CN102773055B - Microwave heating device and application thereof - Google Patents
Microwave heating device and application thereof Download PDFInfo
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- CN102773055B CN102773055B CN201210160686.1A CN201210160686A CN102773055B CN 102773055 B CN102773055 B CN 102773055B CN 201210160686 A CN201210160686 A CN 201210160686A CN 102773055 B CN102773055 B CN 102773055B
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Abstract
The invention provides a microwave heating device and an application thereof, wherein the device comprises a microwave reactor and a microwave generation and transmission device, the microwave generation and transmission device comprises a microwave source, a circulator, a water load, a directional coupler, an automatic tri-dowel regulator and a waveguide according to a microwave transmission sequence, in the waveguide section, a mode of converting a rectangular wave guide into coaxial transmission is adopted, and a probe enters the center of the reactor from the side wall of the microwave reactor for guiding the microwave into the reactor. According to the device, microwaves in the reactor are uniformly distributed; and moreover, the device has good sealing performance, can be practically applied for any reaction which utilizes microwave to heat, such as an application of continuous oil product hydrodesulfurization, technological conditions can be alleviated, the oil product desulfurization degree is effectively improved, and the oil refining economical efficiency is improved.
Description
Technical field
The invention relates to a kind of microwave heating equipment and application thereof, refer to especially and a kind ofly utilize the chemical reaction equipment of heating using microwave and the application of this device.
Background technology
Microwave has the obvious characteristics such as wavelength short (1m ~ 1mm), frequency high (300MHz ~ 300GHz), Quantum Properties.The general principle of heating using microwave is conduction and the dielectric polarization of charged particle.Ionic conduction refers to that the ion in medium produces transference cell at elect magnetic field and produces heat.Dielectric polarization mechanism refers under electromagnetic field effect, and polar molecule is from the polar alignment orientation of random distribution state shift foundation electromagnetic field.Under the effect of microwave high-frequency electromagnetic field, these orientation movements agree to the frequency of alternating electromagnetism constantly to change, and cause strenuous exercise and the collision friction of molecule, thus produce heat, cause electric field energy to be converted into heat energy in medium.Nonpolar molecule is evenly distributed then not by heating using microwave due to internal charge.Heating using microwave has the feature of penetrability, instantaneity and selective heating, and thermal loss is little, easy to operate, sanitation and hygiene are pollution-free, is used widely in life is produced.
Traditional microwave heating technique is mainly used for heated food, and in recent years, along with the development of microwave heating technique, the report be applied to by microwave heating technique on chemical engineering industry is increasing.
The microwave heating equipment reported at present is utilize a closed cavity as microwave heating chamber mostly, microwave source directly can be positioned on heating chamber wall, or offer waveguide mouth on heating chamber wall, and microwave passes through waveguide mouth to heating intracavitary irradiation.In general, adopt this microwave by the mode of heating chamber perisporium to intracavitary irradiation, in chamber, microwave field distribution is more uneven, and centre is the strongest, weak on limit, substantially in Sine distribution.Microwave field distribution in addition in microwave heating chamber be also input to the mode of this cavity with microwave and position directly related, these two factors also can cause the inhomogeneities of microwave field distribution in heating chamber usually.This inhomogeneities makes microwave heating technique be limited by very large in the chemical industry application needing to carry out homogeneous heating or needs strict control reaction temperature.
CN 101473692A disclose a kind of can normally homogeneous heating heating clamber whole inside and realize as required concentration of local heating microwave heating equipment.Wherein mainly utilize at least one rotable antenna, control rotable antenna by control device, be oriented with the part making it have high radiation directivity on the direction determined towards the testing result according to temperature distributing detecting device to heat object.
CN 1826026A discloses a kind of microwave heating equipment of homogeneous radiation, wherein that microwave is transmitted by waveguide impedance transformer, and outwards output to corresponding coupler from waveguide mouth, after reflect/scatter, to heating chamber, export multiple microbeam equably from multiple coupling apertures of a coupler sidewall, thus microwave energy problem pockety in heating chamber can be improved without the need to rotary device.
Above-mentioned microwave heating equipment, although can improve microwave field distribution problem of non-uniform in microwave cavity to a certain extent, improve limitation, and above-mentioned microwave heating equipment mainly heats to food, for needing the chemical process of heating using microwave and inapplicable.
