CN1843552A - Decompressed microwave extraction device and method for extracting plant effective ingredient - Google Patents
Decompressed microwave extraction device and method for extracting plant effective ingredient Download PDFInfo
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- CN1843552A CN1843552A CN 200610044442 CN200610044442A CN1843552A CN 1843552 A CN1843552 A CN 1843552A CN 200610044442 CN200610044442 CN 200610044442 CN 200610044442 A CN200610044442 A CN 200610044442A CN 1843552 A CN1843552 A CN 1843552A
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Abstract
The invention discloses a decompression micro-wave extraction device and method on the plant effective component, which is formed by a micro-wave oven, an extraction pot, a condenser, a liquid-gas separator, and a decompression device. Wherein, the micro-wave oven is arranged outside the extraction pot, while the micro-wave generators are uniformly arranged inside the micro-wave oven; the extraction pot is mounted with electric mixer, while its top is mounted with magnetic eraser; the upper part of extraction pot is a extraction chamber, the lower part is mounted with a solvent warehouse, and they are separated by a baffle plate with uniform solvent penetrate holes. Via decompression and micro-wave, the gas solvent is condensed into liquid solvent via the condenser and fed back into the solvent warehouse via the cycle tubes; the plant via micro-wave radiation is discharged via the discharge device at the lower part of extraction pot; since said invention uses decompression and solvent cycle devices, the process that extracting plant effective components is accelerated; said components will not thermal deteriorated via high temperature; and the extraction rate and quality are improved to apply the industrial production.
Description
Technical field
The present invention relates to a kind of extraction element and method of effective ingredients in plant, relate in particular to a kind of decompressed microwave extraction device and method that effective ingredients in plant extracts that be used for.
Background technology
Active ingredient in the plant is provided with certain obstacle usually by plant cell tissue's embedding to extraction.The separation of active ingredient in the cell at first needs it is discharged in cell.For the separation of macromolecular substances, industrial most employing Mechanical Method or enzyme process are with born of the same parents' broken wall; And, then adopt solvent extraction method to carry out mostly for the separation of small-molecule substance.These method ubiquities extract that energy consumptions are big, and efficient is low, impurity is many, and yield is few, resource problem such as can not be fully used.
The Microwave Extraction technology is to utilize the electromagenetic wave radiation extract of frequency for 300HZ～300GHZ, makes that polar molecule produces high speed swinging and the phase mutual friction takes place in the extract, produces heat, the quick transmission of energy is provided and makes full use of.The microwave radiative process is that frequency electromagnetic waves penetrates spe medium on the one hand, arrive the inside vascular bundle and the glandular cell system of material, the polar molecule that dielectric coefficient is bigger in the plant absorbs microwave and produces heat, the cell interior temperature rises rapidly, vaporization or expansion take place, interior osmotic pressure increases and destroys the eucaryotic cell structure of plant, makes the diffusion duct become big, and extraction rate generation essence changes; On the other hand, under the effect of the friendship frequency electromagnetic field that when microwave treatment, produces, because the variation of extract Semi-polarity molecularly oriented causes rotation, vibration or the swing of molecule, aggravated the collision frequency of molecule in the system, the power that makes its constraint be extracted molecule reduces, make to be extracted molecule and to have entered a kind of state of activation and very easily stripping, quicken to be extracted the part composition to extractant interfacial diffusion speed.It is good that the Microwave Extraction technology has the extraction quality, the selectivity height, and rate of extraction is fast, and the extraction yield is high and impure few, rate of recovery height, characteristics such as less energy consumption.In recent years, microwave technology has obtained application in plant extract, is becoming a kind of novel, extracting method efficiently.
In the microwave abstracting process, no matter be polar extraction solvent (as moisture) and polarity active ingredient contained in polar extraction solvent or the plant cell, all will absorb microwave and produce heat, thereby the state variation of these polar molecules directly influences effect of extracting.Polarity active ingredient in the plant cell and polar solvent absorb microwave and produce heat and be heated, and cause the effective components in plants heating temperature too high and be damaged probably, and especially for the extraction of thermal sensitivity active ingredient, heating using microwave will cause heat damage.Adopt decompression operation, at first can reduce the polar solvent boiling point, reduce the effective ingredients in plant heating temperature, secondly can increase the mechanical stress on the plant cell wall, help broken wall.When decompressed microwave extracts, polar solvent will be vaporized rapidly and will be depressurized the device extraction, be to guarantee effect of extracting, must guarantee the extractant amount of active ingredient, and this just need make the solvent of extraction circulate rapidly.The decompression solvent circulation microwave extraction equipment and the method that with the effective ingredients in plant are application are not appeared in the newspapers.
