipeline (2); holes are uniformly formed in the upper surface and the lower surface of the rectangular quartz carrier tube (5), so that gas can conveniently enter the furnace chamber; the gas distribution devices (4) are distributed up and down and are arranged on the upper side and the lower side of the carrier tube (5) to ensure that the atmosphere in the oven cavity is uniformly distributed, and a gas flow regulating valve is arranged at the inlet of the ventilation pipeline (2) to ensure that the atmosphere in the microwave oven is uniformly and stably kept; the thermocouple (1) is inserted into the carrier tube (5) from the top of the microwave oven, the tail end of the thermocouple is positioned in the middle of the cavity of the carrier tube (5), the other end of the thermocouple is connected with a controller, and the temperature in the oven is changed by adjusting the controller; the rolling wheels (7) and (11) are respectively arranged at the inlet of the annealing microwave oven (3) and the outlet of the pre-oxidation microwave oven (12), and three rolling wheels (8), (9) and (10) are arranged between the two microwave ovens; the rolling wheels (7), (8), (9), (10) and (11) in the traction assembly are externally connected with a power device, wherein the rolling wheels (7), (8), (10) and (11) are connected with torsion sensors, and the magnitude of the traction force can be set according to the fiber traction requirement;
heating an annealing treatment microwave oven (3) to 200 ℃, introducing nitrogen and keeping the gas flow stable, heating a cavity of a pre-oxidation treatment microwave oven (12) to 200 ℃, introducing compressed air into the oven cavity and keeping the gas flow stable, adjusting the rotating speed of a traction assembly to keep the fiber at a certain drawing force of 0.04MPa, and simultaneously enabling the pitch-based carbon fiber precursor to sequentially pass through the annealing treatment microwave oven and the pre-oxidation microwave oven through the traction assembly for carbonization treatment, wherein the obtained carbon fiber has fewer hole structures and skin-core structures, and a few precursors are broken, which shows that continuous heating is realized through annealing-pre-oxidation treatment, and the obtained precursors have stronger orientation of microscopic fiber bundles, more uniform radial direction, fewer internal microscopic defects and higher bulk density, thereby laying a foundation for obtaining high-performance carbon fibers.
Example 2
As shown in fig. 1, the present embodiment provides a multi-chamber microwave heating annealing-pre-oxidation treatment apparatus for carbon fiber precursor, which comprises an annealing treatment microwave oven (3), a multi-chamber pre-oxidation microwave oven (12), and rectangular quartz carrier tubes (5), a gas distribution device (4), a thermocouple (1) and a vent pipe (2) which are respectively arranged in the two microwave ovens; holes are uniformly formed in the upper surface and the lower surface of the rectangular quartz carrier tube (5), so that gas can conveniently enter the furnace chamber; the gas distribution devices (4) are distributed up and down and are arranged on the upper side and the lower side of the carrier tube (5) to ensure that the atmosphere in the oven cavity is uniformly distributed, and a gas flow regulating valve is arranged at the inlet of the ventilation pipeline (2) to ensure that the atmosphere in the microwave oven is uniformly and stably kept; the thermocouple (1) is inserted into the carrier tube (5) from the top of the microwave oven, the tail end of the thermocouple is positioned in the middle of the cavity of the carrier tube (5), the other end of the thermocouple is connected with a controller, and the temperature in the oven is changed by adjusting the controller; the rolling wheels (7) and (11) are respectively arranged at the inlet of the annealing microwave oven (3) and the outlet of the pre-oxidation microwave oven (12), and three rolling wheels (8), (9) and (10) are arranged between the two microwave ovens; the rolling wheels (7), (8), (9), (10) and (11) in the traction assembly are externally connected with a power device, wherein the rolling wheels (7), (8), (10) and (11) are connected with torsion sensors, and the magnitude of the traction force can be set according to the fiber traction requirement;
the multi-cavity pre-oxidation microwave oven is internally provided with a heat insulation baffle (13) to divide the multi-cavity pre-oxidation microwave oven into three cavities, each cavity is independently provided with a thermocouple and a ventilation pipeline, and a microwave generator of each cavity can be independently regulated and controlled to meet the requirements of pre-oxidation temperatures at different stages;
heating an annealing treatment microwave oven (3) to 200 ℃, introducing nitrogen, keeping the gas flow stable, leading the temperature of each chamber of a multi-chamber preoxidation microwave oven (12) to be 100 ℃, 200 ℃ and 300 ℃ respectively from left to right, introducing compressed air into the oven chamber and keeping the gas flow stable, adjusting the rotating speed of a traction assembly to ensure that the fiber keeps a certain traction force of 0.04MPa, simultaneously leading pitch-based carbon fiber protofilament to sequentially pass through the annealing treatment microwave oven (3) and the multi-chamber preoxidation microwave oven (12) through the traction assembly for carbonization treatment, almost eliminating a hole structure and a skin-core structure in the obtained carbon fiber, not finding protofilament fracture, showing that continuous heating and temperature gradient change are realized through annealing-multi-chamber preoxidation treatment, leading the orientation of a microscopic fiber bundle in the obtained protofilament to be stronger, leading the radial oxidation to be more uniform, and avoiding the occurrence of internal microscopic defects, the density of the fiber body is improved, and a foundation is laid for obtaining high-performance carbon fiber.
Comparative example 1
The same equipment as that in example 1 is adopted, except that the pitch-based carbon fiber precursor is directly subjected to pre-oxidation treatment in the same atmosphere without annealing treatment, and it is found that the fiber precursor is easily subjected to severe hole structure and skin-core structure without annealing treatment, and most of the fiber precursor is broken during carbonization; the pitch-based carbon fiber is not suitable for direct microwave heating pre-oxidation due to the particularity of the raw material.
Comparative example 2
The same equipment as in example 2 was used except that the drawing stress was removed and the degree of order of the fiber crystallites was found to be severely reduced after carbonization, both the tensile strength and the elastic modulus were low. And the utility model discloses a change that the subassembly that pulls can be fine is the change of fibre atress in-process in advance for the microcrystalline structure improves the fibrous body density to the development of orderly direction, establishes the basis for obtaining high performance carbon fiber.
Claims (10)
1. The microwave heating carbon fiber precursor annealing-pre-oxidation treatment equipment is characterized by mainly comprising an annealing treatment microwave oven and a pre-oxidation microwave oven, wherein a carrier tube and a gas distribution device which are horizontally arranged along the axial direction of a furnace chamber, a thermocouple and a ventilation pipeline which are vertical to the axial direction are respectively arranged in the annealing treatment microwave oven and the pre-oxidation microwave oven.
2. The microwave-heated annealing-pre-oxidation treatment equipment for the carbon fiber precursor as claimed in claim 1, wherein holes for gas to enter the furnace chamber are uniformly formed on the upper and lower surfaces of the carrier tube, the gas distribution devices are arranged on the upper and lower sides of the carrier tube, the tail end of the thermocouple is positioned in the middle of the cavity of the carrier tube, and the other end of the thermocouple is connected with the controller; the inlet of the ventilation pipeline is provided with a flow regulating valve.
3. The microwave heating annealing-pre-oxidation treatment equipment for the carbon fiber precursor is characterized in that the carbon fiber precursor sequentially passes through an annealing treatment microwave oven and a pre-oxidation microwave oven through a traction assembly; the traction assembly is a rolling wheel externally connected with a power device.
4. The microwave heating annealing-pre-oxidation treatment equipment for the carbon fiber precursor as claimed in claim 3, wherein: the rolling wheel is provided with a torque sensor.
5. The annealing-pre-oxidation treatment equipment for microwave-heated carbon fiber precursors as claimed in claim 3, wherein a rolling wheel is provided at the inlet of the annealing microwave oven and at the outlet of the pre-oxidation microwave oven, and three or more rolling wheels are provided between the two microwave ovens.
6. The microwave heating annealing-pre-oxidation treatment equipment for the carbon fiber precursor as claimed in claim 1, wherein the carrier tube is a rectangular quartz carrier tube, and inert gas is introduced into the annealing treatment microwave oven; gas with oxidation action is introduced into the pre-oxidation microwave oven.
7. The microwave-heated annealing-pre-oxidation treatment equipment for the carbon fiber precursors as claimed in claim 6, wherein the inert gas comprises nitrogen, argon or helium, and the gas with oxidation comprises oxygen, ozone or air.
8. The microwave heating annealing-pre-oxidation treatment equipment for the carbon fiber precursors is characterized in that the pre-oxidation microwave oven is divided into a plurality of chambers by arranging heat insulation baffles, each chamber is independently provided with a thermocouple and a ventilation pipeline, and a microwave generator of each chamber is independently regulated and controlled to meet the requirements of pre-oxidation temperatures in different stages.
9. The microwave-heated annealing-pre-oxidation treatment equipment for the carbon fiber precursors in claim 8, wherein the pre-oxidation microwave oven has three chambers.
10. The microwave-heated annealing-pre-oxidation treatment equipment for the carbon fiber precursors as claimed in any one of claims 1 to 9, wherein the carbon fiber precursors used for the treatment of the equipment are pitch-based carbon fiber precursors, polyacrylonitrile-based carbon fiber precursors or viscose-based carbon fiber precursors.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113502566A (en) * | 2021-09-08 | 2021-10-15 | 江苏美得妮纺织品有限公司 | Carbon fiber precursor pre-oxidation device and use method thereof |
| CN114672899A (en) * | 2022-04-28 | 2022-06-28 | 江西省纳米技术研究院 | Carbon nanotube fiber, and method and system for continuously reinforcing same |
| CN114962398A (en) * | 2022-04-19 | 2022-08-30 | 新创碳谷控股有限公司 | Rotation regulation type gas uniform distribution device, gas distributor and oxidation furnace |
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2019
- 2019-12-19 CN CN201922295504.1U patent/CN211522400U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113502566A (en) * | 2021-09-08 | 2021-10-15 | 江苏美得妮纺织品有限公司 | Carbon fiber precursor pre-oxidation device and use method thereof |
| CN114962398A (en) * | 2022-04-19 | 2022-08-30 | 新创碳谷控股有限公司 | Rotation regulation type gas uniform distribution device, gas distributor and oxidation furnace |
| CN114672899A (en) * | 2022-04-28 | 2022-06-28 | 江西省纳米技术研究院 | Carbon nanotube fiber, and method and system for continuously reinforcing same |
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