WO 2009/064501 discloses a kind of oil desulfurization technology of microwave assisted, wherein utilize a box-type heating using microwave reactor/microwave cavity (microwave equipment of CEM company and the household microwave oven of improvement), under pressurized hydrogen exists, irradiate crude oil and catalyst with microwave energy, carry out hydrodesulfurization reaction.But, there is following problem in this technology: wherein record crude oil and catalyst is mixed by the mode of stirring, but be in fact difficult in described cavity oil, gas and catalyst mix is even, be thisly blended in actual mechanical process also easy blocking pipe; In the method, after hydrodesulfurization reaction completes, need catalyst to be separated with crude oil, by gravitational settling or filtration, complex operation; In addition, described microwave device is batch reactor, and donor has a lot of restrictions.
CN 101560407A discloses a kind of oil liquefied gas or gasoline desulphurization microwave reaction kettle, and its structure has microwave source, micro-wave coupler, tuner, transition waceguide, ventilation safety isolator, isolation window and reaction cavity by microwave transmission order; Reaction cavity, is closed near the cylinder termination of feeding mouth respectively with the cylindrical vessel of feeding mouth and discharging opening in the side by two ends, is connected through isolation window near the cylinder termination of discharging opening with sealing ring with ventilation safety isolator seal; Described ventilation safety isolator is one section of circular waveguide, its side opening air vent.That rectangular waveguide is converted to cylindrical waveguide in the document, then by window microwave burst into.Wherein reached by perforate on safety barrier and avoid the object of combustible gas leakage (be actually and distributed by this some holes by the gas of leakage), but, how to prevent hydrogen or combustible oil gas from not entering, the document is not made and being clearly demonstrated, and the leakage of hydrogen is absolute prohibition for oil hydrogenation reaction, there is potential safety hazard.
In sum, the microwave heating equipment of above-mentioned prior art report is difficult to the industrial production being applied to scale, more can not be used for the chemical reaction process realizing needing reactant continous way input and output microwave heating chamber.
Summary of the invention
One object of the present invention is, for above-mentioned prior art microwave heating equipment Problems existing, to provide a kind of microwave heating equipment, and in microwave cavity, microwave field distribution is even, and conscientiously can be applied to the chemical process of scale, and improves processing safety.
Another object of the present invention is to the application that described microwave heating equipment is provided.
For reaching above-mentioned purpose, the invention provides a kind of microwave heating equipment, this device comprises:
Microwave reactor; And
Microwave occurs and transmitting device, this microwave occurs and transmitting device comprises by microwave transmission order: microwave source, circulator, water load, directional coupler, three pin automatic regulator and waveguides, at waveguide segment, rectangular waveguide is adopted to be converted into the form of coaxial transmission, probe into reactor central authorities with a probe from microwave reactor sidewall, and microwave is burst in reactor.That is, be that microwave cavity is done reactor in the present invention.
According to specific embodiment of the invention scheme, in microwave heating equipment of the present invention, the material of described microwave reactor can be any one or alloy in stainless steel, copper, silver or aluminium, such as, high-temperature high-pressure reaction kettle transformation conventional in chemical process can be adopted to form.
In the present invention, the place that described probe probes into reactor should adopt not absorbing material to seal.Such as, in a detailed description of the invention of the present invention, by probe, the probe segment cover probeed in reactor cavity gets up and seals the place that probe on reactor wall probes into the hat shape cover body (or being called ceramic cap, glass cap) adopting not absorbing material to make as pottery, lucite, quartz glass etc.The mode of sealing can be adopt the various sealing means in affiliated field, such as, adopt flange seal and/or welded seal etc.
According to specific embodiment of the invention scheme, the described probe length probeed in reactor cavity is generally the middle position to reactor cavity, and microwave is dispersed in cavity from middle position.
Microwave heating equipment of the present invention, even microwave distribution in microwave cavity, and device good airproof performance, can conscientiously be applied to device of the present invention the chemical process needing heating using microwave, can relax process conditions, improves economy.
In a specific embodiment of the present invention, microwave heating equipment provided by the present invention is the device for the desulfurization of continuous-type microwave oil hydrogenation, wherein, described microwave reactor is the fixed bed reactors for completing microwave desulphurization reaction, this reactor is provided with reactant entrance and product exit, can be connected with the after-treatment system of product with the heater of oil product raw material respectively.
According to specific embodiment of the invention scheme, microwave heating equipment of the present invention, also can comprise further:
Superpressure parking auto-controller, it comprises electro connecting pressure gauge and relay, when pressure exceedes setup pressure value in reactor cavity, automatically can cut off microwave power supply.This superpressure parking auto-controller also can control preheating current source, pumping source etc. as the case may be, the supply of donor can also be controlled further on the basis being equipped with magnet-controlled valve, such as oil hydrogenation desulphurization reaction, the supply of hydrogen can be cut off when reactor pressure exceedes setup pressure value.