Summary of the invention
Purpose of the present invention just provides a kind of Microwave Extraction efficient height, and the target component matter of extraction is measured, is used for decompressed microwave extraction device and method that effective ingredients in plant extracts.
For achieving the above object, the present invention adopts following technical scheme: a kind of decompressed microwave extraction device that is used for the effective ingredients in plant extraction, it comprises micro-wave oven, extractor is set in the micro-wave oven, extractor is connected with condenser, described condenser is connected with gas-liquid separator, and gas-liquid separator is connected with the solvent storage chamber of extractor bottom, and it also is connected with decompressor simultaneously.
Described micro-wave oven is interior, the periphery of extractor is provided with the layer of metal overcoat, arranges evenly that outside overcoat microwave generator, micro-wave oven outer wall and extractor are positioned at the microwave cavity of the sealing of outer wall section formation beyond the micro-wave oven.
Be extraction cell in the described extractor, the extraction cell top is provided with demagnetizer, and agitator is installed in the extraction cell, is provided with sealing device between agitator and extraction cell; Bleeding point and charge door are also arranged respectively at the top of extraction cell simultaneously; The bottom of extraction cell is connected with the solvent storage chamber by the dividing plate that has equally distributed solvent permeability hole; Solvent permeability hole aperture is 0.05～4mm, and the comminuted plants material is greater than solvent permeability hole aperture.
The bottom of described solvent storage chamber is provided with the circulation fluid inlet, and it is connected with gas-liquid separator by pipeline; The bottom of solvent storage chamber also has the solvent outlet simultaneously.
Described solvent outlet is provided with solvent and discharges control valve.
The bottom of described micro-wave oven and extractor is a device for discharging.
Described gas-liquid separator is provided with gas-liquid separator inlet, decompressing connection and gas-liquid separator liquid outlet, and decompressing connection links to each other with decompressor, and the gas-liquid separator inlet links to each other with condenser.
Cooling liquid outlet and cooling fluid inlet is arranged on the described condenser.
A kind of decompressed microwave extracting process that is used for the effective ingredients in plant extraction is sent into extractor with extractant through charge door with a certain amount of plant material pulverizing back; Start agitator, decompressor, start micro-wave oven, make the material of microwave radiation keep certain temperature; Under depressurization, solvent is vaporized rapidly, through condenser condenses, after the gas-liquid separator separates, enters the solvent storage chamber by liquid circulating pipe, overflows back extraction cell at last; The microwave abstracting certain hour stops micro-wave oven, decompressor, agitator after finishing successively, opens the solvent control valve, discharges solvent by the solvent outlet, again by the device for discharging discharging, will separate the target effective composition that can extract wherein after the solvent collection.
Described microwave radiative process reduces pressure continuously to extraction cell, and vacuum is 100～620mmHg post, and the extraction time is 2-120 minute; Described extractant has certain polarity, and dielectric constant is in 12～94 scopes.
The invention has the beneficial effects as follows: owing to set up decompression solvent circulation microwave extracting system, can make the quantity of solvent of microwave irradiation in the following microwave abstracting process of decompression keep stable, the recycling of solvent guaranteed around the plant cell that the target effective constituent concentration is lower in the middle of the solvent, thereby the active ingredient that has increased extraction process is transmitted motive force, has improved the decompressed microwave extraction rate.The while decompression operation; can increase the mechanical stress on the plant cell wall on the one hand; help broken wall; quicken the extraction stripping of active ingredient; can reduce the solvent vapourizing temperature on the other hand, thereby reduce the temperature of microwave irradiation active ingredient, improve the quality of extracting product; be particularly conducive to protection thermal sensitivity active ingredient, to avoid thermal metamorphism.
