CN101342425B - Microwave separation method and apparatus used thereof - Google Patents
Microwave separation method and apparatus used thereof Download PDFInfo
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- CN101342425B CN101342425B CN2008100489826A CN200810048982A CN101342425B CN 101342425 B CN101342425 B CN 101342425B CN 2008100489826 A CN2008100489826 A CN 2008100489826A CN 200810048982 A CN200810048982 A CN 200810048982A CN 101342425 B CN101342425 B CN 101342425B
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Abstract
The present invention provides a microwave separation method and a device. Under different vacuum degrees, the method utilizes the microwave as a heat source to heat separated substances with different dielectric constants and utilizes a cold end insensitive to the microwave to cool and collect distillate steam, thus realizing the separation between a mixture with a high dielectric constant and a mixture with a low dielectric constant. An overflowplate is arranged below the feed opening of the microwave molecular still of the present invention, a slit is designed below the overflowplate to reallocate fluid, moreover, the thickness of a fluid film is controlled, so that the thickness of the fluid film can be uniform, and separation is fulfilled under the microwave heat source. The method of the present invention can be conveniently operated, and the structure of the adopted microwave molecular still is simple, so the separation of substances with different dielectric constants can be conveniently realized.
Description
Technical field
The present invention relates to a kind of with microwave realization chemical separating method and device.
Background technology
Microwave is the electromagnetic wave of a kind of frequency between 300MHz to 300GHz, carry out different with traditional heating from outside to inside in modes such as heat conduction, heat radiations, characteristics such as microwave is to heat simultaneously by dipole rotation and ionic conduction dual mode inside and outside, has high selectivity, and firing rate is fast.Microwave technology at present by and the grafting of traditional handicraft, brought into play increasing effect at aspects such as auxiliary synthetic, the microwave dryings of microwave auxiliary extraction, microwave.The application of microwave technology has also entered ripe promotional period.This will provide good research basis for the research of microwave molecular distillation technique.
Molecular distillation technique has obtained the scale application in that many countries are industrial at present, in industries such as medicine, fine chemistry industry, oil and fat chemical, food additives.The molecular clock main feature is to adopt the control of constant temperature hot wall to treat the heating-up temperature of separation of material, can under XHV, operate, make liquid under temperature, break away from liquid level far below its boiling point, free path according to effusion liquid is provided with the bigger molecule of colling end cooling free path, realize the separation of material, can solve the indeterminable separation difficult problem of conventional distillation technique.Because it has the characteristics such as boiling point, low, the heated time weak point of distillation pressure, separation degree height that vapo(u)rizing temperature is lower than material, thereby can reduce the separation costs of high boiler material greatly.
Summary of the invention
Problem to be solved by this invention is: providing a kind of is the chemical separating method of thermal source with microwave, the method for utilizing the difference of the dielectric constant of separated material realize to separate.
The technical scheme that the present invention solves the problems of the technologies described above employing is: be thermal source with the microwave, under different vacuums, the separated materials different to dielectric constant heat, by the insensitive cold junction of microwave is cooled off collection to distillating part steam, realize separating of high-k and low-k mixture, specifically may further comprise the steps: the separated material that dielectric constant is different places and makes it to form one deck liquid film on the flat board, put into microwave source after flat board put into airtight reagent bottle, driving vavuum pump treats to open microwave source and be adjusted to power demand after the pressure stability, after molecular clock finishes, close microwave, open exhauster regulating valve, collect target components.
Above-mentioned microwave distillation cold junction has microwave or shielding.
Above-mentioned separated material places the liquid level of accepting heating using microwave on the flat board to be the thin layer distribution.
The present invention also provides a kind of above-mentioned microwave separation method equipment therefor, this device comprises cold plate and distil container at least, cold plate is positioned at the distil container middle part distil container is divided into vaporization chamber and condensation chamber, the one side relative with cold plate is evaporating surface in the vaporization chamber, the top of evaporating surface is provided with overflow plate, the end face of vaporization chamber has aspirating hole and material inlet, and the bottom surface of vaporization chamber has mother liquor outlet and cut outlet, and is provided with baffle plate between mother liquor outlet and the cut outlet; The top of condensation chamber has cooling liquid outlet, and the bottom of condensation chamber has the cooling fluid inlet.