It should be noted that, microwave heating equipment of the present invention is not limited to the hydrodesulfurization reaction being applied to oil product, but any high-temperature high-voltage reaction can be applied to, reaction temperature (in the temperature range that reactor material such as stainless steel bears), reaction pressure can reach 10MPa through pressure measurement up to 800 DEG C.
That is, on the other hand, present invention also offers described microwave device in the application for realizing utilizing microwave to carry out in the reaction of heating.
Particularly, the described reaction utilizing microwave to carry out heating can be any high-temperature high-voltage reaction in reaction unit material tolerance range, such as, can be that temperature is less than or equal to 800 DEG C, pressure is less than or equal to the reaction of 10MPa.
Utilize microwave heating equipment of the present invention, the continuous high-temperature reaction under high pressure under microwave field effect can be realized.Such as, in a specific embodiments of the present invention, be used for by described microwave device realizing continous way oil hydrogenation sulfur method, the method comprises:
Stage casing filling immobilization Hydrobon catalyst in reactor cavity;
Oil product raw material is mixed with hydrogen, is conveyed into described fixed bed reactors continuously, make oil product raw material contact with Hydrobon catalyst and under microwave action, hydrodesulfurization reaction occur; More specifically, due to microwave action, reaction condition can relax compared with traditional operation condition, such as, when carrying out oil product of gasoline hydrodesulfurization reaction under microwave action, the reaction condition that can control in reactor is: reaction temperature 220 ~ 280 DEG C, operating pressure 1.5 ~ 2.5MPa, weight (hourly) space velocity (WHSV) 1 ~ 4h
-1, hydrogen to oil volume ratio 100: 1 ~ 400: 1, microwave power 1.2 ~ 2.2kW;
The product of above-mentioned hydrodesulfurization reaction is drawn reactor continuously and carries out post processing.
According to specific embodiment of the invention scheme, described catalyst is seated in around probe.
In the present invention, the device structure do not mentioned in detail can with reference to the legacy equipment in affiliated field.Such as, described reactor can be traditional industrial high temperature autoclave, and key of the present invention is the probe introducing microwave device at reactor-side wall opening, thus microwave is introduced this reactor cavity; The microwave source of described microwave generating apparatus, circulator, water load, directional coupler, three pin automatic regulators and waveguide etc. also can conventionally in the component of microwave generating apparatus design, key of the present invention is that at waveguide segment be the form adopting rectangular waveguide to be converted into coaxial transmission, probe into reactor cavity central authorities with a probe from sidewall of reactor, and microwave is introduced reactor cavity.Superpressure parking auto-controller used in the present invention, the product after-treatment system etc. of hydrodesulfurizationsystem system all can adopt the conventional equipment in affiliated field.
In sum, the invention provides a kind of microwave heating equipment and application thereof, pass through coaxial transmission, the mode of probe is adopted to be introduced by microwave, microwave technology can be applied to conscientiously the chemical reaction needing heating using microwave, can process conditions be relaxed, and in device microwave cavity, microwave field distribution is even, good airproof performance, processing safety is good.
Accompanying drawing explanation
Fig. 1 is the structural representation of microwave heating equipment of the present invention.Wherein: 1-microwave source, 2-circulator, 3-water load, 4-directional coupler, 5-tri-pin automatic regulator, 6-waveguide, 7-reactor.
Fig. 2 is the structural representation that microwave device middle probe of the present invention probes into reactor part.Wherein, 61-rectangular waveguide, 62-coaxial waveguide, 621-coaxial waveguide shell, 622-probe, 623-ceramic cap.
Fig. 3 is the process chart utilizing microwave device of the present invention to carry out oil hydrogenation sulfur method.Wherein: 8-superpressure parking auto-controller, 9-condenser, 10-high-pressure separator, 11-low pressure separator, 12-counterbalance valve, 13-device for absorbing tail gas.
Fig. 4 is the distribution map of the electric field according to beds in a specific embodiment applied microwave heater timer of the present invention.Wherein picture A is overall diagram, and picture B, C, D are the profile of X-direction, Y-direction and Z-direction respectively.Also the uniformity of microwave field distribution can be found out from figure.
Detailed description of the invention
Describe the beneficial effect of implementation process of the present invention and generation below by way of specific embodiment in detail, be intended to help reader to understand essence of the present invention and feature better, not as can the restriction of practical range to this case.
