CN102773055A - Microwave heating device and application thereof - Google Patents
Microwave heating device and application thereof Download PDFInfo
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- CN102773055A CN102773055A CN2012101606861A CN201210160686A CN102773055A CN 102773055 A CN102773055 A CN 102773055A CN 2012101606861 A CN2012101606861 A CN 2012101606861A CN 201210160686 A CN201210160686 A CN 201210160686A CN 102773055 A CN102773055 A CN 102773055A
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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, be meant a kind of application that utilizes chemical reaction equipment and this device of heating using microwave especially.
Background technology
Microwave has the short (high (obvious characteristics such as 300MHz～300GHz), Quantum Properties of 1m～1mm), frequency of wavelength.The basic principle of heating using microwave is the conduction and the dielectric polarization of charged particle.Ionic conduction is meant that the ion in the medium produces transference cell and produces heat in electromagnetic field.Dielectric polarization mechanism is meant that under electromagnetic field effect polar molecule is from the polarity oriented of random distribution state shift according to 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 the strenuous exercise and the collision friction of molecule, thereby produce heat, cause electric field energy to be converted into the heat energy in the medium.Nonpolar molecule is evenly distributed then not by heating using microwave owing to internal charge.Heating using microwave has the characteristics of penetrability, instantaneity and selectivity heating, and thermal loss is little, easy to operate, sanitation and hygiene are pollution-free, in life is produced, is used widely.
Traditional microwave heating technique mainly is to be used for heated food, and is in recent years, along with the development of microwave heating technique, that the report that microwave heating technique is applied on the chemical engineering industry is increasing.
The microwave heating equipment of being reported at present is to utilize a closed cavity as microwave heating chamber mostly, can microwave source directly be positioned on the heating chamber wall, or on the heating chamber wall, offer the waveguide mouth, microwave through the waveguide mouth to heating intracavitary irradiation.In general, adopt this microwave through the heating chamber perisporium to the mode of intracavitary irradiation, in the chamber in the microwave field distribution more inhomogeneous, the centre is the strongest, on the limit a little less than, be Sine distribution basically.Microwave field in the microwave heating chamber distributes also in addition and to be input to mode and the position of this cavity directly related for microwave, and these two factors also can cause the inhomogeneities of microwave field distribution in the heating chamber usually.This inhomogeneities makes microwave heating technique evenly heat or need strictness to control in the chemical industry application of reaction temperature at needs and has received very big restriction.
CN 101473692A discloses a kind of microwave heating equipment that can normally evenly heat the whole inside of heating clamber and realize the concentration of local heating as required.Wherein mainly be to utilize at least one rotable antenna, through control device control rotable antenna so that its part with high radiation directivity be oriented towards according to the testing result of temperature distributing detecting device and on definite direction so that object is heated.
CN 1826026A discloses a kind of microwave heating equipment of homogeneous radiation; Wherein be that microwave is transmitted by waveguide impedance transformer; And outwards output to the corresponding coupler from the waveguide mouth; Be reflected/scattering after, from a plurality of coupling apertures of a sidewall of coupler a plurality of microbeams of output to heating chamber equably, can improve microwave energy problem pockety in the heating chamber thereby need not rotary device.
Above-mentioned microwave heating equipment, although can improve microwave field skewness problem in the microwave cavity to a certain extent, the improvement degree is limited, and above-mentioned microwave heating equipment mainly is that food is heated, for the chemical process that needs heating using microwave and inapplicable.
WO 2009/064501 discloses the oil desulfurization technology that a kind of microwave promotes; Wherein be to utilize a box-type heating using microwave reactor/microwave cavity (microwave equipment of CEM company and improved household microwave oven); In the presence of pressurized hydrogen; With microwave energy irradiation crude oil and catalyst, carry out hydrodesulfurization reaction.Yet; There is following problem in this technology: wherein record is through the mode that stirs crude oil and catalyst to be mixed; But in fact be difficult in the described cavity oil, gas and catalyst mix is even, this also easy blocking pipeline that is blended in the actual mechanical process; In this method, after accomplishing, hydrodesulfurization reaction needs catalyst is separated with crude oil, through gravitational settling or filtration, complex operation; In addition, described microwave device is a batch reactor, supplies with body and 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, isolates window and reaction cavity by the microwave conduction sequence; Reaction cavity has the cylindrical vessel of feeding mouth and discharging opening respectively in the side of leaning on two ends, near the cylinder termination sealing of feeding mouth, be connected with the ventilation safety isolator seal with sealing ring through the isolation window near the cylinder termination of discharging opening; Described ventilation safety isolator is one section circular waveguide, and air vent is opened in its side.Be to convert rectangular waveguide into cylindrical waveguide in the document, then through window with microwave burst into.Wherein reach the purpose (be actually the gas that leaks is distributed through these holes) of avoiding combustible gas leakage through perforate on the safety isolator; Yet; How to prevent that but hydrogen or fuel vapor from not getting into; The document is not made and being clearly demonstrated, and the leakage of hydrogen is an absolute prohibition for the oil hydrogenation reaction, has potential safety hazard.
In sum, the microwave heating equipment of above-mentioned prior art report is difficult to be applied to the commercial production of scale, more can not be used to needing to realize the chemical reaction process of reactant continous way input and output microwave heating chamber.
Summary of the invention
One object of the present invention is to the problem of above-mentioned prior art microwave heating equipment existence a kind of microwave heating equipment to be provided, and microwave field is evenly distributed in the microwave cavity, and can be applied to the chemical process of scale conscientiously, and improves processing safety.
Another object of the present invention is to provide the application of said microwave heating equipment.
For reaching above-mentioned purpose, the invention provides a kind of microwave heating equipment, this device comprises:
Microwave reactor; And
Microwave takes place and transmitting device; This microwave takes place and transmitting device comprises by the microwave conduction sequence: microwave source, circulator, water load, directional coupler, three pin automatic regulator and waveguides; At waveguide segment; Adopt rectangular waveguide to be converted into the form of coaxial transmission, probe into reactor central authorities from the microwave reactor sidewall, and microwave is burst in the reactor with a probe.That is be that microwave cavity is done reactor among the present invention.
According to specific embodiments of the present invention, in the microwave heating equipment of the present invention, the material of said microwave reactor can be any or the alloy in stainless steel, copper, silver or the aluminium, for example can adopt high-temperature high-pressure reaction kettle transformation commonly used in the chemical process to form.
Among the present invention, the place that said probe probes into reactor should adopt not that absorbing material seals.For example; In a specific embodiment of the present invention, adopt cap shape cover body (or being called ceramic cap, glass cap) that absorbing material not processes like pottery, lucite, quartz glass etc. that probe is probeed into probe segment cover in the reactor cavity and get up and the place that probe on the reactor wall probes into is sealed.The mode of sealing can be the various sealing means in the field under adopting, and for example adopts flange seal and/or welded seal etc.
According to specific embodiments of the present invention, the length that said probe probes in the reactor cavity generally is the middle position to reactor cavity, and microwave is dispersed in cavity from middle position.
Even microwave distribution in the microwave heating equipment of the present invention, microwave cavity, and install good airproof performance, can device of the present invention need be applied to conscientiously the chemical process of heating using microwave, can relax process conditions, improve economy.
In a specific embodiment of the present invention; Microwave heating equipment provided by the present invention is the device that is used for the desulfurization of continuous-type microwave oil hydrogenation; Wherein, Said microwave reactor is the fixed bed reactors that are used to accomplish the microwave hydrodesulfurization reaction, and this reactor is provided with reactant entrance and product outlet, can link to each other with the heater of oil product raw material and the after-treatment system of product respectively.
According to specific embodiments of the present invention, microwave heating equipment of the present invention also can further comprise:
Superpressure parking auto-controller, it comprises electro connecting pressure gauge and relay, when the reactor cavity internal pressure surpasses setup pressure value, can cut off microwave power supply automatically.This superpressure parking auto-controller also can be controlled preheating power supply, pumping source etc. as the case may be; Further on the basis that is equipped with the magnetic control valve, can also control the supply of supplying with body; For example be used for the oil hydrogenation desulphurization reaction, when reactor pressure surpasses setup pressure value, can cut off the supply of hydrogen.
Need to prove; Microwave heating equipment of the present invention is not limited to be applied to the hydrodesulfurization reaction of oil product; But can be applied to any high-temperature high-voltage reaction, reaction temperature can be up to 800 ℃ (reactor material for example in the stainless steel temperature range of bearing all can), reaction pressure can reach 10MPa through pressure measurement.
That is, on the other hand, the present invention also provides the application of described microwave device in the reaction that is used for realizing utilizing microwave to heat.
Particularly, the said reaction that utilizes microwave to heat can be any high-temperature high-voltage reaction in the reaction unit material tolerance range, for example can be temperature smaller or equal to the reaction smaller or equal to 10MPa of 800 ℃, pressure.
Utilize microwave heating equipment of the present invention, can be implemented in the continous way high-temperature high-voltage reaction under the microwave field effect.For example, in a specific embodiments of the present invention, be that said microwave device is used to realize continous way oil hydrogenation sulfur method, this method comprises:
Stage casing filling immobilization Hydrobon catalyst in reactor cavity;
The oil product raw material is mixed with hydrogen, be conveyed into said fixed bed reactors continuously, the oil product raw material is contacted and generation hydrodesulfurization reaction under microwave action with Hydrobon catalyst; More specifically, because microwave action, reaction condition is compared with the traditional operation condition and can be relaxed; For example, when under microwave action, carrying out the oil product of gasoline hydrodesulfurization reaction, the reaction condition that can control in the reactor is: 220～280 ℃ of reaction temperatures; 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 carry out post processing.
According to specific embodiments of the present invention, said catalyst is to be seated in around the probe.
Among the present invention, the device structure of not mentioning in detail can be with reference to the legacy equipment in affiliated field.For example, said reactor can be the Traditional industrial high-temperature high-pressure reaction kettle, and key of the present invention is to introduce at the reactor-side wall opening probe of microwave device, thereby 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 design according to the member of microwave generating apparatus of the prior art; It is to adopt rectangular waveguide to be converted into the form of coaxial transmission that key of the present invention is at waveguide segment; Probe into reactor cavity central authorities with a probe from sidewall of reactor, and microwave is introduced reactor cavity.Conventional equipment under used superpressure parking auto-controller, the product after-treatment system of hydrodesulfurization system etc. all can adopt among the present invention in the field.
In sum, the invention provides a kind of microwave heating equipment and application thereof, through coaxial transmission; Adopt the mode of probe that microwave is introduced; Can microwave technology need be applied to conscientiously the chemical reaction of heating using microwave, can relax process conditions, and microwave field is evenly distributed in the device microwave cavity; Good airproof performance, processing safety is good.
Description of drawings
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-three pin automatic regulators, 6-waveguide, 7-reactor.
Fig. 2 probes into the structural representation of reactor part for microwave device middle probe of the present invention.Wherein, 61-rectangular waveguide, 62-coaxial waveguide, 621-coaxial waveguide shell, 622-probe, 623-ceramic cap.
Fig. 3 utilizes microwave device of the present invention to carry out the process chart of 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 of beds in the device during according to a specific embodiment applied microwave heater of the present invention.Wherein picture A is an overall diagram, and picture B, C, D are respectively the profiles of directions X, Y direction and Z direction.From figure, also can find out the uniformity that microwave field distributes.
The specific embodiment
Below specify the beneficial effect of implementation process of the present invention and generation through specific embodiment, be intended to help the reader to understand essence of the present invention and characteristics better, but not as qualification to this case practical range.
See also shown in Figure 1ly, microwave heating equipment of the present invention comprises microwave source 1, circulator 2, water load 3, directional coupler 4, three pin automatic regulators 5, waveguide 6 by the microwave conduction sequence; And microwave reactor 7.See also the detailed structure of waveguide segment part shown in Figure 2 again; Wherein, waveguide 6 comprises rectangular waveguide 61 and coaxial waveguide 62, and coaxial waveguide 62 comprises the metal shell 621 (cylindric) and the probe 622 (elongated is cylindrical) of coaxial setting; Adopt rectangular waveguide to be converted into the form of coaxial transmission; Probe into reactor cavity central authorities with probe 622 from reactor 7 sidewalls, and microwave is introduced reactor cavity (that is, microwave cavity being done reactor).This reactor material is a stainless steel, can anti-higher temperature (temperature can bear within the scope at stainless steel), and pressure depends on the thickness of reactor wall metal.In the seals at of probe and reactor, can ceramic cap and ring flange be made of one, and then with flange (just adopting the form of three flanges) sealing and fixing of both sides among the figure; Also can pottery directly be welded or be bonded on the leftmost ring flange, seal (as shown in Figure 2) through two flanges.Ceramic cap itself does not influence microwave and distributes, and its gauge makes it can tolerate operating pressure and gets final product.
See also shown in Figure 3; In this embodiment; Be that microwave heating equipment of the present invention is used for the oil hydrogenation desulfurization; Wherein, microwave reactor 7 is as hydrodesulphurisatioreactors reactors, and this system that is used for the oil hydrogenation desulfurization also comprises: the after-treatment system of superpressure parking auto-controller 8 and product (condenser 9, high-pressure separator 10, low pressure separator 11, counterbalance valve 12, device for absorbing tail gas 13 etc.).
Wherein, Superpressure parking auto-controller 8 is a safety control device; Mainly form, when pressure surpasses setup pressure value, can cut off microwave power supply, preheating power supply, pumping source automatically by parts such as electro connecting pressure gauge and relays; On the basis that is equipped with the magnetic control valve, can cut off the supply of hydrogen, so this auto-controller has improved the security of experimental implementation to a great extent.
When utilizing this device to carry out continuous-type microwave oil hydrogenation desulphurization reaction, the concrete operations 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, closely knit after, adorn the red copper pad and tighten ring flange.
(2) inspection air-tightness:
Reactor is inserted the hydrogenation micro-reactor, open the hydrogen valve on the panel then, the mass flowmenter protective valve is closed, open the logical H2 of cleaning valve, regulate pressure-reducing valve and counterbalance valve, check with the fuel gas leak detector whether whole gas circuit leaks gas to reaction pressure.
(3) presulfiding of catalyst:
In the pre-vulcanization process, should in time close the middle valve of high-low pressure knockout drum, bleed off the liquid in the low pressure separation pot; After presulfurization finished, progressively cooling was closed pump, is closed hydrogen, and the mass flowmenter protective valve is closed, and slowly opens atmospheric valve then, whole device pressure release.Open cleaning valve, then atmospheric valve cuts out, flushing line is 3-5 time repeatedly, drains carbon disulfide residual in the pipeline.
(4) hydrodesulfurization reaction:
Open circulator bath, open hydrogen valve and regulate whole device pressure.When the demonstration of question response device thermometric is hanged down 20 ℃ than operating temperature, open the gasoline sampling valve, start oil pump, be adjusted to required flow; Open microwave, be adjusted to the test power demand.When treating thermometric display instrument display operation temperature, pick up counting, balance 7 hours is closed the middle valve sampling of high and low pressure knockout drum then.Sampling in per 1 hour later on sees in the sampling process till the gas that once action is wanted to get altogether 2 times rapidly.Experimental session record reactor outlet, microwave reflection power etc., after reaction finished, hydrogen valve was closed in termination of pumping, closed microwave, closed power supply.
Embodiment 1
Select Co-Mo/ γ-Al for use
2O
3The catalytically cracked gasoline of catalyst and certain oil plant, wherein total sulfur content is 340ppm, sulfur compound is mainly: thiophene, C1 thiophene, C2 thiophene and C3 thiophene etc.At weight (hourly) space velocity (WHSV) 2h
-1, reaction pressure 2MPa, 250 ℃ of reaction temperatures, hydrogen-oil ratio 200: 1.Investigated the HDS situation when microwave action (1.2kW) and no microwave action are arranged respectively.Desulfurization degree was 78.2% when the result found that microwave is arranged, and was 52.6% when not having microwave, this shows that under the same operation condition, the existence of microwave field can significantly improve FCC gasoline hydrodesulfurizationmethod rate.Further research to the FCC gasoline hydrodesulfurizationmethod shows; When having microwave to exist, the hydrogenation of olefins degree is lower, and this is the effect of the selectivity heating of microwave just; Just because of this; Discover after the hydrodesulfurization that its octane number does not only reduce the unit that raise on the contrary (the hydrodesulfurization octane number of no microwave action is 93.5, and the microwave hydrodesulfurization is 94.6).
Fig. 4 has shown in the above-mentioned course of reaction distribution map of the electric field of beds in the device.Wherein picture A is an overall diagram, and picture B, C, D are respectively the profiles of directions X, Y direction and Z direction.Can find out also that from figure it is uniformly that microwave distributes, and not have the generation of microwave leakage situation, handling safety is reliable.
Claims (8)
1. microwave heating equipment, this device comprises:
Microwave reactor; And
Microwave takes place and transmitting device; This microwave takes place and transmitting device comprises by the microwave conduction sequence: microwave source, circulator, water load, directional coupler, three pin automatic regulator and waveguides; At waveguide segment; Adopt rectangular waveguide to be converted into the form of coaxial transmission, probe into reactor central authorities from the microwave reactor sidewall, and microwave is burst in the reactor with a probe.
2. microwave heating equipment according to claim 1, wherein, the material of said microwave reactor is any or the alloy in stainless steel, copper, silver or the aluminium, the place that said probe probes into reactor is adopted and is not inhaled the ripple material and seal.
3. microwave heating equipment according to claim 1; This device is for being used for the device of continuous-type microwave reacting by heating; Wherein, said microwave reactor is the fixed bed reactors that are used to accomplish the heating using microwave reaction, and this reactor is provided with reactant entrance and product outlet.
4. according to claim 1 or 3 described microwave heating equipments, this device also comprises:
Superpressure parking auto-controller, it comprises electro connecting pressure gauge and relay, when reactor pressure surpasses setup pressure value, can cut off microwave power supply automatically.
5. each described microwave heating equipment of claim 1～4 is in the application of the reaction that is used for realizing utilizing microwave to heat.
6. application according to claim 5, wherein, said utilize reaction that microwave heats for temperature smaller or equal to the reaction of 800 ℃, pressure smaller or equal to 10MPa.
7. application according to claim 5 wherein, is that said microwave device is used to realize continous way oil hydrogenation sulfur method, and this method comprises:
Stage casing filling immobilization Hydrobon catalyst in reactor;
The oil product raw material is mixed with hydrogen, be conveyed into said fixed bed reactors continuously, the oil product raw material is contacted and generation hydrodesulfurization reaction under microwave action with Hydrobon catalyst;
The product of above-mentioned hydrodesulfurization reaction is drawn reactor continuously carry out post processing.
8. application according to claim 7, wherein, said catalyst is seated in around the probe.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105974994A (en) * | 2016-04-28 | 2016-09-28 | 广东美的厨房电器制造有限公司 | Circuit and method for power output of microwave oven |
| 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 |
| CN108633158A (en) * | 2018-05-25 | 2018-10-09 | 中国科学院合肥物质科学研究院 | A kind of portable normal pressure microwave plasma torch generation device and method |
| CN109092226A (en) * | 2018-08-30 | 2018-12-28 | 长沙新材料产业研究院有限公司 | A kind of MPCVD synthesis device microwave reflection regulating device and control method |
| CN109092227A (en) * | 2018-08-30 | 2018-12-28 | 长沙新材料产业研究院有限公司 | A kind of MPCVD synthesis device and control method |
| CN110215946A (en) * | 2019-05-29 | 2019-09-10 | 西南大学 | A kind of novel metal test tube device for microwave heating |
| CN111033889A (en) * | 2018-04-20 | 2020-04-17 | 松下知识产权经营株式会社 | Directional coupler and microwave heating device with same |
| 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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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105974994A (en) * | 2016-04-28 | 2016-09-28 | 广东美的厨房电器制造有限公司 | Circuit and method for power output of microwave oven |
| 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 |
| CN111033889A (en) * | 2018-04-20 | 2020-04-17 | 松下知识产权经营株式会社 | Directional coupler and microwave heating device with same |
| 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 |
| CN108633158A (en) * | 2018-05-25 | 2018-10-09 | 中国科学院合肥物质科学研究院 | A kind of portable normal pressure microwave plasma torch generation device and method |
| CN109092226A (en) * | 2018-08-30 | 2018-12-28 | 长沙新材料产业研究院有限公司 | A kind of MPCVD synthesis device microwave reflection regulating device and control method |
| CN109092227A (en) * | 2018-08-30 | 2018-12-28 | 长沙新材料产业研究院有限公司 | A kind of MPCVD synthesis device 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 |
| 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 |
| 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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