Above-mentioned overflow plate and evaporating surface have angle, and angle is positioned at material inlet below, and have a slit below the overflow plate, and slit is positioned at 1cm place, overflow plate below, and slit width is 0.5mm.
Add material from charging hole, material drops on the overflow plate along evaporating surface, along with material accumulates gradually, material will overflow gradually from the upper end of overflow plate, forming one deck liquid film flows along whole evaporating surface, and at the slit below overflow plate flow fluid is redistributed, and the thickness of control liquid film makes that the thickness of liquid film is even.When the effect of material owing to gravity, when evaporating surface constantly descended, under the effect of certain microwave intensity and vacuum, light components will obtain energy and overflow from evaporating surface, and finally reaches on the cold plate.Material on the cold plate is discharged from the cut outlet, and the evaporating surface material is sent from the mother liquor outlet.Baffle plate separates material that evaporating surface flows down and the material that flows down from cryosurface.
Refrigerant is passed in the condensation chamber from the cooling fluid inlet, flows out from cooling liquid outlet.Used refrigerant is the less material that does not absorb microwave of dielectric constant (for example cyclohexane, benzene etc.)
When electromagnetic wave entered from the surface of medium and portion propagates within it, because energy constantly is absorbed and is converted into heat energy, its entrained energy was decayed with exponential form just along with the distance of going deep into dielectric surface.This fuel factor of microwave converts microwave energy to heat energy medium is heated, and forms unique medium and be heated by hot mode-medium integral body, promptly so-called no thermograde heating.Molecule with certain polarity produces instantaneous polarization under the microwave electromagnetic field action, when microwave frequency is 2450MHz, molecule is just done the reversal campaign with the speed of 24.5 hundred million times/s, thereby produce key vibration, tear and particle between phase mutual friction, collision, promotion molecular activity part (polarity part) contacts better and reacts, generate a large amount of heat energy simultaneously rapidly, cause that temperature raises.Because its chemical composition can not be single, and different chemical constituents has different dielectric propertys, absorb microwave energy degree difference for most of material, show as heating using microwave and have selectivity.
The present invention not only utilizes the difference of molecular free path in the molecular clock process, and can utilize the separation of the difference realization mixture of intermolecular polarity.The present invention has following characteristics: 1. heating process is more targeted, and polar molecule absorbs microwave, and nonpolar molecule does not absorb or seldom absorb microwave, has improved the separation degree of polar molecule and nonpolar molecule like this.2. because little molecule can obtain the cold junction condensation process that microwave is omnidistance to be supported escaping into from liquid level, little molecule can increase greatly from the liquid level overflow capability, can reduce the requirement of separation process, and can improve molecular free path, help improving molecular clock level and ability liquid level thickness.3. the controllability of microwave conveniently designs and carries out multi-stage separation, and the diversity that also helps equipment is used and maintenance.Can reach the purpose of separation to the sensitiveness of microwave according to each component that is distilled object, for separation provides a kind of new approach.
Description of drawings
Fig. 1 is the structural representation of microwave separation device of the present invention.Among the figure, 1. microwave generator tube, 2. vavuum pump bleeding point, material inlet 3. to be separated, 4. overflow plate, 5. isolating bar 6. distills back mother liquor outlet, and 7. baffle plate 8. is distilled the cut outlet, 9. cold plate, 10. cooling fluid enters the mouth, 11. condensation chambers, 12. cooling liquid outlets, 13. evaporating surfaces.
Fig. 2 distills the influence schematic diagram of progression to cyclohexane purity among the embodiment 8.
The specific embodiment
The separated material that dielectric constant is different places and makes it to form one deck liquid film on the flat board, put into microwave source after flat board put into airtight reagent bottle, driving vavuum pump treats to open microwave source and be adjusted to power demand after the pressure stability, after finishing, collects molecular clock the dull and stereotyped target components that goes up, close microwave, open exhauster regulating valve, collect target components, carry out content analysis with the Abbe refractometer.The present invention is further illustrated with the specific embodiment of different separated objects under different actual conditionses below.
With cyclohexane content is the cyclohexane-ethanol biliquid components system of 80.11% (mass fraction), and operating pressure is 16KPa, and microwave power is 462W, the microwave action time is under the condition of 20s, when thickness of liquid film is respectively 0.5mm, and 1.0mm, 2.0mm, 3.0mm, 4.0mm, 5.0mm the time, cyclohexane content becomes 97.278%, 95.904% respectively in the distillation substrate, 94.571%, 92.132%, 88.362%, 86.265%.
Benzene content is the benzene-ethanol biliquid component of 80.61% (mass fraction), and when operating pressure was 16KPa, microwave power was respectively 0W, 259W, 462W, 595W is under the condition of 700W, the microwave action time is under the condition of 15s, benzene content in ethanol-benzene distillation substrate is respectively 80.613%, 95.902%, 95.065%, 96.431%, 94.794%.
Cyclohexane content is the cyclohexane-ethanol biliquid component of 80.11% (mass fraction), and when operating pressure was 16KPa, microwave power was respectively that the microwave action time is 0,5 under the condition of 462W, 10,15,20,25,30,35,40,50, in the time of 60 seconds, the cyclohexane purity in cyclohexane-ethanol biliquid component is respectively 82.112%, 89.194%, 92.007%, 95.233%, 96.586%, 90.637%, 84.007%, 80.51%, 75.384%, 72.258%, 72.007%.
Benzene content is the benzene-ethanol biliquid component of 80.61% (mass fraction), when operating pressure is 16KPa, microwave power be under the condition of 462W the biliquid component microwave action time of isopropyl alcohol benzene be 0,5,10,15,20,25,30,35,40,50, in the time of 60 seconds, the benzene purity in benzene-ethanol biliquid component is respectively 81.117%, 93.848%, 94.774%, 96.433%, 94.203%, 84.565%, 83.353%, 79.509%, 74.502%, 70.365%, 69.741%.
Benzene content is the benzyl carbinol biliquid component of 80.61% (mass fraction), is 15s in the microwave action time, and microwave power is under the 595w condition, and system pressure is 0.06,1,11,16,21,41,61, during 100KPa, the benzene purity in benzene-ethanol biliquid component is respectively 99.986%, 99.794%, 98.58%, 98.555%, 97.387%, 94.897%, 90.401%, 88.955%.
Microwave molecular still structure of the present invention comprises vavuum pump bleeding point 2 as shown in Figure 1, material inlet 3 to be separated, overflow plate 4, slit 5, distillation back mother liquor outlet 6, baffle plate 7 is distilled cut outlet 8, cold plate 9, cooling fluid inlet 10, condensation chamber 11, cooling liquid outlet 12 and evaporating surface 13.
Separated material is added from charging hole 3, material drops on the overflow plate 4 along evaporating surface 13, along with material accumulates gradually, material will overflow gradually from the upper end of overflow plate 4, forming one deck liquid film flows along whole evaporating surface, and at the slit below overflow plate 5 flow fluid is redistributed, and the thickness of control liquid film makes that the thickness of liquid film is even.When the effect of material owing to gravity, when evaporating surface 13 constantly descended, under the effect of certain microwave 1 intensity and vacuum, light components will obtain energy and overflow from evaporating surface, and finally reaches on the cold plate 9.Material on the cold plate 9 is discharged from cut outlet 8, and the evaporating surface material is discharged from mother liquor outlet 6.Baffle plate 7 separates material that flows down from evaporating surface and the material that flows down from cryosurface.
Refrigerant is passed in the condensation chamber 11 from cooling fluid inlet 10, flows out from cooling liquid outlet 12, used refrigerant is the less material that does not absorb microwave of dielectric constant.
Adopting the microwave power of microwave generator tube 1 is 462W, material flow 1cm
3/ s, the different distillation of research pressure is as shown in the table to the influence of molecular clock effect in cyclohexane-ethanol system:
Adopting microwave molecular still of the present invention, is 462W at microwave power, material flow 1cm
3Under the condition of/s, measure in cyclohexane-ethanol system evaporating surface to the cryosurface distance to liquid film in the influence of component purity and yield, as shown in the table:
Adopting microwave molecular still of the present invention, is 462W at microwave power, and operating pressure is 1KPa, and feed rate is 1cm
3Under the condition of/s; Difference was separated the influences of progression to cyclohexane component content and yield in cyclohexane-ethanol system when evaporating surface was 35mm to the cryosurface distance.Stock blend cyclohexane crude product 51.477% component content after three grades of separation can reach 98.947%, and yield is 88.165%.Distillation progression to the influence of cyclohexane purity as shown in Figure 2.
Claims (7)
1. microwave separation method, it is characterized in that with the microwave being thermal source, under different vacuums, the separated materials different to dielectric constant heat, by the insensitive cold junction of microwave is cooled off collection to distillating part steam, realize separating of high-k and low-k mixture.
2. according to the described microwave separation method of claim 1, it is characterized in that may further comprise the steps: the separated material that dielectric constant is different places and makes it to form one deck liquid film on the flat board, put into microwave source after flat board put into airtight reagent bottle, driving vavuum pump treats to open microwave source and be adjusted to power demand after the pressure stability, after molecular clock finishes, close microwave, open exhauster regulating valve, collect target components.
3. microwave separation method as claimed in claim 2 is characterized in that the microwave distillation cold junction has microwave or shielding.
4. microwave separation method as claimed in claim 3 is characterized in that separated material accepts the liquid level of heating using microwave and be thin layer and distribute.
5. used device of the described microwave separation method of claim 1, at least comprise cold plate and distil container, it is characterized in that: cold plate is positioned at the distil container middle part distil container is divided into vaporization chamber and condensation chamber, the one side relative with cold plate is evaporating surface in the vaporization chamber, the top of evaporating surface is provided with overflow plate, overflow plate and evaporating surface have angle, and angle is positioned at the material inlet below, the end face of vaporization chamber has aspirating hole and material inlet, the bottom surface of vaporization chamber has mother liquor outlet and cut outlet, and is provided with baffle plate between mother liquor outlet and the cut outlet; The top of condensation chamber has cooling liquid outlet, and the bottom of condensation chamber has the cooling fluid inlet.
6. device according to claim 5 is characterized in that: have a slit below the overflow plate.
7. device according to claim 6 is characterized in that: slit is positioned at 1cm place, overflow plate below, and slit width is 0.5mm.
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| CN2008100489826A CN101342425B (en) | 2008-08-27 | 2008-08-27 | Microwave separation method and apparatus used thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115068972B (en) * | 2021-03-16 | 2023-08-15 | 上海梅山钢铁股份有限公司 | Crystallization tank capable of adjusting solid-to-liquid ratio of ammonium sulfate mother liquor |
Families Citing this family (6)
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| CN101797439B (en) * | 2010-03-02 | 2012-01-25 | 天津大学 | Microwave field reinforced molecular distillation separation device |
| CN102989319A (en) * | 2011-09-16 | 2013-03-27 | 中国科学院生态环境研究中心 | Apparatus and method for microwave enhanced membrane distillation process |
| CN102519782A (en) * | 2011-12-16 | 2012-06-27 | 天津大学 | Microwave field vapor-liquid equilibrium measuring device and determination method |
| CN105435485B (en) * | 2015-12-31 | 2017-05-10 | 宁夏东吴农化有限公司 | Radial type waste acid rectification device |
| CN106830140A (en) * | 2017-01-22 | 2017-06-13 | 广东美的厨房电器制造有限公司 | Microwave distillation component and the distilling apparatus with it |
| CN114381808B (en) * | 2021-12-27 | 2023-03-28 | 济南晶正电子科技有限公司 | Method for preparing composite film by microwave heating, composite film and electronic component |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115068972B (en) * | 2021-03-16 | 2023-08-15 | 上海梅山钢铁股份有限公司 | Crystallization tank capable of adjusting solid-to-liquid ratio of ammonium sulfate mother liquor |
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