Shown in Figure 1, microwave heating equipment of the present invention comprises microwave source 1, circulator 2, water load 3, directional coupler 4, three pin automatic regulator 5, waveguide 6 by microwave transmission order; And microwave reactor 7.The detailed construction of waveguide segment part shown in Figure 2 again, wherein, waveguide 6 comprises rectangular waveguide 61 and coaxial waveguide 62, coaxial waveguide 62 comprises metal shell 621 (cylindrical shape) and the probe 622 (elongated is cylindrical) of coaxial setting, rectangular waveguide is adopted to be converted into the form of coaxial transmission, probe into reactor cavity central authorities with probe 622 from reactor 7 sidewall, and microwave is introduced reactor cavity (that is, microwave cavity being done reactor).This reactor material is stainless steel, can resistance to higher temperature (temperature can bear within scope at stainless steel), and pressure depends on the thickness of reactor wall metal.In sealing place of probe and reactor, ceramic cap and ring flange can be made of one, and then fixing with flange (namely adopting the form of three flanges) sealing of both sides in figure; Also pottery directly can be welded or be bonded on leftmost ring flange, be undertaken sealing (as shown in Figure 2) by two flanges.Ceramic cap itself does not affect microwave distribution, and its gauge can tolerate operating pressure.
Shown in Figure 3, in this embodiment, that microwave heating equipment of the present invention is used for oil hydrogenation desulfurization, wherein, microwave reactor 7 is used as hydrodesulphurisatioreactors reactors, and this system being used for oil hydrogenation desulfurization also comprises: the after-treatment system (condenser 9, high-pressure separator 10, low pressure separator 11, counterbalance valve 12, device for absorbing tail gas 13 etc.) of superpressure parking auto-controller 8 and product.
Wherein, superpressure parking auto-controller 8 is safety control device, form primarily of the parts such as electro connecting pressure gauge and relay, when pressure exceedes setup pressure value, can automatically cut off microwave power supply, preheating current source, pumping source, the basis being equipped with magnet-controlled valve can cut off the supply of hydrogen, and therefore this auto-controller greatly enhances the security of experimental implementation.
When utilizing this device to carry out continuous-type microwave oil hydrogenation desulphurization reaction, concrete operation step is:
(1) loading catalyst:
Beds filler order is successively: quartzy silk floss → porcelain ball → quartzy silk floss → quartz sand → quartzy silk floss → catalyst → quartzy silk floss → quartz sand → quartz is continuous, after closely knit, fill red copper pad and tightens ring flange.
(2) air-tightness is checked:
Reactor is accessed hydrogenation micro-reactor, then open the hydrogen valve on panel, mass flowmenter protective valve is closed, opens cleaning valve and lead to H2, regulate pressure-reducing valve and counterbalance valve to reaction pressure, check whether whole gas circuit leaks gas with fuel gas leak detector.
(3) presulfiding of catalyst:
In pre-vulcanization process, the valve in the middle of high-low pressure knockout drum should be closed in time, bleed off the liquid in low pressure separation pot; After presulfurization terminates, progressively lower the temperature, close pump, close hydrogen, mass flowmenter protective valve is closed, then slowly opens atmospheric valve, whole device pressure release.Open cleaning valve, then atmospheric valve cuts out, flushing line 3-5 time repeatedly, drain carbon disulfide residual in pipeline.
(4) hydrodesulfurization reaction:
Open circulator bath, open hydrogen valve and regulate whole device pressure.During lower than operating temperature 20 DEG C of question response device thermometric display, open gasoline sampling valve, start oil pump, be adjusted to required flow; Open microwave, be adjusted to test power demand.When thermometric display instrument display operating temperature, start timing, balance 7 hours, then close the valve sampling in the middle of high and low pressure knockout drum.Once, till seeing gas in sampling process, action is wanted rapidly, to get 2 times altogether in sampling in every 1 hour later.Experimental session record reactor outlet, microwave reflection power etc., after reaction terminates, termination of pumping, closes hydrogen valve, closes microwave, closes power supply.
Embodiment 1
Select Co-Mo/ γ-Al
2o
3the catalytically cracked gasoline of catalyst and certain oil plant, wherein total sulfur content is 340ppm, and sulfur compound is mainly: thiophene, C1 thiophene, C2 thiophene and C3 thiophene etc.At weight (hourly) space velocity (WHSV) 2h
-1, reaction pressure 2MPa, reaction temperature 250 DEG C, hydrogen-oil ratio 200: 1.Having investigated respectively has microwave action (1.2kW) and without HDS situation during microwave action.When found that microwave, desulfurization degree is 78.2%, and without being 52.6% during microwave, as can be seen here, under identical operating conditions, the existence of microwave field can significantly improve FCC gasoline hydrodesulfurization rate.The further research of FCC gasoline hydrodesulfurization is shown, when having microwave to exist, hydrogenation of olefins degree is lower, the effect of this selective heating of microwave just, Just because of this, after hydrodesulfurization, research finds that its octane number does not only reduce, and increases a unit (the hydrodesulfurization octane number without microwave action is 93.5, and microwave sulfur removal technology is 94.6) on the contrary.
Fig. 4 shows the distribution map of the electric field of beds in device in above-mentioned course of reaction.Wherein picture A is overall diagram, and picture B, C, D are the profile of X-direction, Y-direction and Z-direction respectively.From figure, also can find out that microwave distribution is uniform, and produce without microwave leakage situation, handling safety is reliable.
Claims (7)
1. can realize a microwave heating equipment for the continuous high-temperature reaction under high pressure under microwave field effect, this device comprises:
Microwave reactor; Described microwave reactor is the fixed bed reactors for completing heating using microwave reaction, and this reactor is provided with reactant entrance and product exit; And
Microwave occurs and transmitting device, this microwave occurs and transmitting device comprises by microwave transmission order: microwave source, circulator, water load, directional coupler, three pin automatic regulator and waveguides, at waveguide segment, rectangular waveguide is adopted to be converted into the form of coaxial transmission, probe into reactor central authorities with a probe from microwave reactor sidewall, and microwave is burst in reactor; Further, wherein, the hat shape cover body probe segment cover probeed into by probe in reactor cavity adopting not absorbing material to make gets up and seals the place that probe on reactor wall probes into.
2. microwave heating equipment according to claim 1, wherein, the material of described microwave reactor is any one or alloy in stainless steel, copper, silver or aluminium, and described not absorbing material is pottery, lucite or quartz glass.
3. microwave heating equipment according to claim 1, this device also comprises:
Superpressure parking auto-controller, it comprises electro connecting pressure gauge and relay, when reactor pressure exceedes setup pressure value, automatically can cut off microwave power supply.
4. the microwave heating equipment described in any one of claims 1 to 3 is in the application for realizing utilizing microwave to carry out in the reaction of heating.
5. application according to claim 4, wherein, the described reaction utilizing microwave to carry out heating for temperature be less than or equal to 800 DEG C, pressure is less than or equal to the reaction of 10MPa.
6. application according to claim 4, wherein, be used for by described microwave device realizing continous way oil hydrogenation sulfur method, the method comprises:
Stage casing filling immobilization Hydrobon catalyst in reactor;
Oil product raw material is mixed with hydrogen, is conveyed into described fixed bed reactors continuously, make oil product raw material contact with Hydrobon catalyst and under microwave action, hydrodesulfurization reaction occur;
The product of above-mentioned hydrodesulfurization reaction is drawn reactor continuously and carries out post processing.
7. application according to claim 6, wherein, described Catalyst packing is around probe.
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| CN201210160686.1A CN102773055B (en) | 2012-05-22 | 2012-05-22 | Microwave heating device and application thereof |
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| CN102773055B true CN102773055B (en) | 2015-01-07 |
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| CN106374178A (en) * | 2016-09-29 | 2017-02-01 | 南京三乐微波技术发展有限公司 | Self-adaptive matching device and control method for microwave equipment |
| CN111033889B (en) * | 2018-04-20 | 2021-10-08 | 松下知识产权经营株式会社 | Directional coupler and microwave heating device with same |
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| CN109092227B (en) * | 2018-08-30 | 2021-06-29 | 长沙新材料产业研究院有限公司 | MPCVD synthesis equipment and control method |
| CN109092226B (en) * | 2018-08-30 | 2021-05-14 | 长沙新材料产业研究院有限公司 | Microwave reflection adjusting device and control method for MPCVD synthesis equipment |
| CN110215946A (en) * | 2019-05-29 | 2019-09-10 | 西南大学 | A kind of novel metal test tube device for microwave heating |
| CN113483570A (en) * | 2021-05-25 | 2021-10-08 | 中国工程物理研究院应用电子学研究所 | Vacuum microwave smelting device |
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| CN1533831A (en) * | 2004-03-09 | 2004-10-06 | 四川大学 | Multimagnetron microwave chemical reactor |
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| CN202921297U (en) * | 2012-08-31 | 2013-05-08 | 中国石油大学(北京) | Microwave heating device |
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| CN1533831A (en) * | 2004-03-09 | 2004-10-06 | 四川大学 | Multimagnetron microwave chemical reactor |
| CN101560407A (en) * | 2009-06-04 | 2009-10-21 | 吉林大学 | Liquefied petroleum gas or gasoline desulphurization microwave reaction kettle |
| CN202921297U (en) * | 2012-08-31 | 2013-05-08 | 中国石油大学(北京) | Microwave heating device |
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