CN2284100Y - Microwave reaction unit - Google Patents
Microwave reaction unit Download PDFInfo
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- CN2284100Y CN2284100Y CN 97201861 CN97201861U CN2284100Y CN 2284100 Y CN2284100 Y CN 2284100Y CN 97201861 CN97201861 CN 97201861 CN 97201861 U CN97201861 U CN 97201861U CN 2284100 Y CN2284100 Y CN 2284100Y
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- reaction
- temperature sensor
- microwave
- reaction unit
- reaction vessel
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Abstract
The utility model relates to a novel microwave reaction device and the application thereof. The novel microwave reaction device comprises a microwave oven, a reaction vessel, a refrigerating device and a temperature sensor, wherein the reaction vessel is arranged in the microwave oven, the refrigerating device is arranged at the upper part of the reaction vessel, and the temperature sensor is inserted in the reaction vessel. The application of the novel microwave reaction device comprises various reactions of organic catalysis or pharmaceutical catalysis chemistry and relevant reactions of biochemistry and molecular biology. The application of the novel microwave reaction device can quicken the chemical reaction velocity, increase the reaction yield, and improve the reaction selectivity. The utility model also relates to the application of the microwave in the fields of inorganic chemistry, analytical chemistry, material science and biological and medical pharmacology.
Description
The utility model relates to chemical reaction equipment, more particularly, relates to a kind of chemical reaction equipment of microwave as heating, catalysis means that it is characterized in that using, and can be used for the relevant reaction of organic or pharmaceutical chemical multiple reaction and molecular biology and material science.
Chemical reaction often needs heating or high temperature, high pressure, and heating means in the past all are with the mode of heat conduction and thermal convection current, cause reaction speed relatively slow, and reaction yield and selectivity are also not too satisfactory; Although accelerate, improve organic with traditional chemical catalysis method in addition and pharmaceutical chemistry reaction effectively, can not satisfy the requirement of current era high speed development far away.So quickening chemical reaction velocity, the selectivity that increases reaction yield, simplification last handling process, improvement reaction, raising research and production efficient have become the key subjects that people press for solution.
Microwave is known as a kind of heating energy source, but does not also use it for the synthetic report of catalysis medicine at present.The design people transforms micro-wave oven, and is used for catalyzed chemical reaction, and especially organic and pharmaceutical chemistry reaction finds that it has the fuel factor and the entropic effect of inducing or quickening chemical reaction.
The purpose of this utility model provides a kind of novel microwave reaction unit, this device this heating of applied microwave and physics catalysis new technology, shortened the time of chemical reaction, the selectivity and the yield of reaction have been improved, but the reaction of catalysis polytype is for microwave technology contributes applying of association area such as Synthetic Organic Chemistry, molecular biology, analytical chemistry, inorganic chemistry, mineral chemistry, material science, pharmaceutical chemistry and biologic pharmacological sciences.
The novel microwave reaction unit is made up of four parts: micro-wave oven, reaction vessel, cooling device and temperature sensor.Wherein, reaction vessel places micro-wave oven, and cooling device can be connected the top of reaction vessel, and temperature sensor can insert in the reaction vessel.Above-mentioned cooling device is a reflux condensing tube, or places the surface plate of placing the band ice bag on the funnel of band ice bag or the high beaker on the conical flask.Temperature sensor is meant the temperature sensor of being made up of thermistor-resistive conductor, or fibre optic temperature sensor, or the thermoelectricity of band shielding protection cover infrared temperature sensor occasionally.Reaction vessel is meant two neck bottles, three-necked bottle, conical flask or beaker, flask and glass, plastics, pottery or with the withstand voltage retort of one or more sealings of the band pressure sensor of being made by high polymer that can see through microwave, or 2 and 960 reaction vessels of above as many as are comprised test tube reasonable combination combinatorial chemistry dish together.
Shown in the drawings is a kind of of novel microwave reaction unit of the present utility model, and it comprises micro-wave oven 1, three-necked bottle 2, and reflux condenser 3, temperature sensor 4, wherein micro-wave oven is to be that the household microwave oven of 2.45GHz converts with frequency.This novel microwave reaction unit as reactor body, has been installed reflux condensing tube 3 in micro-wave oven top boring by micro-wave oven 1, and by in joint and the micro-wave oven 1 three-necked bottle 2 be connected tapping micro-wave screening material seal; Air vent through the micro-wave oven left side or the right has been installed the temperature sensor of being made up of thermistor-resistive conductor 4, side mouth by three-necked bottle inserts in the three-necked bottle, can show temperature in the reaction vessel in real time by charactron 5, reaction time and power are regulated by control panel 6.This novel microwave reaction unit meets national safety standard through units concerned's leak-testing.