Description of drawings
Fig. 1 is a structural representation of the present invention;
Fig. 2 is the A-A profile of Fig. 1.
Wherein: 1. micro-wave oven, 2. extractor, 3. extraction cell, 4. bleeding point, 5. demagnetizer, 6. sealing device, 7. agitator, 8. charge door, 9. cooling liquid outlet, 10. condenser, 11. cooling fluids inlet, 12. gas-liquid separators, 13. the gas-liquid separator inlet, 14. decompressing connections, 15. decompressors, 16. the gas-liquid separator liquid outlet, 17. liquid circulating pipes, 18. flexible pipes, 19. the circulation fluid inlet, 20. devices for discharging, 21. solvent outlets, 22. discharge the solvent control valve, solvent storage chambers 23., 24. dividing plates, 25. solvent permeability hole, 26. sealing gasket, 27. microwave generators, 28. overcoats.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment invention is described further.
Embodiment one:
Among Fig. 1, the present invention is the microwave abstracting system of decompression solvent circulation, comprises that micro-wave oven 1, extractor 2, condenser 10, gas-liquid separator 12 and decompressor 15 form; The metal protection layer 28 outer microwave generators 27 of evenly arranging in the micro-wave oven 1, overcoat 28 is positioned at the periphery of extractor 2, as shown in Figure 2; Micro-wave oven 1 outer wall and extractor 2 are positioned at the microwave cavity of the sealing of outer wall section formation beyond the micro-wave oven, prevent the leakage of microwave.
In the extractor 2 is extraction cell 3, and demagnetizer 5 is arranged on it, stops microwave to be revealed and the metal sparking; Agitator 7 is installed in the extraction cell 3, to guarantee that material evenly mixes in the extraction cell 3, the place of being in contact with it is provided with sealing device 6, the top of extraction cell 3 also has charge door 8, bleeding point 4 simultaneously, bleeding point 4 is connected with condenser 10, the front portion of condenser 10 is a cooling liquid outlet 9, and the rear portion is a cooling fluid inlet 11.Condenser 10 is connected with the gas-liquid separator inlet 13 of gas-liquid separator 12, and the decompressing connection 14 on the gas-liquid separator 12 is connected with decompressor 15, and its underpart is connected with liquid circulating pipe 17, flexible pipe 18 by gas-liquid separator liquid outlet 16.Be provided with the dividing plate 24 that has equally distributed solvent permeability hole 25 in the bottom of extraction cell 3, the comminuted plants material guarantees the extractant free permeation greater than solvent permeability hole aperture, and material is difficult for spilling simultaneously.3 of dividing plate 24 and extraction cells are provided with sealing gasket 26.Circulation fluid inlet 19 is arranged at the bottom of solvent storage chamber 23, and it is connected with flexible pipe 18; Also have solvent outlet 21 simultaneously, the solvent of discharge control valve 22 is arranged on it.
In extractor 2 bottoms and micro-wave oven 1 bottom device for discharging 20 is set, starts device for discharging 20 extraction cell 3 of extractor 2 and solvent storage chamber 23 are separated, thereby lay down the material after the extraction.
Wherein, extractant has certain polarity (as water, acetone, ethanol water etc.), and dielectric constant is in 12～94 scopes.Microwave power 5～20KW, extractor volume are 0.0684m
3, solvent storage chamber volume is 0.0012m
3, comminuted plants material order number is 5～250 orders, solvent permeability hole 25 apertures are 0.05～4mm, the material that the solvent permeability hole diameter that uses is pulverized as plant 20～80% of the screen-aperture that sieves.
Extracting process of the present invention is, dried honeysuckle powder is broken into 50～100 orders, add weight of material 50～160%, concentration be 30%～90% ethanol in container fully wetting after, join again in the extraction cell of extractor, in extractor, add weight of material 200～800% then, concentration is 30%～90% ethanol, the volume of extractant and honeysuckle accounts for 30～70% of total extractor volume, vacuum is to heat under 100～400mmHg column condition in 2450MHz frequency microwave field, carry out the extraction of 5～20 minutes decompression solvent circulation microwaves, close microwave extracting apparatus after the end, collect extractant, filter, filtrate concentrates through reducing pressure and obtains chlorogenic acid medicinal extract.Compare with existing normal pressure microwave extraction method, the recovery rate of chlorogenic acid increases by 10%, and the purity of chlorogenic acid in medicinal extract improves 18%.
