CN108114664B - Microwave high-pressure annular reaction device - Google Patents

Microwave high-pressure annular reaction device Download PDF

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CN108114664B
CN108114664B CN201711419236.9A CN201711419236A CN108114664B CN 108114664 B CN108114664 B CN 108114664B CN 201711419236 A CN201711419236 A CN 201711419236A CN 108114664 B CN108114664 B CN 108114664B
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microwave
pressure
annular reaction
reaction device
outer pipe
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CN108114664A (en
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李艳君
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Hunan Change Microwave Technology Co ltd
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Hunan Change Microwave Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves
    • B01J3/044Pressure vessels, e.g. autoclaves in the form of a loop
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/12Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
    • B01J19/122Incoherent waves
    • B01J19/126Microwaves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00139Controlling the temperature using electromagnetic heating
    • B01J2219/00141Microwaves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/12Processes employing electromagnetic waves
    • B01J2219/1203Incoherent waves
    • B01J2219/1206Microwaves
    • B01J2219/1209Features relating to the reactor or vessel
    • B01J2219/1221Features relating to the reactor or vessel the reactor per se
    • B01J2219/1224Form of the reactor
    • B01J2219/1227Reactors comprising tubes with open ends
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/12Processes employing electromagnetic waves
    • B01J2219/1203Incoherent waves
    • B01J2219/1206Microwaves
    • B01J2219/1248Features relating to the microwave cavity
    • B01J2219/1251Support for the reaction vessel
    • B01J2219/1254Static supports
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/12Processes employing electromagnetic waves
    • B01J2219/1203Incoherent waves
    • B01J2219/1206Microwaves
    • B01J2219/1275Controlling the microwave irradiation variables

Abstract

The invention discloses a microwave high-pressure annular reaction device, which comprises an annular reaction device, a microwave generation device, a liquid distributor, a liquid inlet and a liquid outlet, wherein the annular reaction device comprises an outer pipe and an inner pipe sleeved in the outer pipe, a space between the outer pipe and the inner pipe forms an annular reaction channel, the microwave generation devices are arranged on the outer surfaces of the outer pipe and the inner pipe, the liquid distributor is vertical to the annular reaction channel, the microwave generation devices arranged on the outer pipe and the inner pipe are arranged in a staggered mode, and reinforcing ribs can be arranged between the outer pipe and the inner pipe. The microwave generating device can bear higher pressure, a plurality of microwave generating devices are uniformly arranged inside and outside, the microwave distribution is uniform and controllable, and the microwave layout is not influenced by the size of equipment; the distance between the outer pipe and the inner pipe can be freely adjusted according to the feed depth of the microwave energy, so that the amplification production is not influenced by the penetration depth of the microwave during the large-scale planning production; easy installation and maintenance, small occupied area and no laminar flow influence during production.

Description

Microwave high-pressure annular reaction device
Technical Field
The invention belongs to chemical reaction equipment, and particularly relates to a microwave high-pressure annular reaction device.
Background
The penetration depth of microwave as an energy wave heating is always a main problem restricting the amplification production, and the effective penetration depth of the microwave is from several centimeters to tens of centimeters in the common aqueous reaction liquid.
In the process of a large number of reaction chemistry and chemical engineering, high temperature and high pressure are usually accompanied, the conventional microwave high-pressure reaction device has a tubular structure for a common bed, the treatment capacity is small, and the daily treatment capacity is generally within 10 tons. Simultaneously present reaction unit bears pressure and generally adopts two kinds of modes, 1) ceramic inner tube, when using ceramic inner tube, its problem: due to the influence of the properties of the material, the high-temperature and large-size pipe is difficult to bear, the processing difficulty of the large-size pipe is high, and the large-size pipe bears high pressure. Meanwhile, the material is brittle and is very easy to damage during installation and maintenance. 2) A plurality of microwave generators are directly installed on the metal pipeline, and the metal pressure bearing capacity is sharply reduced after a plurality of microwave feed-in ports are provided with holes. Meanwhile, the size of the pipeline is difficult to enlarge due to the influence of the feeding depth of the microwaves. At present, in a microwave continuous high-pressure reaction device, a continuous high-power high-capacity microwave high-pressure high-temperature reaction device is not reported. The method of introducing microwaves into the reaction kettle cannot fully reflect the catalytic promotion effect of the microwaves due to the limited penetration depth of the microwaves.