We have successfully finished polytype chemical reaction with the novel microwave reaction unit, and sum up and to have formulated several effective methods and be used to finish different reactions.The novel microwave reaction unit can not only be finished low boiling expeditiously or the solution reaction of penetrating odor is arranged, and also can not reinstall the stream condenser pipe, cover the organic solid phase reaction of catalysis preferably and reaction of higher boiling polar liquid phase or liquid-solid opening wide or confined reaction under the situation in reactor head duct with copper mesh.The research work that we finish with the novel microwave reaction unit comprises: esterification, ester exchange reaction, condensation reaction, annulation, ring closure reaction, alkylated reaction, phase transfer reaction, hydrolysis, saponification, addition reaction, elimination reaction, substitution reaction, the Tipon-Cohen reaction, the Krapcho reaction, the Knoevenagel reaction, the Reformatsky reaction, the organic chemistry of many types such as organometallic reaction and drug synthetic reaction, synthetic and the degraded of high polymer, the relevant reaction of superconductor and mineral material, and the synthetic and degraded of sugar, synthetic and the degraded of polypeptide, the relevant reaction of the synthetic and montage reaction equimolecular field of biology of DNA and RNA, and the research of microwave biological effect and application.We mainly contain the reasonable combination utilization that back flow reaction, sealed reaction, combinatorial chemistry synthetic reaction and different catalysis process comprise chemical catalysis or ultrasonic wave catalysis and microwave catalysis by the experimental technique of usefulness.Experimental result shows, the novel microwave reaction unit is being accelerated the organic medicinal chemistry reaction speed, is being improved aspects such as reaction selectivity and yield and demonstrate many superiority, makes over manyly to be difficult to take place or chemical reaction that speed is very slow becomes and realizes easily and high speed is finished.
With concrete examples of implementation the utility model is described below.
Embodiment 1:
With the synthetic two benzoglycolic acid methyl esters of novel microwave reaction unit
With two benzoglycolic acid 1.14g (0.005mol), methyl alcohol 10mL places the 50mL conical flask, splashes into 6 dense H
2SO
4, put into the three-necked bottle of WP800BS type Glanz micro-wave oven.Connect reflux condensing tube by tube connector, the temperature sensor that thermistor-resistive conductor is formed inserts wherein by three-necked bottle side mouth.Microwave power 800W is set, and low fire reaction 3min obtains orange-red solution.Add 10mL water, Na with 20%
2CO
3Solution is neutralized to neutrality, with 4 * 10mL extracted with diethyl ether, combined ether layer, with the washing of 2 * 10mL distilled water, with the anhydrous MgSO of the diethyl ether solution that obtains
4Dry, filtration with rotating thin film evaporimeter concentrated solution, are used the benzene crystallization, obtain beautiful white crystal 0.85g, productive rate 72.5%.Product is identified through elementary analysis and wave spectrum.Reaction time, reaction yield also more former 50% had a more substantial increase than shortening 80 times with the used time of the method that adds hot reflux.
Embodiment 2:
Prepare the phthalimide caproic acid with the novel microwave reaction unit
In the conical flask of 50mL, add and grind uniform 5.66g (0.005mol) caprolactam, 7.41g (0.005mol) phthalic anhydride, add 2 in water, place the funnel of band ice bag on the conical flask, place the NN-K652 of Panasonic type micro-wave oven, power 850W, moderate heat 3min, high fiery 1min gets pale red brown crystal.Tlc analysis productive rate 60%.
Use 6 sealing load jars simultaneously, heating using microwave, power 850W, moderate heat 3min, productive rate 65%, product passes through Analysis and Identification.And needed pressurization 304KPa originally, 160 ℃ of temperature, reaction 5h, productive rate 55%.
Embodiment 3:
Realize the tetraphenylporphyrin annulation with the novel microwave reaction unit
Get 1.4mL pyrroles and 2.1mL benzaldehyde, join in the 45mL dimethylbenzene, make chemical catalyst with paranitrobenzoic acid, above mixture is put into the three-necked bottle of 150mL, put into the NN-K652 of Panasonic type micro-wave oven again, load onto reflux condensing tube by tube connector, microwave power 850W, high fire heating 5min.Be cooled to room temperature then, product obtains the pure tetraphenylporphyrin of purple with ethyl alcohol recrystallization 2～3 times, and productive rate 40%, product have passed through elementary analysis and wave spectrum is identified.With the method that common heating refluxes, reaction 4h, productive rate is less than 10%; With the about 30min of ultrasonic wave catalytic reaction, effect is also undesirable, may be too big owing to this reaction negentropy, and ultrasonic cavitation and agitation effects are too violent, and difficulty is gathered at a formation porphyrin ring 8 molecules.As seen, with chemical catalysis and the utilization of microwave catalysis reasonable combination, the reaction that is difficult to take place is carried out at a relatively high speed.