Embodiment two:
Extracting process of the present invention is, the dried root of large-flowered skullcap is ground in the extraction cell that 50～100 orders join extractor, in extractor, add weight of material 600～1200% water then, the volume of the water and the root of large-flowered skullcap accounts for 50～65% of total extractor volume, vacuum is to heat under 300～500mmHg column condition in 2450MHz frequency microwave field, carry out the extraction of 8～16 minutes decompression solvent circulation microwaves, close microwave extracting apparatus after the end, the collection extractant is placed on and is heated to 70～85 ℃ in the water-bath, and insulation 20～40min makes precipitation fully, leave standstill 10～14h, sediment separate out, with distilled water washing 2～3 times, the dry scutelloside crude product that gets.Compare with existing normal pressure microwave extraction method, the recovery rate of scutelloside increases by 6%, and the purity of scutelloside in medicinal extract improves 8%.
In the present embodiment, device therefor is identical with embodiment one with extracting process.
Protection content of the present invention is not limited to the extractions of above-mentioned two kinds of plants, also can be used for the extraction of other various effective ingredients in plant.
Claims (10)
1, a kind of decompressed microwave extraction device that is used for the effective ingredients in plant extraction, it comprises micro-wave oven (1), extractor (2) is set in the micro-wave oven (1), extractor (2) is connected with condenser (10), it is characterized in that: described condenser (10) is connected with gas-liquid separator (12), gas-liquid separator (12) is connected with the solvent storage chamber (23) of extractor bottom, and it also is connected with decompressor (15) simultaneously.
2, the decompressed microwave extraction device that is used for the effective ingredients in plant extraction according to claim 1, it is characterized in that: described micro-wave oven (1) is interior, the periphery of extractor (2) is provided with layer of metal overcoat (28), evenly arrange microwave generator (27) outside overcoat (28), micro-wave oven (1) outer wall and extractor (2) are positioned at the microwave cavity of the sealing of outer wall section formation beyond the micro-wave oven.
3, the decompressed microwave extraction device that is used for the effective ingredients in plant extraction according to claim 1, it is characterized in that: be extraction cell (3) in the described extractor (2), extraction cell (3) top is provided with demagnetizer (5), agitator (7) is installed in the extraction cell (3), is provided with sealing device (6) between agitator (7) and extraction cell (3); Bleeding point (4) and charge door (8) are also arranged respectively at the top of extraction cell (3) simultaneously; The bottom of extraction cell (3) is connected with solvent storage chamber (23) by the dividing plate (24) that has equally distributed solvent permeability hole (25); Solvent permeability hole (25) aperture is 0.05～4mm, and the comminuted plants material is greater than solvent permeability hole (25) aperture.
4, according to claim 1 or the 3 described decompressed microwave extraction devices that are used for the effective ingredients in plant extraction, it is characterized in that: the bottom of described solvent storage chamber (23) is provided with circulation fluid inlet (19), and it is connected with gas-liquid separator (12) by pipeline; The bottom of solvent storage chamber (23) also has solvent outlet (21) simultaneously.
5, the decompressed microwave extraction device that is used for the effective ingredients in plant extraction according to claim 4, it is characterized in that: described solvent outlet (21) is provided with solvent and discharges control valve (22).
6, the decompressed microwave extraction device that is used for the effective ingredients in plant extraction according to claim 1, it is characterized in that: the bottom of described micro-wave oven (1) and extractor (2) is a device for discharging.
7, the decompressed microwave extraction device that is used for the effective ingredients in plant extraction according to claim 1, it is characterized in that: described gas-liquid separator (12) is provided with gas-liquid separator inlet (13), decompressing connection (14) and gas-liquid separator liquid outlet (16), decompressing connection (14) links to each other with decompressor (15), and gas-liquid separator inlet (13) links to each other with condenser (10).
