CN103721660A - Microwave microchip reaction device - Google Patents
Microwave microchip reaction device Download PDFInfo
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- CN103721660A CN103721660A CN201310561830.7A CN201310561830A CN103721660A CN 103721660 A CN103721660 A CN 103721660A CN 201310561830 A CN201310561830 A CN 201310561830A CN 103721660 A CN103721660 A CN 103721660A
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- microwave
- microchip
- reaction
- micro passage
- generation module
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 74
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 239000012530 fluid Substances 0.000 claims abstract description 5
- 238000007599 discharging Methods 0.000 claims description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 238000012546 transfer Methods 0.000 claims description 6
- 239000003990 capacitor Substances 0.000 claims description 4
- 238000009825 accumulation Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 20
- 230000005540 biological transmission Effects 0.000 abstract 2
- 238000010924 continuous production Methods 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 5
- 239000011343 solid material Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 238000012805 post-processing Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- OHBQPCCCRFSCAX-UHFFFAOYSA-N 1,4-Dimethoxybenzene Chemical compound COC1=CC=C(OC)C=C1 OHBQPCCCRFSCAX-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 2
- 238000001311 chemical methods and process Methods 0.000 description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- CUONGYYJJVDODC-UHFFFAOYSA-N malononitrile Chemical compound N#CCC#N CUONGYYJJVDODC-UHFFFAOYSA-N 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a microwave microchip reaction device which is characterized by comprising a microwave generation module, a micro-channel reactor and a feeding system, wherein the microwave generation module generates microwave to heat a fluid in the micro-channel reactor; and the feeding system is communicated to a micro-channel inlet of the micro-channel reactor through a pipeline. According to the microwave microchip reaction device, the heating power of any horizontal plane perpendicular to the microwave transmission direction in a microwave cavity is consistent, so that the heating temperature in the plane is uniform, and materials can enter a reaction cavity continuously; the total size of the microchip is small, the channel characteristic scale cannot reach a critical scale of flame transmission, and a small quantity of reaction holdings exist in the microchip, so that the microchip reaction device has internal safety; and in a microwave field, the device can be applied to a flammable and combustible reaction process with strong heat release, accordingly, the safety of the reaction process can be remarkably improved, and continuous production is realized.
Description
Technical field
The present invention relates to a kind of microwave microchip reactor, belong to micro-chemical machinery field.
Background technology
Microwave current is widely used in heating material and the field such as dry, and there is heat dissipation effect during due to its carry out microwave radiation heating solid, make microwave when heat solid material, the phenomenon that there will be hot-spot, cause solid material to melt, the phenomenons such as coking, so microwave is difficult to be used in chemical reaction field.Overheated due to part more, when the reaction of heating fluid foods, the container of carrying material also there will be hot-spot, and causes container deformation and destruction.And existing document and technology report are limited to heating and the reaction of clearance-type more, therefore for most chemical process reactions, the demand of homogeneous radiation heating and uninterrupted mobile reaction is continuously the most urgent, and being also has most technology to be solved and research.
Patent of invention (CN103055778A) is a kind of dry for solid material, and continuous axle streaming microwave reactor, is only applicable to solid material, for most chemical process reactions, cannot realize.And this material inventory is large, in material inside, because material is thicker along microwave relay direction material, there will be the gradient of my temperature, also there is the inhomogeneous phenomenon of this heating material.Especially for the reaction of some reaction time within the several seconds, the problem of its homogeneous heating is more aobvious outstanding.Patent of invention (CN102491321A) is a kind of single microwave energy generator that passes through to change in a heating chamber, change by a plurality of generators and launch into heating chamber from multiple directions, passing through the method that repeatedly microwave density is encrypted in refraction, change microwave heterogeneity on the whole, and from can add uniformly thermal material in some horizontal planes.This invents related object same problem, remains solid material, and charging that cannot be continuous and discharging.
Summary of the invention
Goal of the invention: the microwave microchip reaction unit that the object of the present invention is to provide a kind of homogeneous heating safety.
Technical scheme: a kind of microwave microchip reaction unit of the present invention comprises microwave generation module, micro passage reaction and feeding system, described feeding system is communicated with micro passage reaction through pipeline, and described microwave generation module provides heating using microwave to the fluid in micro passage reaction.Wherein microwave generation module comprises magnetron, microwave energy follower, wave guide, waveguide array, this waveguide array is the two dimensional surface accumulation bodies of some waveguides in the plane perpendicular to waveguide array microwave transmit direction, the sensing of each waveguide is identical with waveguide array transmit direction, and magnetron transfers to microwave energy follower after producing microwave, transfers to waveguide array launch by wave guide.So arrange, through waveguide array, not only can filter out needed heating microwave section, be convenient to the control of control system to power output, and microwave direction can be adjusted, make evenly vertically transmitting downwards of microwave, microchip reactor is further set perpendicular to transmit direction, makes microchip reactor homogeneous heating everywhere.In addition, microwave generation module also comprises high-tension transformer and capacitor.
Further, micro passage reaction of the present invention can see through the micro passage reaction that microwave material is made for transparent PVC, polytetrafluoroethylene (PTFE), silicon, pottery, glass etc.Micro passage reaction microchannel width is 0.04～3 millimeter.
Further, feeding system is communicated with the microchannel entrance of micro passage reaction through pipeline, is communicated with on both pipeline and is also provided with feed check valve, and the exit, microchannel of described micro passage reaction is also provided with discharging check valve.
Further, this device can also comprise control system, control system comprises temperature sensor, pressure sensor, controller, after the pressure in temperature sensor and pressure sensor measurement exit, micro passage reaction microchannel and temperature, be sent to controller, controller is controlled the feeding rate of feeding system and the microwave power of microwave generation module according to the pressure reading and Temperature numerical.
Specifically temperature sensor can be serially connected in after the pipeline of discharging check valve, described pressure sensor is serially connected in after the pipeline of temperature sensor.
The present invention compared with prior art, its beneficial effect is: the present invention can make the heating power of interior any one horizontal plane perpendicular to microwave propagation direction of device consistent, thereby make the heating-up temperature in this plane even, that is heating power is consistent to make this microchip reactor everywhere, material can enter in reaction chamber continuously.Because microchip overall volume is little, channel characteristics yardstick does not reach critical dimension and the interior a small amount of reaction having of microchip of flame propagation, make microchip reactor there is inherent security, in microwave field, can be applicable to the inflammable and explosive course of reaction of strong heat release, can significantly improve the security of course of reaction, and realize serialization and produce.
Accompanying drawing explanation
Fig. 1 is microwave microchip reaction unit schematic side view of the present invention;
Fig. 2 is the microchip reactor schematic diagram in microwave microchip reaction unit of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing, technical solution of the present invention is elaborated, but protection scope of the present invention is not limited to described embodiment.
Embodiment 1:
The microwave microchip reaction unit of the present embodiment, comprise microwave generation module, micro passage reaction 6 and feeding system 11, described feeding system 11 is communicated with micro passage reaction 6 through pipeline, and described microwave generation module provides heating using microwave to the fluid in micro passage reaction 6.Microwave generation module comprises magnetron 9, microwave energy follower 10, wave guide 4, waveguide array 5, described waveguide array 5 is the two dimensional surface accumulation bodies of some waveguides in the plane perpendicular to waveguide array microwave transmit direction, the sensing of each waveguide is identical with waveguide array 5 transmit directions, transfers to microwave energy follower 10 and transfer to waveguide array 5 transmittings by wave guide 4 after magnetron 9 generation microwaves.The present embodiment micro passage reaction 6 be arranged in the plane perpendicular to waveguide array 5 transmit directions.The microwave generation module of the present embodiment also comprises that high-tension transformer 7 and capacitor 8 come for magnetron power supply.
The present embodiment micro passage reaction 6 be silicon micro passage reaction processed, but other it may occur to persons skilled in the art that see through and can all can be used as the material of this micro passage reaction as transparent PVC, polytetrafluoroethylene (PTFE), pottery, glass etc. through the material of microwave.
It is 004 millimeter that the present embodiment arranges micro passage reaction 6 microchannel width.
And the present embodiment is communicated with the microchannel entrance 62 of micro passage reaction 6 through pipeline in described feeding system 11, be communicated with on both pipeline and be also provided with feed check valve (3), the microchannel outlet (61) of described micro passage reaction (6) locates to be also provided with discharging check valve (33).
The present embodiment is also provided with control system, control system comprises temperature sensor 2, pressure sensor 1, controller 12, described temperature sensor 2 and pressure sensor 1 are sent to controller 12 after measuring pressure that micro passage reaction 6 microchannels export 61 places and temperature, and controller 12 is according to pressure and the temperature data control feeding rate of feeding system 11 and the microwave power of microwave generation module.Wherein temperature sensor 2 is serially connected in after the pipeline of discharging check valve 33, and described pressure sensor 1 is serially connected in after the pipeline of temperature sensor 2.
The present embodiment device course of work is as follows:
Material is carried reaction raw materials by one-way relief valves 3 toward microchannel entrance 61 from feeding system 11, enter micro passage reaction, evenly microwave field is by high-tension transformer 7, capacitor 8, magnetron 9, microwave energy follower 10, waveguide array 5 and wave guide 4, by programme-control, under setting power, produce, temperature signal is by temperature sensor 2, be transferred to controller 12, controller is compared the real time temperature detecting with design temperature, the setting pressure that real-time pressure is corresponding with setting feeding rate is compared.The corresponding relation of feeding rate and setting pressure can calculate by the flow resistance of system, also can record by experiment in advance.If real-time pressure value feeding system 11 feeding rates that improve less than normal, if real-time pressure value feeding system 11 feeding rates that reduce bigger than normal, if record, real time temperature is higher improves magnetron 9 microwave transmitting powers, if record real time temperature magnetron 9 transmitting powers that reduce on the low side.When continuing normal reaction, start to collect reaction product material.The reaction time of material is controlled by flow velocity.
So set temperature can be controlled reaction temperature, force value is set and can controls reaction pressure on the one hand, also can control W-response device material flow by controlled pressure value on the other hand, and then adjust material through the reaction time of microreactor.
The algorithm function of this controller is:
1, read real time temperature value Tt and real-time pressure value Pt;
2, Tt is compared with controller storing temperature setting value T;
If 3 Tt are more than or equal to T, reduce magnetron 9 microwave transmitting powers;
If 4 Tt are less than T, improve magnetron 9 and launch all rates;
5, by implementing the pressure value P t setup pressure value P corresponding with the setting feed flow velocity of controller storage, compare;
If 6 Pt are more than or equal to P, the feeding system that slows down 11 feeding rates;
If 7 Pt are less than P, accelerate feeding system 11 feeding rates;
8, read on off state value;
If 9 switch opens, get back to the 1st step program;
If 10 switches cut out, program stops.
Embodiment 2
Other arranges same embodiment 1, but micro passage reaction 6 microchannel width are 3 millimeters.
Embodiment 3
Device described in employing embodiment 1, pass into material salicylide 1mmol, malononitrile 2mmol, to methylbenzene phenyl-sulfhydrate 1mmol, pyridine 0.2mmol is dissolved in 4mL ethanol, microwave: temperature setting is set to 110 degrees Celsius, under the feeding rate of 0.267mL/min, reaction continues 15 minutes, cooling through post processing, filters, ethanol washs to obtain 0306g white solid, yield 85%.
Popular response 3 hours, obtains 0266g white solid, yield 74%;
Microwave reaction time shorten is original 8.3%, and yield improves 11%.
Device material 2 described in employing embodiment 1,4-dimethoxy benzene first 10mmol, 1-((4-benzyloxy)-3-methoxyphenyl) ethyl ketone 10mmol is dissolved in 3mL ethanol, add 0.5mL60% potassium hydroxide solution, set 25 degrees Celsius of reactions of reaction temperature 15 minutes, under the feeding rate of 0.2mL/min, the lasting post processing in 15 minutes of reaction obtains 343g product 1-((4-benzyloxy)-3-methoxyphenyl)-3-(2,4-Dimethoxyphenyl) third-2-alkene-1-ketone, yield 85%
Popular response 16 hours, post processing obtains 319g product 1-((4-benzyloxy)-3-methoxyphenyl)-3-(2,4-Dimethoxyphenyl) third-2-alkene-1-ketone, yield 79%;
Microwave reaction time shorten is original 1.56%, and yield improves 11%.
As mentioned above, although represented and explained the present invention with reference to specific preferred embodiment, it shall not be construed as the restriction to the present invention self.Not departing under the spirit and scope of the present invention prerequisite of claims definition, can make in the form and details various variations to it.
Claims (9)
1. a microwave microchip reaction unit, it is characterized in that, comprise microwave generation module, micro passage reaction (6) and feeding system (11), described feeding system (11) is communicated with micro passage reaction (6) through pipeline, and described microwave generation module provides heating using microwave to the fluid in micro passage reaction (6).
2. microwave microchip reaction unit according to claim 1, it is characterized in that, described microwave generation module comprises magnetron (9), microwave energy follower (10), wave guide (4), waveguide array (5), described waveguide array (5) is the two dimensional surface accumulation bodies of some waveguides in the plane perpendicular to waveguide array microwave transmit direction, the sensing of each waveguide is parallel with waveguide array (5) transmit direction, transfers to microwave energy follower (10) and transfer to waveguide array (5) transmitting by wave guide (4) after magnetron (9) generation microwave.
3. microwave microchip reaction unit according to claim 2, is characterized in that, described micro passage reaction (6) is in the plane perpendicular to waveguide array (5) transmit direction.
4. microwave microchip reaction unit according to claim 2, is characterized in that, described microwave generation module also comprises high-tension transformer (7) and capacitor (8).
5. according to the microwave microchip reaction unit described in claim 1,2,3 or 4, it is characterized in that described micro passage reaction (6) is for the micro passage reaction of transparent PVC, polytetrafluoroethylene (PTFE), silicon, pottery, glass system.
6. according to the microwave microchip reaction unit described in claim 1,2,3 or 4, it is characterized in that, described micro passage reaction (6) microchannel width is 0.04～3 millimeter.
7. according to the microwave microchip reaction unit described in claim 1,2,3 or 4, it is characterized in that, described feeding system (11) is communicated with the microchannel entrance (62) of micro passage reaction (6) through pipeline, be communicated with on both pipeline and be also provided with feed check valve (3), the microchannel outlet (61) of described micro passage reaction (6) locates to be also provided with discharging check valve (33).
8. according to the microwave microchip reaction unit described in claim 1,2,3,4, it is characterized in that, this device also comprises control system, described control system comprises temperature sensor (2), pressure sensor (1), controller (12), after the pressure that described temperature sensor (2) and pressure sensor (1) measurement micro passage reaction (6) microchannel outlet (61) are located and temperature, be sent to controller (12), controller (12) is controlled the feeding rate of feeding system (11) and the microwave power of microwave generation module according to the pressure reading and Temperature numerical.
9. microwave microchip reaction unit according to claim 8, it is characterized in that, described temperature sensor (2) is serially connected in after the pipeline of discharging check valve (33), and described pressure sensor (1) is serially connected in after the pipeline of temperature sensor (2).
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| CN201310561830.7A CN103721660B (en) | 2013-11-12 | 2013-11-12 | Microwave microchip reaction unit |
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| CN201310561830.7A CN103721660B (en) | 2013-11-12 | 2013-11-12 | Microwave microchip reaction unit |
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| CN103721660B CN103721660B (en) | 2016-08-17 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107051347A (en) * | 2017-06-19 | 2017-08-18 | 北京化工大学 | A kind of device of microwave coupling reaction and its application |
| CN109078590A (en) * | 2017-06-13 | 2018-12-25 | 中国石油化工股份有限公司 | Micro passage reaction |
| CN109718876A (en) * | 2018-12-28 | 2019-05-07 | 路煜恒 | A kind of micro-fluidic chip that tube side is controllable |
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| WO2005102510A1 (en) * | 2004-04-20 | 2005-11-03 | Sanko Chemical Industry Co., Ltd. | Chemical reaction apparatus utilizing microwave |
| US20080124253A1 (en) * | 2004-08-31 | 2008-05-29 | Achim Schmidt | Fluidized-Bed Reactor For The Thermal Treatment Of Fluidizable Substances In A Microwave-Heated Fluidized Bed |
| CN101954267A (en) * | 2010-08-20 | 2011-01-26 | 同济大学 | Microwave reactor for preparing loaded fuel cell catalyst |
| CN102946655A (en) * | 2012-11-13 | 2013-02-27 | 中国石油大学(北京) | Microwave heating device capable of being continuously operated and resisting high temperature and high pressure and application thereof |
| CN102949974A (en) * | 2012-08-31 | 2013-03-06 | 中国石油大学(北京) | Microwave heating device and application thereof |
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2013
- 2013-11-12 CN CN201310561830.7A patent/CN103721660B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005102510A1 (en) * | 2004-04-20 | 2005-11-03 | Sanko Chemical Industry Co., Ltd. | Chemical reaction apparatus utilizing microwave |
| US20080124253A1 (en) * | 2004-08-31 | 2008-05-29 | Achim Schmidt | Fluidized-Bed Reactor For The Thermal Treatment Of Fluidizable Substances In A Microwave-Heated Fluidized Bed |
| CN101954267A (en) * | 2010-08-20 | 2011-01-26 | 同济大学 | Microwave reactor for preparing loaded fuel cell catalyst |
| CN102949974A (en) * | 2012-08-31 | 2013-03-06 | 中国石油大学(北京) | Microwave heating device and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109078590A (en) * | 2017-06-13 | 2018-12-25 | 中国石油化工股份有限公司 | Micro passage reaction |
| CN109078590B (en) * | 2017-06-13 | 2021-05-14 | 中国石油化工股份有限公司 | Micro-channel reactor |
| CN107051347A (en) * | 2017-06-19 | 2017-08-18 | 北京化工大学 | A kind of device of microwave coupling reaction and its application |
| CN109718876A (en) * | 2018-12-28 | 2019-05-07 | 路煜恒 | A kind of micro-fluidic chip that tube side is controllable |
| CN109718876B (en) * | 2018-12-28 | 2021-04-02 | 路煜恒 | Controllable micro-fluidic chip of tube pass |
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| CN103721660B (en) | 2016-08-17 |
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