Simple tubular reactors often cannot withstand a certain operating pressure, in particular at higher temperatures. The traditional tubular reactor has small pipe diameter range and small flow, and is completely not suitable for being used in industrial reaction. The batch reaction result difference is large and the reaction volume is small in the gap type reaction kettle or reaction tank or reaction tube, so that the industrial application of the batch reaction kettle or reaction tank or reaction tube is hindered. In the past, the working pressure of the reaction system and the microwave power output by the microwave source cannot be continuously adjusted at the same time. In the ceramic pipeline reactor, the ceramic pipe is limited in bearing pressure, and meanwhile, the material is fragile and inconvenient to disassemble and install; meanwhile, the size cannot be enlarged due to the influence of the material.
The literature: the key technical research of the frequency conversion high-temperature steam microwave oven indicates that in a general microwave reaction device, it is difficult to find a waveguide port with good coupling in the same resonant cavity, and the work of matching a waveguide port meeting the performance requirement almost accounts for more than 80% of the experimental workload of the whole product. The microwave high-temperature reaction kettle not only needs to consider the problem of microwave excitation, but also needs to consider the problem of high-pressure bearing, so that the design difficulty is higher. The design scheme which only considers one aspect and does not consider the other aspect is not in accordance with the actual requirement.
The feeding method and the feeding structure of the microwave device are the key and difficult points for realizing the air pressure, and are limited by the feeding mode and the feeding structure, the feeding structure is difficult to ensure the pressure resistance of the feeding part, the air flow is easy to leak from the microwave device due to the overhigh pressure, the internal pressure is continuously reduced, the heat loss rate is high, and meanwhile, the leaked liquid flow is easy to impact the microwave source, so that the function failure of the microwave source, the equipment damage and the great safety risk exist.
At present, the feed-in pressure-bearing structure of a microwave device mainly comprises:
firstly, a waveguide-blind plate feeding pressure-bearing mode of a conventional microwave device is adopted.
Secondly, feeding in by adopting a round bottom test tube type wave-transparent element pressure-bearing mode.
In patent CN200610046206, a rectangular waveguide flange is adopted, a quartz plate is adopted for sealing and bearing, a BJ26 microwave rectangular waveguide flange is commonly used, and the size of a rectangular opening is 43.2 × 86.4 mm; the microwave feeding mode seriously influences the pressure design of the autoclave body by opening a rectangular hole in the autoclave body; because the penetration depth of microwaves in a solution, particularly an aqueous solution, is limited, the penetration depth in the aqueous solution is generally not more than 3-8cm, a reaction kettle needs to be produced in an enlarged size, and a plurality of microwave devices are required to be uniformly matched and used from the angle of uniform heating or the angle of microwave feeding depth, when rectangular waveguide energy feeding is adopted, a plurality of rectangular openings are formed, high borosilicate glass and quartz glass are generally selected on a pressure bearing part of a pressure container, national standards GB/T23259 and NB/T47017-2011 clearly indicate that the diameter of the pressure bearing glass is in inverse proportion to the allowable pressure bearing, the stress of the rectangular right-angle position is concentrated, the opening size is large, and the pressure bearing design and the processing difficulty of a kettle body of the reaction kettle and a microwave feeding window are greatly increased.
In patents CN201410471234 and CN201410471231, a round-bottom tube-type wave-transparent element pressure-bearing manner is adopted for feeding, a large-size waveguide opening is adopted for connection on a reaction furnace body, and similarly, when a plurality of microwave devices are used in combination, the uniform arrangement of the microwave devices is seriously influenced due to the limitation of the opening size of a pressure container and the number of corresponding openings, and the design and processing difficulty of the pressure-bearing pressure of a kettle body of a high-pressure reaction kettle and a microwave feeding window is increased; meanwhile, the length of the microwave magnetron antenna is generally between 25 and 50mm, in a large-size high-pressure container, the thickness of 2 fixed flange surfaces and the thickness of a kettle wall are generally more than 10mm, and the exposed length of standard 2450MHz and 915MHz magnetron antennas commonly used in the industry and a rectangular cavity are difficult to match and combine to excite microwaves.
In the prior art, the pressure design and processing difficulty of the reaction device is greatly increased and the application range of the microwave high-pressure device is limited by the limitation of a microwave energy-feeding pressure-bearing structure.