More than the example of three enforcements show, use novel microwave reaction unit and method, not only can improve reaction speed greatly, simplify last handling process, also can increase substantially reaction yield, have a extensive future in fields such as pharmacy, chemical industry, material and national defence.
Claims (5)
1. a new type of microwave reaction unit is characterized in that reaction vessel places micro-wave oven, and cooling device can be connected the top of reaction vessel, and temperature sensor can insert in the reaction vessel.
2. according to the novel microwave reaction unit of claim 1, it is characterized in that cooling device is a reflux condensing tube, it is installed on the micro-wave oven top by boring.
3. according to the novel microwave reaction unit of claim 1, it is characterized in that cooling device is the surface plate of placing the funnel of band ice bag on the conical flask or place the band ice bag on high beaker.
4. according to the novel microwave reaction unit of claim 1, it is characterized in that temperature sensor is meant the temperature sensor of thermistor-resistive conductor composition or the thermocouple or the infrared temperature sensor of fibre optic temperature sensor or band shielding protection cover.
5. according to the novel microwave reaction unit of claim 1, it is characterized in that reaction vessel is meant two neck bottles, three-necked bottle or beaker, conical flask, flask, or with the withstand voltage retort of one or more sealings of the band pressure sensor that manufactures by high polymer that can see through microwave, or 2 and 960 reaction vessels of above as many as are comprised test tube reasonable combination combinatorial chemistry dish together.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97201861 CN2284100Y (en) | 1997-03-19 | 1997-03-19 | Microwave reaction unit |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 97201861 CN2284100Y (en) | 1997-03-19 | 1997-03-19 | Microwave reaction unit |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN2284100Y true CN2284100Y (en) | 1998-06-17 |
Family
ID=33923173
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 97201861 Expired - Fee Related CN2284100Y (en) | 1997-03-19 | 1997-03-19 | Microwave reaction unit |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN2284100Y (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1091394C (en) * | 1999-04-02 | 2002-09-25 | 徐有生 | Industrial microwave oven specially for fluid treatment |
| CN1093430C (en) * | 1999-09-30 | 2002-10-30 | 东南大学 | Resonating cavity type circular-channel waveguide microwave chemical reaction apparatus |
| CN1093773C (en) * | 1999-09-08 | 2002-11-06 | 东南大学 | Travelling-wave type microwave chemical reactor with slot wave guide |
| CN100333825C (en) * | 2004-08-04 | 2007-08-29 | 昆明贵金属研究所 | Microwave chemical reaction device |
| CN100443157C (en) * | 2006-11-16 | 2008-12-17 | 中国科学院长春应用化学研究所 | Application of continuous microwave reactor |
| CN107592986A (en) * | 2015-04-10 | 2018-01-16 | 丹麦科技大学 | The pharmaceutical preparation container of sensor cluster including microwave power supply |
| CN108218068A (en) * | 2018-01-22 | 2018-06-29 | 沈阳建筑大学 | A kind of coagulation-microwave reinforced water treatment experimental device |
-
1997
- 1997-03-19 CN CN 97201861 patent/CN2284100Y/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1091394C (en) * | 1999-04-02 | 2002-09-25 | 徐有生 | Industrial microwave oven specially for fluid treatment |
| CN1093773C (en) * | 1999-09-08 | 2002-11-06 | 东南大学 | Travelling-wave type microwave chemical reactor with slot wave guide |
| CN1093430C (en) * | 1999-09-30 | 2002-10-30 | 东南大学 | Resonating cavity type circular-channel waveguide microwave chemical reaction apparatus |
| CN100333825C (en) * | 2004-08-04 | 2007-08-29 | 昆明贵金属研究所 | Microwave chemical reaction device |
| CN100443157C (en) * | 2006-11-16 | 2008-12-17 | 中国科学院长春应用化学研究所 | Application of continuous microwave reactor |
| CN107592986A (en) * | 2015-04-10 | 2018-01-16 | 丹麦科技大学 | The pharmaceutical preparation container of sensor cluster including microwave power supply |
| CN108218068A (en) * | 2018-01-22 | 2018-06-29 | 沈阳建筑大学 | A kind of coagulation-microwave reinforced water treatment experimental device |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |