CN109881467B - Ceramic long fiber microwave continuous treatment device and method - Google Patents
Ceramic long fiber microwave continuous treatment device and method Download PDFInfo
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- CN109881467B CN109881467B CN201910282528.5A CN201910282528A CN109881467B CN 109881467 B CN109881467 B CN 109881467B CN 201910282528 A CN201910282528 A CN 201910282528A CN 109881467 B CN109881467 B CN 109881467B
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Abstract
The invention discloses a ceramic long fiber microwave continuous treatment device and a method. The ceramic long fiber microwave continuous treatment device comprises: the microwave reaction unit comprises at least one microwave cavity for continuous passage of fibrils, and a fiber inlet and a fiber outlet connected with the microwave cavity; a microwave generating unit comprising a microwave generator capable of providing at least an irradiated microwave, the microwave output from the microwave generator being capable of performing a microwave irradiation treatment on fibrils passing through the microwave cavity. The invention applies the microwave technology to continuous treatment of long fibers, realizes continuous operation such as fibril crosslinking solidification and/or firing, and simultaneously improves energy efficiency and overcomes the inherent defects of low energy efficiency, incapability of continuous operation and the like of the prior art and equipment for realizing the same treatment purpose by utilizing the characteristic of integral microwave heating; the device shortens the process time greatly, improves the production efficiency, saves a large amount of energy sources, and has important practical application value.
Description
Technical Field
The invention particularly relates to a device and a method for continuously treating ceramic long fibers by microwaves, belonging to the technical field of preparation of ceramic fibers.
Background
In recent years, a ceramic fiber (oxide fiber or non-oxide fiber) manufacturing technology has been significantly advanced. The main driving force is derived from the requirements of the fields of aerospace, high-temperature heat insulation and the like on high-performance fibers (high strength, high temperature resistance, high modulus and the like).
Although the manufacturing processes of different kinds of ceramic fibers are different, most of the ceramic fibers are obtained by sol-gel, solution or slurry containing volatile components, or precursor polymer is spun to obtain fibrils, then the fibrils are dried, solidified, crosslinked, modified and the like under certain temperature and atmosphere conditions, and finally the fibrils are converted into the ceramic fibers by using a controllable firing process.
The price of high performance ceramic fibers is relatively high, with highly complex processes accounting for a significant amount of weight. At the same time, the complex process also results in a fiber whose properties and quality are difficult to control stably. The drying, crosslinking, curing or firing of fibrils has been accomplished in the past by batch processes using heating equipment such as ovens and/or kilns. The method has low energy efficiency and high cost due to the use of conduction and convection heating, and enables related process links to be intermittent or intermittent working conditions, so that the continuity of the whole production process and the stability of product performance are affected.
Disclosure of Invention
The invention mainly aims to provide a ceramic long fiber microwave continuous treatment device and a ceramic long fiber microwave continuous treatment method, which utilize microwaves (single-mode microwaves) to dry, crosslink, solidify and/or burn fibrils, realize high-efficiency heating and continuous treatment of the fibrils, and overcome the defects in the prior art.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a ceramic long fiber microwave continuous treatment device, which comprises:
the microwave reaction unit comprises at least one microwave cavity for continuous passage of fibrils, and a fiber inlet and a fiber outlet connected with the microwave cavity;
a microwave generating unit comprising a microwave generator capable of providing at least an irradiated microwave, the microwave output from the microwave generator being capable of performing a microwave irradiation treatment on fibrils passing through the microwave cavity.
Specifically, the microwave reaction unit may be a microwave cavity, or may include more than two microwave cavities connected in series; more than two microwave cavities are connected in series, i.e. two adjacent microwave cavities may be connected by having the fiber inlet (fiber outlet) of one microwave cavity connected to the fiber outlet (fiber inlet) of the other microwave cavity.
Further, the microwave cavity is a resonant cavity.
Further, the microwave cavity is a single-mode microwave resonant cavity.
Further, the shape of the microwave cavity may be cylindrical, square or other shapes.
Further, the material of the microwave cavity is conductive metal, for example, the material of the microwave cavity may be one or more conductive metals or metal alloys, such as aluminum, stainless steel, brass, etc., but not limited thereto.
Further, the fiber inlet and the fiber outlet are oppositely arranged at two ends of the microwave cavity.
Further, the irradiated microwaves are single-mode microwaves.
Further, the microwave generator comprises a microwave power supply and a magnetron, or the microwave generator comprises a microwave oscillator, an adjustable attenuator and a solid-state microwave amplifier, wherein the adjustable attenuator is respectively connected with the microwave oscillator and the solid-state microwave amplifier.
Specifically, the microwave generator generates microwaves with certain frequency and power by utilizing electric energy; specifically, the output power of the microwave generator may be determined according to the processing power requirements of the device, the composition, characteristics, dielectric loss factors of fibrils, and the like.
In some more specific embodiments, the ceramic long fiber microwave continuous processing device further comprises: the microwave transmission unit is respectively connected with the microwave generation unit and the microwave reaction unit and is used for transmitting the irradiation microwaves provided by the microwave generator to the microwave reaction unit.
In some more specific embodiments, the microwave transmission unit comprises a circulator, an impedance matching regulator, and a coupler (as in fig. 1) connected to each other via a waveguide; or the microwave transmission unit includes a circulator and a coupler (see fig. 2) connected to each other via a coaxial line.
In some more specific embodiments, the ceramic long fiber microwave continuous processing device further comprises: the information acquisition unit comprises at least a sensor for acquiring the electric field intensity in the microwave cavity, the temperature of the fibril and the input power and the output power of the microwave reactor. The type and number of the sensors can be determined according to the controllable input type and number of the microwave generator, the processed fibrils and the reaction process variables and parameters which can be detected by the microwave reactor, for example, the sensors can be infrared thermometers, the infrared thermometers and field intensity sensors, the infrared thermometers, the incident reflected power sensors and the like.
Further, the information acquisition unit comprises an infrared thermometer, a field intensity sensor and an incident reflected power sensor.
In some more specific embodiments, the ceramic long fiber microwave continuous processing device further comprises: and the control unit is connected with the microwave generating unit and the information acquisition unit.
Specifically, the control unit may include a microcomputer, a memory, a sensor signal input interface, a control signal output interface, a communication interface with an upper computer and other systems of the fiber production line, a man-machine interface, and the like. The microcomputer is mainly used for determining an output control signal according to a sensor output signal and a control algorithm, then feeding the control signal to a magnetron, a microwave oscillator, an adjustable attenuator, a preamplifier or the like through a control signal output interface, and adjusting the working state of the microwave generator to enable the controlled quantity such as temperature, microwave mode in a microwave cavity, microwave frequency, microwave power and the like to be consistent with a set value or a target state; the communication interface is used for exchanging information with other equipment so that the running condition of the device is coordinated with the other equipment; the man-machine interface is used for setting the operation parameters of the device and displaying the size, the change trend and the like of the input and output signals of the control system; the memory is used for storing device operation data, so that the processing process management and the subsequent analysis and processing of the device operation data are facilitated. The program control software, the control program and the like adopted by the control unit can be commodity software or written by oneself, and the adopted hardware can be obtained through commercial purchase.
The embodiment of the invention also provides a method for continuously treating the ceramic long fiber by microwaves, which comprises the following steps:
providing the ceramic long fiber microwave continuous treatment device; the device works in such a way that the fibrils pass continuously through the microwave cavity via the fiber inlet and the fiber outlet and the fibrils passing through the microwave reaction unit are subjected to microwave irradiation treatment by means of single mode microwaves.
Further, the microwave irradiation treatment is performed under an air atmosphere or a protective gas (such as nitrogen or inert gas) atmosphere.
Further, the microwave irradiation treatment comprises at least one of heating, drying, crosslinking, curing and firing.
Compared with the prior art, the invention applies the single-mode microwave technology to continuous treatment of long fibers, realizes continuous operation such as fibril crosslinking solidification and/or firing, and simultaneously improves energy efficiency and overcomes inherent defects such as low energy efficiency, incapability of continuous operation and the like of the prior art and equipment for realizing the same treatment purpose by utilizing the characteristic of integral microwave heating; the device shortens the process time greatly, improves the production efficiency, saves a large amount of energy sources, and has important practical application value.
Drawings
FIG. 1 is a schematic diagram of a continuous microwave treatment apparatus for ceramic long fibers according to embodiment 1 of the present invention;
FIG. 2 is a schematic structural view of a ceramic long fiber microwave continuous processing apparatus according to the embodiment 2 and the embodiment 3 of the present invention;
fig. 3 is a schematic diagram of a structure in which a plurality of microwave cavities are connected in series in embodiment 4 of the present invention.
Detailed Description
In view of the shortcomings in the prior art, the inventor of the present invention has long studied and practiced in a large number of ways to propose the technical scheme of the present invention. The technical scheme, implementation process and principle and the like will be further explained with reference to the attached drawings and specific embodiments.
Precursor conversion is a common ceramic fiber manufacturing process, and the general process is that the precursor is melt-spun to obtain fibrils (also called as primary filaments, primary fibers, primary spinning, primary fibers, precursor filaments, etc., which are collectively called as fibrils herein), or the precursor is obtained by a sol-gel process through an extruder; then, the fibril is crosslinked and solidified by heating, oxidation and other modes; finally, ceramic fiber is obtained through high temperature pyrolysis.
Whether it is oxide ceramic fiber or non-oxide ceramic fiber, it is very important to reduce the production cost and improve the product quality, and realizing the continuity of production and manufacture is an important factor for reducing the cost, the cost reduction and the improvement of quality will expand the application range of ceramic fiber and open the application market with great demands on the usage amount, such as chemical industry, automobiles, heat resistant (heat insulating) structures, etc.
Compared with the traditional treatment method, the microwave treatment has obvious advantages, heat is directly generated inside the material, the material is heated from inside to outside, conduction and convection are not needed, related devices do not need to be heated, and the surface of the fiber is not affected. The microwave action brings additional translational and rotational movement to the fiber molecule movement, so that the possibility and opportunity of intermolecular crosslinking are increased, and intermolecular crosslinking can be promoted.
The micro structure and mechanical property of the fibers can be greatly changed due to small changes of the ceramic fiber manufacturing process and parameters, the energy power acted on reactants can be rapidly controlled by means of a microwave technology, and the temperature response hysteresis phenomenon caused by pure hysteresis existing between the control quantity change and the temperature response in the traditional heat conduction and convection heating mode is eliminated, so that the rapid real-time control of the reaction temperature can be realized, the reaction speed can be accelerated by selecting proper microwave parameters, and the crosslinking degree, grain growth and the like related to the crosslinking curing and firing reaction process of the fibers can be better controlled, thereby being beneficial to the stability of the product quality and the improvement of the product performance.
Example 1
The ceramic long fiber microwave continuous processing device in this embodiment is shown in fig. 1, and mainly comprises three parts:
the first part is a microwave generating and transmitting part (a microwave generating part is the microwave generating unit, and a microwave transmitting part is the microwave transmitting unit, and the following is the same), and comprises a magnetron 21, a circulator 22, a dummy load 23, an impedance matching regulator 24 and a coupler 25, wherein the circulator 22 is respectively connected with the magnetron 21, the dummy load 23 and the impedance matching regulator 24, the impedance matching regulator 24 is also connected with the coupler 25, and the coupler 25 is also connected with the microwave cavity 1; wherein the magnetron 21 is a microwave generator mainly for generating microwaves of a fixed frequency; the circulator 22 is mainly used for protecting the magnetron 21, and guides the microwaves reflected from the microwave cavity 1 into the dummy load 23 so as to prevent the magnetron 21 from being influenced by the reflected microwaves; dummy 23 is used to absorb reflected microwaves, and the microwave energy absorbed by dummy 23 is carried away by a cooling system (the cooling system is not shown in fig. 1); the impedance matching adjuster 24 is mainly used for adjusting the impedance matching state between the microwave transmission part and the microwave reactor so as to minimize the reflected microwave power; the coupler 25 is mainly used for coupling microwaves into the microwave reactor.
The second part is a microwave reactor and comprises a microwave cavity 1, a fiber inlet 11 and a fiber outlet 12; wherein the microwave cavity 1 is made of a high conductivity metal material (e.g., aluminum, brass, stainless steel, etc.). The microwave cavity is a single-cavity, the inner size of the single-cavity is determined by the microwave frequency and the microwave mode required by operation, the direction of an electric field in the microwave cavity is parallel to the axis of the microwave cavity when the device works, and the intensity of the electric field on the axis of the microwave cavity takes the maximum value.
The third part is a measuring and controlling system (namely the information acquisition unit and the control unit) and comprises an infrared thermometer 7 and a control system 8; wherein, the infrared thermometer 7 is used for measuring the temperature of the fiber and transmitting a temperature signal to a control system (mainly a temperature control system); the control system is composed of a microcomputer, an input/output interface, a human-computer interface and the like, receives fiber temperature signals from the infrared thermometer, obtains control signals according to a control algorithm, then feeds the control signals to a magnetron, and controls microwave power output by the magnetron so as to keep the actual temperature of the fibers consistent with the set temperature.
The working process for processing the fibrils based on the ceramic long fiber microwave continuous processing device comprises the following steps: after the Polycarbosilane (PCS) is sprayed out from a melt spinning port, PCS fibers (or fiber bundles consisting of a plurality of PCS fibers) 100 enter a microwave cavity 1 of a microwave reactor through a fiber inlet, microwave irradiation of a microwave generator is received in the process of passing through the microwave cavity, the PCS fibers are heated to 140-210 ℃ in air atmosphere, and then leave the treatment device through a fiber outlet. When the PCS fiber is in the microwave cavity, the microwave led into the microwave cavity by the microwave generating and transmitting part interacts with the PCS fiber, and meanwhile, the fiber is solidified and crosslinked by the oxygen, the measuring and controlling system continuously detects the temperature of the fiber in the microwave cavity, and calculates a magnetron power control signal according to the error between the fiber set temperature and the actual temperature and a control algorithm, and controls the microwave output power of the magnetron, so that the actual temperature of the temperature measuring point is consistent with the set temperature.
Example 2
The ceramic fiber microwave continuous processing apparatus in this example is shown in fig. 2, which is similar to example 1, and the whole apparatus is still composed of three parts of a microwave generating and transmitting part, a microwave reactor and a measuring and controlling system, which are different from example 1 in the following points:
first, the microwave generator mainly comprises a microwave oscillator 31, an adjustable attenuator 32 and a solid-state microwave amplifier 33, wherein the adjustable attenuator 32 is respectively connected with the microwave oscillator 31 and the solid-state microwave amplifier 33. Wherein, the output frequency of the microwave oscillator 31 is adjustable, and the output frequency of the microwave oscillator is adjusted by utilizing the frequency control signal output by the control system; the adjustable attenuator is mainly used for controlling the amplitude of a microwave signal output by the microwave oscillator to enable the amplitude to be within the allowable range of the microwave amplifier; the microwave amplifier consists of solid-state devices, amplifies the microwave signals and outputs microwave power; the loop 22 is directly connected to the coupler 25 without using an impedance matching regulator in the transmission part of the microwave generating and transmitting part in this embodiment, the solid state microwave amplifier 33 is connected to the loop 22, and the loop 22 is also connected to the dummy load 23.
Secondly, the measuring and controlling system measures the distribution state of the electric field intensity in the microwave cavity through the field intensity sensor besides measuring the fiber temperature, and the controlling system respectively determines a frequency control signal and a power control signal according to a control algorithm by utilizing the temperature signal and the field intensity signal.
The working process for processing the fibrils based on the ceramic long fiber microwave continuous processing device comprises the following steps: alumina sol is extruded from the spinneret orifices, and long fibers (which can be understood as fibrils) formed from the alumina sol enter the microwave cavity 1 from the fiber inlet, are subjected to microwave irradiation while passing through the microwave cavity 1, and then leave the treatment device from the fiber outlet 12. When the fiber is in the microwave cavity, the microwave which is guided into the microwave cavity by the microwave generating and transmitting part interacts with the long fiber, and the sol precursor is gelled and converted; the measuring and controlling system continuously detects the temperature and field intensity state of the fiber in the microwave cavity, if the actual temperature deviates from the set temperature, the controlling system adjusts the power control signal according to the control algorithm, and the output power of the microwave amplifier is controlled by changing the output signal of the attenuator so as to keep the actual temperature consistent with the set temperature; if the microwave mode in the microwave cavity deviates from the predetermined mode due to the influence of the fiber bundle, the control system 8 calculates and determines a microwave frequency control signal by using the output signal of the field strength sensor 6 and a corresponding frequency control algorithm, adjusts the output frequency of the microwave oscillator, and returns the microwave mode in the microwave cavity to the predetermined mode.
In this embodiment, since the long fiber in the microwave cavity is always located near the axis with the maximum electric field strength, the microwave has the strongest effect on the fiber and the highest effect efficiency, and this embodiment is applicable to the fiber material with smaller dielectric loss factor and the fiber material with larger dielectric loss factor.
Example 3
The ceramic fiber microwave continuous processing apparatus in this example is similar to that of fig. 2, and the entire apparatus is still composed of three parts, a microwave generating and transmitting part, a microwave reactor, and a measuring and controlling system, similar to that of example 2.
The working process for processing the fibrils by the ceramic long fiber microwave continuous processing device comprises the following steps: extruding alumina and silica sol with a certain proportion from a spinneret orifice, wherein long fibers formed by the extrusion enter a microwave cavity from a fiber inlet, are irradiated by microwaves when passing through the microwave cavity, and leave a treatment device from a fiber outlet; when the fiber is in the microwave cavity, the microwave which is guided into the microwave cavity by the microwave generating and transmitting part interacts with the long fiber, the sol precursor is gelled and converted at 80-400 ℃ and is crystallized and converted into mullite fiber at 900-1400 ℃; the measuring and controlling system continuously detects the temperature and field intensity state of the fiber in the microwave cavity, if the actual temperature deviates from the set temperature, the controlling system adjusts the power control signal according to the control algorithm, and the output power of the microwave amplifier is controlled by changing the output signal of the attenuator so as to keep the actual temperature consistent with the set temperature; if the microwave mode in the microwave cavity deviates from the preset mode due to the influence of the fiber bundle, the control system calculates and determines a microwave frequency control signal by utilizing the output signal of the field intensity sensor and a corresponding frequency control algorithm, and adjusts the output frequency of the microwave oscillator so that the microwave mode in the microwave cavity returns to the preset mode.
In this embodiment, the fibers in the microwave cavity are always located near the axis with the maximum electric field strength, so that the effect of microwaves on the fibers is strongest and the effect efficiency is highest.
Example 4
For the fiber material requiring a long reaction time or the process of continuously completing the crosslinking curing and firing of the long fiber once, a plurality of microwave treatment apparatuses may be used to operate in series, as shown in fig. 3, in which only a structure in which a plurality of microwave reactors are connected in series is shown, and a microwave generator, a sensor, a control system, etc. associated with each microwave treatment apparatus may be any one of the cases of embodiment 1, embodiment 2, and embodiment 3.
The microwave reactor is composed of conductive metal materials, the internal space of the microwave reactor is a single-mode microwave resonant cavity (namely the microwave cavity) which can be cylindrical or rectangular, and for microwaves with different frequencies, the single-mode microwaves can be formed in the microwave reactor by adopting resonant cavities with different sizes, which are determined by partial differential equations and boundary conditions for describing the microwaves, and the microwave reactor is a physical constraint; the reflection and superposition of single-mode microwaves in the resonant cavity form standing waves, so that strong field intensity can be obtained, materials (such as fibers) with poor microwave absorption capacity can be processed, and the single-mode microwave field intensity is deterministic in the cavity, so that the single-mode microwave cavity is suitable for processing continuous materials with small or fine cross sections (the main effect of the processed materials is electric field components in microwaves, the cylindrical microwave cavity adopted in the embodiment of the invention has the strongest electric field intensity along the cylindrical axis, and the farther from the axis, the lower the electric field intensity).
The invention applies the microwave technology to continuous treatment of long fibers, realizes continuous operation such as fibril crosslinking solidification and/or firing, and simultaneously improves energy efficiency and overcomes the inherent defects of low energy efficiency, incapability of continuous operation and the like of the prior art and equipment for realizing the same treatment purpose by utilizing the characteristic of integral microwave heating; the device shortens the process time greatly, improves the production efficiency, saves a large amount of energy sources, and has important practical application value.
It should be noted that, the present invention is mainly related to providing a continuous microwave processing device for ceramic long fibers, in which the parts or components forming the device, such as a magnetron, a circulator, a dummy load, an impedance matching regulator, a coupler, etc., may all be existing standard components, and all be obtained by commercial purchase or homemade, and the program control software and programs adopted in the device may all be obtained by commercial purchase or homemade.
It should be understood that the above embodiments are merely for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the present invention and implement the same according to the present invention without limiting the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (7)
1. A method for microwave continuous treatment of ceramic long fibers, which is characterized by comprising the following steps:
providing a ceramic long fiber microwave continuous processing device, wherein the ceramic long fiber microwave continuous processing device comprises:
the microwave reaction unit comprises at least one microwave cavity for continuous passage of fibrils, and a fiber inlet and a fiber outlet connected with the microwave cavity;
a microwave generation unit including a microwave generator capable of providing at least irradiation microwaves, the single-mode microwaves outputted from the microwave generator being capable of performing microwave irradiation treatment on fibrils passing through the inside of the microwave cavity;
and passing fibrils continuously through the microwave cavity via a fiber inlet and a fiber outlet, and setting the microwave cavity to an air atmosphere comprising oxygen;
and carrying out microwave irradiation treatment on the fibrils passing through the microwave reaction unit by using single-mode microwaves output by the microwave generator, enabling the direction of an electric field in the microwave cavity to be parallel to the axis of the microwave cavity, enabling the intensity of the electric field to be at the maximum value on the axis of the microwave cavity, enabling the fibrils in the microwave cavity to be always positioned near the axis with the maximum intensity of the electric field, and heating the temperature of the fibrils to 140-210 ℃.
2. The method for continuous microwave treatment of ceramic long fibers according to claim 1, characterized in that: the microwave cavity is a single-mode microwave resonant cavity; and the microwave cavity is made of conductive metal.
3. The method for continuous microwave treatment of ceramic long fibers according to claim 1, characterized in that: the microwave generator comprises a microwave power supply and a magnetron; alternatively, the microwave generator comprises a microwave oscillator, an adjustable attenuator and a solid state microwave amplifier.
4. The method for microwave continuous processing of ceramic long fibers according to claim 1, further comprising: the microwave transmission unit is respectively connected with the microwave generation unit and the microwave reaction unit and is used for transmitting the irradiation microwaves provided by the microwave generator to the microwave reaction unit.
5. The method for continuous microwave treatment of ceramic long fibers according to claim 1, characterized in that: the microwave transmission unit comprises a circulator, an impedance matching regulator and a coupler which are connected with each other, wherein the circulator, the impedance matching regulator and the coupler are connected by a waveguide or a coaxial line.
6. The method for microwave continuous processing of ceramic long fibers according to claim 1, further comprising: the information acquisition unit comprises a sensor for acquiring and obtaining the electric field intensity, the fibril temperature and the input power and the output power of the microwave reactor in the microwave cavity, wherein the sensor is an infrared thermometer, a field intensity sensor and an incident and reflected power sensor.
7. The method for microwave continuous processing of ceramic long fibers according to claim 6, further comprising: and the control unit is connected with the microwave generating unit and the information acquisition unit.
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