In microwave sintering, because the electromagnetic field in the sintering area has intensity in different areas, so the materials need to be mixed uniformly, the mixing equipment commonly used at present adopts a stirring mode, and when the sintering temperature is higher, the requirements on the materials are very high, the cost is higher, and the requirements are difficult to meet.
Disclosure of Invention
The invention aims to solve the technical problem of providing a microwave high-pressure annular reaction device which has the advantages of high heating power, uniform distribution of a plurality of high-efficiency microwave energy feedback devices, uniform microwave distribution, good pressure bearing capacity, easy amplification production and convenient installation and maintenance.
The annular reaction device comprises an outer pipe and an inner pipe sleeved in the outer pipe, a space between the outer pipe and the inner pipe forms an annular reaction channel, the microwave generating devices are arranged on the outer surfaces of the outer pipe and the inner pipe, the liquid distributor is perpendicular to the annular reaction channel, and the microwave generating devices arranged on the outer pipe and the microwave generating devices arranged on the inner pipe are arranged in a staggered mode. The microwave generating devices are arranged in a staggered mode, so that the heating uniformity of the reaction substances is improved.
And a reinforcing rib is arranged between the outer pipe and the inner pipe.
The annular reaction device is also provided with a safety valve, a pressure measuring device and a temperature measuring device.
The microwave generating device comprises a magnetron and a microwave excitation feed-in pressure-bearing device;
the microwave excitation feed-in pressure-bearing device comprises a circular tube arranged on the annular reaction device, a horn positioned in the annular reaction device, a cone pressure-bearing part positioned in the horn and a wave-transmitting fixing part for limiting the movement of the cone pressure-bearing part;
the antenna of the magnetron is positioned in the circular tube, the antenna and the circular tube form a coaxial resonant cavity, and the coaxial resonant cavity and the horn form a microwave excitation device.
The inner diameter of the circular tube is 5-30 mm. The length of the round tube is 1/4-1/2 of transmitting microwave wavelength. When the wall thickness is reduced, the uniform distribution of a plurality of microwave devices and the efficient excitation energy feedback of microwaves are ensured, and the heating uniformity of the substance is realized.
The height of the cone of the horn is 10-100 mm, the diameter of the horn is 45-180 mm, the preferred height of the cone is 20-50 mm, and the diameter of the horn is 60-140 mm.
The cone bearing part is made of at least one of polytetrafluoroethylene, quartz glass, high-purity alumina, high borosilicate glass and PEEK plastic. The material is wave-transparent material and has pressure resistance.
A sealing gasket is arranged between the cone pressure-bearing part and the inner wall of the horn, and a sealing gasket is arranged between the cone pressure-bearing part and the wave-transmitting fixing part. The sealing gasket is made of at least one of polytetrafluoroethylene, fluororubber and nitrile rubber.
The wave-transmitting fixing piece is a hollow metal flange or a flat plate made of wave-transmitting materials. When the fixing piece is a hollow metal flange, a gasket for force buffering is arranged between the flange and the cone pressure-bearing piece.
The invention has the beneficial effects that: the antenna of the magnetron is positioned in the circular tube, the antenna and the circular tube form a coaxial resonant cavity, the coaxial resonant cavity is combined with the horn according to a certain size proportion to form a microwave excitation device, microwaves enter the annular reaction channel through the cone bearing part after being excited by the microwave excitation device to realize high-efficiency microwave excitation energy feedback, the microwave feed port on the annular reaction device is a circular tube, the inner diameter of the circular tube can be reduced to 5-30mm, the cone bearing part is attached to the inner wall of the horn and fixed through the wave-transparent fixing part, gas or liquid is effectively prevented from leaking from the microwave feed port, the opening size of the kettle body is greatly reduced under the condition of ensuring the effective excitation of the microwaves, the opening shape is improved, the stress condition of the annular reaction device, the microwave feed port and the cone bearing part is improved, the use pressure can be increased to higher pressure, the use range is expanded, a plurality of microwave generation devices are uniformly arranged on the annular reaction device, when realizing even heating, greatly reduced reaction unit and microwave present the bearing pressure design of ability device and the degree of difficulty of processing. Meanwhile, the microwave feed point is moved into the reaction device, the microwave can penetrate to the more central position of the reaction system, the influence of weakened reaction effect caused by the penetration depth of the microwave is reduced, and the reaction device with larger size can be arranged in the same reaction system, so that the amplification and continuous production are easy.
The invention has the advantages that the reinforcing ribs are lined in the device, the stress is more uniform, and the device can bear higher pressure. A plurality of microwave generating devices are uniformly arranged inside and outside, the microwave distribution is uniform and controllable, and the microwave layout is not influenced by the size of the equipment. The ring structure, the depth size of the ring can freely adjust the distance between the outer pipe and the inner pipe according to the feed depth of the microwave energy, so that the amplification production is not influenced by the penetration depth of the microwave during the large-scale planning production. And components such as a ceramic inner tube and the like are not needed, so that the installation and maintenance are easy, and the occupied area is small. Liquid distributors are uniformly distributed up and down, and no laminar flow influence is generated during production.
Drawings
FIG. 1 is a schematic structural diagram of a microwave generating device according to the present invention.
Fig. 2 is a schematic cross-sectional structure of the present invention.
Fig. 3 is a schematic structural diagram of the present invention.
In the figure, 1 annular reaction device, 101 outer tube, 102 inner tube, 2 magnetron, 3 round tube, 4 wave-transparent fixing piece, 5 cone bearing piece, 6 sealing pad, 7 antenna, 8 coaxial resonant cavity, 9 microwave generating device, 10 liquid distributor, 11 reinforcing rib, 12 safety valve, 13 pressure measuring device, 14 annular reaction channel, 15 temperature measuring device, 16 liquid inlet, 17 liquid outlet, 20 loudspeaker.
Detailed Description
As shown in fig. 1-3, the present invention includes an annular reaction device 1, a microwave generating device 9, a liquid distributor 10, a liquid inlet 16 and a liquid outlet 17, wherein the annular reaction device 1 includes an outer tube 101 and an inner tube 102 sleeved in the outer tube 101, a space between the outer tube 101 and the inner tube 102 forms an annular reaction channel 14, the microwave generating device 9 is installed on the outer surface of the outer tube 101 and the outer surface of the inner tube 102, the liquid distributor 10 is perpendicular to the annular reaction channel 14, and the microwave generating device 9 installed on the outer tube 101 and the microwave generating device 9 installed on the inner tube 102 are arranged in a staggered manner.
A reinforcing rib 11 is installed between the outer pipe 101 and the inner pipe 102.
The annular reaction device 1 is also provided with a safety valve 12, a pressure measuring device 13 and a temperature measuring device 15.
The microwave generating device 9 comprises a magnetron 2 and a microwave excitation feed-in pressure-bearing device;
the microwave excitation feed-in pressure-bearing device comprises a circular tube 3 arranged on the annular reaction device 1, a loudspeaker 20 positioned in the annular reaction device 1, a cone pressure-bearing part 5 positioned in the cone 20 and a wave-transparent fixing part 4 for limiting the movement of the cone pressure-bearing part 5;
the antenna 7 of the magnetron 2 is positioned in the circular tube 3, the antenna 7 and the circular tube 3 form a coaxial resonant cavity 8, and the coaxial resonant cavity 8 and the horn 20 form a microwave excitation device.
The outer tube 101 and the inner tube 102 are preferably circular rings.
The invention adopts an annular reaction device, microwave generating devices 9 are uniformly arranged on the metal walls of an outer pipe 101 and an inner pipe 102, reinforcing ribs are lined in the microwave generating devices, liquid conveying pipelines and liquid distributors 10 are arranged at the top and the bottom of the microwave generating devices, a plurality of temperature detection devices are arranged on the reaction device, and a highly integrated control system and a fluid conveying pressurization system are arranged outside the equipment.
The fluid conveying system of the equipment conveys reaction fluid into the annular reaction device 1 from a conveying pipeline at the top or the bottom of the equipment, the reaction fluid uniformly flows into the equipment through the liquid distributor 10, the process temperature to be controlled of each temperature detection device of the equipment is set in the control system, microwave heating is started, the temperature detection devices feed back the actual temperature of each point to the control system, and the microwave heating power of each position is regulated and controlled to realize the stable temperature control of each point. Meanwhile, through the fluid conveying device, the mass of the fluid flowing into the reaction device is controlled to control the residence time of the reaction fluid in the device and control the pressure of the reaction device, and the fluid after the reaction is finished flows out from the other end.
The cone pressure bearing 5 seals the pressure in the annular reaction channel 14 and prevents gas and/or liquid in the annular reaction channel 14 from leaking out of the barrel 3. If the cone pressure-bearing part 5 is not arranged, leaked gas or/and liquid can damage the microwave generating device 9, the reaction device can not guarantee the pressure required by the reaction, and safety risks exist.
The magnetron 2 is fixed with the annular reaction device 1 through screws and a fixing plate and is tightly pressed with the circular tube 3, the antenna 7 of the magnetron 2 is arranged in the circular tube 3 to form a coaxial resonant cavity 8, and a microwave excitation device formed by the coaxial resonant cavity 8 and the loudspeaker 20 is used for effectively exciting microwaves. The round tube 3 and the horn 20 are both made of high-strength metal.
According to the magnetron 2, the antenna 7 and the circular tube 3 form the coaxial resonant cavity 8 when the antenna 7 enters the circular tube 3, and after microwaves are effectively excited by the microwave excitation device formed by combining the coaxial resonant cavity 8 and the loudspeaker 20, the microwaves penetrate through the conical bearing part 5, so that high-efficiency energy feedback with controllable microwave conduction directions is realized; the feed-in port of the annular reaction device 1 is optimized to be a circular tube, the bearing part is optimized to be a cone bearing part 5 and is attached to the inner wall of the horn 20, the cone bearing part 5 is fixed in the horn through the wave-transparent fixing part 4, pressure is sealed in the annular reaction device 1 through the cone bearing part 5, the sealing strength of the whole microwave generating device 9 is improved, gas or/and liquid in the annular reaction device 1 is effectively prevented from leaking from the microwave feed-in port, the microwave effective excitation is ensured, the stress condition of the annular reaction device 1 and the cone bearing part 5 is greatly improved under the condition that the conduction direction is controllable, and meanwhile, the cone bearing part 5 is not exposed outside and is not easy to damage.
Without the cone bearing part 5, the pressure required by the reaction device during working cannot be guaranteed. If the horn 20 which is matched and combined with the coaxial resonant cavity according to a certain size is not adopted, but a rectangular or round-bottom test tube type wave-transmitting element is adopted, a microwave excitation device cannot be formed, and therefore microwave excitation and microwave conduction direction control cannot be effectively achieved.
The inner diameter of the circular tube 3 is 5-50mm, preferably 5-30mm, and more preferably 10-20 mm. The waveguide 9 of patent application No. 200610046206.3 has a rectangular cross section of 90 × 45mm, and is equipped with a pressure-bearing glass having a diameter of 120 mm. Meanwhile, due to the rectangular holes, the stress at the right-angle position is easy to concentrate. The aperture of the through hole 5 of patent application No. 201410471231.0 is 20mm-30mm, which is much higher than the sectional dimension of the present application. The smaller the cross-sectional area of the circular tube 3 is, the stronger the pressure-bearing capacity is. Although the round tube has a small size, the horn 20 and the coaxial resonant cavity 8 which are arranged in the reaction device are matched and combined into a microwave excitation cavity according to a certain size, so that the microwave can be effectively transmitted and controlled, meanwhile, a microwave feed point is moved into the reaction device, and the microwave can penetrate to a more central position of a reaction system. More uniform heating of the reaction system is realized, and the promotion influence of the microwave on the reaction is strengthened.
The wavelength of the microwave is 12.24cm at the frequency of 2.45GHz, and the length of the round tube 3 is 1/4-1/2 cm, preferably 3.06-6.12 cm. The cone height of the loudspeaker 20 is 10-100 mm, the caliber is 45-180 mm, the preferred cone height is 20-50 mm, and the caliber is 60-140 mm. In the design specification of the pressing force container, in the implementation process of the technology of patent application No. 200610046206.3, the reaction device with the diameter of 350mm is difficult to realize rectangular openings of 90 × 45mm at 2 and more than 2 positions at the same latitude. Meanwhile, the phi 120mm pressure-bearing glass allows the use of the reaction device to be no more than 2.5 mpa. In patent application No. 201410471231, for example, in high voltage equipment, the thickness of the fixed flange surface of the pressure-bearing part and the thickness of the kettle wall need to be more than 10mm, the length of the microwave magnetron antenna is generally between 25-50mm, and in the structure, the exposed length of the antenna and the inner wall of the pressure-resistant waveguide are difficult to form an effective microwave resonant cavity; meanwhile, when microwave conduction is carried out at the rear end of the waveguide, BJ26 (rectangular waveguide, size 86.3X 43.2mm) or BY22 (circular waveguide, size phi 97.9mm) or more is also needed. Taking the reaction kettle body with the diameter of 350mm as an example, the rectangular openings of 90 × 45mm at 2 and more than 2 positions are difficult to realize at the same latitude of the structure. In the application, if 10-20mm circular holes are used for feeding microwaves, 4 or more than 4 microwave feeding holes can be easily formed in the same latitude without influencing the stress of the reaction device. Meanwhile, the small-size hole is formed, and the processing is simpler and more convenient. The bearing plate is internally arranged, the wave-transmitting fixing piece 4 does not need to be stressed, and compared with the two patents, the fixing piece is simpler and more convenient to process, less in used materials and lighter in weight.
The material of the cone bearing part 5 is at least one of polytetrafluoroethylene, quartz glass, high-purity alumina, high borosilicate glass and PEEK plastic.
Different materials of the cone bearing piece 5 can be selected according to different requirements, so that the bearing capacity of the cone bearing piece 5 is ensured. The material of the cone bearing part 5 can adopt one type of material or adopt a plurality of types of materials to be mutually overlapped.
When quartz glass, high-purity alumina, high borosilicate glass and other materials are used as the material of the cone bearing part 5, a sealing gasket which plays a role in stress buffering is arranged between the cone bearing part 5 and the inner wall of the horn 20 and between the cone bearing part 5 and the wave-transmitting fixing part 4. The material of the sealing gasket 6 is at least one of polytetrafluoroethylene, fluororubber and nitrile rubber.
The wave-transparent fixing piece 4 is a hollow metal flange or a flat plate made of wave-transparent material.
The edge of the horn 20 is provided with a linking flange surface, the cone bearing part 5 is fixed in the horn 20 by linking with the hollow metal flange, the sealing gasket 6 plays a role in sealing and stress buffering, and the hollow metal flange can effectively penetrate through microwaves while fixing the cone bearing part 5.
The microwave generating devices 9 are uniformly arranged on the annular reaction device 1.
The penetration depth of the microwave serving as an energy wave for heating is always a main problem restricting the amplification production of the microwave, the effective penetration depth of the microwave is 3-8cm in the general aqueous reaction liquid, and according to the wave absorbing capacity and the handling capacity of materials, a plurality of microwave generating devices 9 are required to be uniformly arranged on the annular reaction device 1 to realize the uniform energy feedback of the microwave pressure sintering furnace. Because of using this microwave generating device 9, annular reaction unit 1 and pipe 3 welded fastening, the internal diameter of pipe can be as little as 5-30mm, very big improvement annular reaction unit 1 and microwave generating device 9's bearing capacity, even set up a plurality of microwave generating device 9 on annular reaction unit 1, can not increase the degree of difficulty of pressure design and processing of microwave pressure fritting furnace yet, equipment can allow to use to higher pressure environment simultaneously. Meanwhile, the microwave feed point is moved into the reaction device, the microwave can penetrate to the more central position of the reaction system, the influence of weakened reaction effect caused by the penetration depth of the microwave is reduced, and the reaction device with larger size can be arranged in the same reaction system, so that the amplification production is facilitated.
The microwave generating devices 9 used in the invention are more in number, and when a high-pressure environment is required, higher requirements are provided for the pressure bearing capacity of the microwave generating devices, and the pressure bearing capacity of the microwave generating devices 9 can be improved by adopting the microwave generating devices 9.
The annular reaction device 1 is provided with a safety valve 12, a pressure measuring device 13 and a temperature measuring device 15. The annular reaction device 1 is also externally provided with a controller for controlling the temperature and pressure in the annular reaction device 1.
The annular reaction device 1 is also provided with a liquid inlet 16 and a liquid outlet 17 for feeding and discharging liquid into and from the annular reaction device 1.
The pressure measuring device 13 is used for detecting and controlling the pressure of the microwave pressure sintering furnace during operation, and because the pressure sensor can be interfered by microwaves, a wave suppression device is required to be arranged at the pressure detection position, the wave suppression device can be a metal plate with single holes or densely distributed round small holes to ensure the accuracy of pressure detection, and the pressure measuring device 13 is connected with a controller.
The temperature measuring device 15 is used for detecting and controlling the temperature of the microwave pressure sintering furnace during working, the temperature measuring device 15 can adopt galvanic couple temperature measurement or infrared temperature measurement, the temperature measuring device 15 is connected with the controller, the temperature measuring device 15 sends a detection control signal to the controller, the controller controls the feed-in microwave power of the magnetron 2 of the microwave generating device 9 to realize temperature control, and multipoint combined temperature measurement and control can be adopted to ensure the uniformity of a temperature field.
In order to ensure safety, a safety valve 12 is arranged on the annular reaction device 1, and when the pressure exceeds the designed pressure, the safety valve 12 automatically pops open.
The following test table is obtained by comparing the pressure resistance, heating and other performances by adopting devices with the same microwave frequency, the same size and the like but different pressure-bearing devices.
TABLE 1 Performance test Table for reaction apparatus of phi 350mm
Figure GDA0002826961060000071
It can be seen from table 1 that, for reaction devices with the same diameter, the pressure-bearing structure of the present invention can significantly reduce the thickness of the pressure-bearing portion and increase the maximum allowable pressure, and the number of microwave generation devices arranged at the same latitude is larger, so that the heating uniformity of the reaction substance can be improved.

Claims (9)

1. The microwave high-pressure annular reaction device is characterized by comprising an annular reaction device (1), a microwave generating device (9), a liquid distributor (10), a liquid inlet (16) and a liquid outlet (17), wherein the annular reaction device (1) comprises an outer pipe (101) and an inner pipe (102) sleeved in the outer pipe (101), a space between the outer pipe (101) and the inner pipe (102) forms an annular reaction channel (14), the microwave generating device (9) is arranged on the outer surfaces of the outer pipe (101) and the inner pipe (102), the liquid distributor (10) is perpendicular to the annular reaction channel (14), the microwave generating device (9) arranged on the outer pipe (101) and the microwave generating device (9) arranged on the inner pipe (102) are arranged in a staggered mode;
the microwave generating device (9) comprises a magnetron (2) and a microwave excitation feed-in pressure-bearing device;
the microwave excitation feed-in pressure-bearing device comprises a circular tube (3) arranged on the annular reaction device (1), a loudspeaker (20) positioned in the annular reaction device (1), a cone pressure-bearing piece (5) positioned in the loudspeaker (20) and a wave-transmitting fixing piece (4) for limiting the movement of the cone pressure-bearing piece (5);
the antenna (7) of the magnetron (2) is positioned in the circular tube (3), and the antenna (7) and the circular tube (3) form a coaxial resonant cavity (8).
2. A microwave high-pressure annular reactor according to claim 1, characterized in that a reinforcing rib (11) is installed between the outer pipe (101) and the inner pipe (102).
3. The microwave high-pressure annular reaction device according to claim 1 or 2, characterized in that the annular reaction device (1) is further provided with a safety valve (12), a pressure measuring device (13) and a temperature measuring device (15).
4. A microwave high-pressure annular reactor according to claim 1, characterized in that the inner diameter of the circular tube (3) is 5-30mm, and the length of the circular tube (3) is 1/4-1/2 for transmitting microwave wavelength.
5. The microwave high-pressure annular reaction device according to claim 1, wherein the conical height of the horn (20) is 10-100 mm, and the caliber is 45-180 mm.
6. The microwave high-pressure annular reaction device according to claim 1, wherein the cone height of the horn (20) is 20-50 mm, and the caliber is 60-140 mm.
7. A microwave high-pressure annular reaction device according to claim 1, 4, 5 or 6, characterized in that the material of the conical bearing part (5) is at least one of Teflon, quartz glass, high-purity alumina, high-borosilicate glass, PEEK plastic.
8. A microwave high-pressure annular reaction device according to claim 1, 4, 5 or 6, characterized in that a sealing gasket (6) is arranged between the cone pressure-bearing piece (5) and the inner wall of the horn (20), and a sealing gasket (6) is arranged between the cone pressure-bearing piece (5) and the wave-transparent fixing piece (4).
9. The microwave high-pressure annular reaction device according to claim 1, 4, 5 or 6, wherein the wave-transparent fixing member (4) is a hollow metal flange or a flat plate made of wave-transparent material.
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