8, according to claim 1 or the 7 described decompressed microwave extraction devices that are used for the effective ingredients in plant extraction, it is characterized in that: cooling liquid outlet (9) and cooling fluid inlet (11) is arranged on the described condenser (1).
9, a kind of decompressed microwave extracting process that is used for the effective ingredients in plant extraction is characterized in that: a certain amount of plant material pulverizing back is sent into extractor (2) with extractant through charge door (8); Start agitator (7), decompressor (15), start micro-wave oven (1), make the material of microwave radiation keep certain temperature; Under depressurization, solvent is vaporized rapidly, and through condenser (10) condensation, gas-liquid separator (12) enters solvent storage chamber (23) by liquid circulating pipe (17) after separating, and overflows back extraction cell (3) at last; After the microwave abstracting certain hour finishes, stop micro-wave oven (1), decompressor (15), agitator (7) successively, open solvent control valve (22), discharge solvent by solvent outlet (21), by the device for discharging discharging, the target effective composition that can extract wherein will be separated after the solvent collection again.
10, the decompressed microwave extracting process that is used for the effective ingredients in plant extraction according to claim 9, it is characterized in that: described microwave radiative process reduces pressure continuously to extraction cell, and vacuum is 100～620mmHg post, and the extraction time is 2-120 minute; Described extractant has certain polarity, and dielectric constant is in 12～94 scopes.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100462121C (en) * | 2006-10-23 | 2009-02-18 | 天水华圆制药设备科技有限责任公司 | Continuous extracting method of microwave |
| CN101543686B (en) * | 2008-03-28 | 2011-10-26 | 湖北中烟工业有限责任公司 | Multifunctional microwave extraction apparatus for extracting fragrances and flavors from Chinese cigarette |
| CN101209384B (en) * | 2006-12-26 | 2012-01-04 | 上海屹尧分析仪器有限公司 | Continuous type microwave extracting device |
| CN104957620A (en) * | 2015-07-02 | 2015-10-07 | 河源市探索人发明科技有限公司 | Extraction method applied to medicinal or edible material |
| CN106867828A (en) * | 2017-04-24 | 2017-06-20 | 贵州省仁怀市茅台镇永泰酒业股份有限公司 | A kind of Quick production method of Chinese chestnut wine |
| CN114849275A (en) * | 2022-05-18 | 2022-08-05 | 郑州远洋油脂工程技术有限公司 | Ethanol extraction process of powdery material |
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| CN102847340B (en) * | 2012-09-25 | 2014-05-14 | 湖北民族学院 | Full-automatic traditional Chinese medicinal material ingredient extracting device |
Family Cites Families (4)
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| FR2705035B1 (en) * | 1993-05-11 | 1995-08-04 | Archimex Pibs | Process and installation for solvent-free extraction of natural products by microwave. |
| EP1618798B1 (en) * | 2004-07-20 | 2009-01-07 | Milestone S.r.l. | Microwave extraction of volatile natural substances |
| CN2748147Y (en) * | 2004-12-17 | 2005-12-28 | 邹世春 | Ultrasonic microwave digestion extraction arrangement |
| CN2885375Y (en) * | 2006-03-10 | 2007-04-04 | 山东轻工业学院 | Decompression microwave extraction device for plant active ingredient extraction |
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- 2006-03-10 CN CNB2006100444421A patent/CN100421759C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100462121C (en) * | 2006-10-23 | 2009-02-18 | 天水华圆制药设备科技有限责任公司 | Continuous extracting method of microwave |
| CN101209384B (en) * | 2006-12-26 | 2012-01-04 | 上海屹尧分析仪器有限公司 | Continuous type microwave extracting device |
| CN101543686B (en) * | 2008-03-28 | 2011-10-26 | 湖北中烟工业有限责任公司 | Multifunctional microwave extraction apparatus for extracting fragrances and flavors from Chinese cigarette |
| CN104957620A (en) * | 2015-07-02 | 2015-10-07 | 河源市探索人发明科技有限公司 | Extraction method applied to medicinal or edible material |
| CN104957620B (en) * | 2015-07-02 | 2017-03-01 | 河源市探索人发明科技有限公司 | It is applied to medicinal or edible materials extracting method |
| CN106867828A (en) * | 2017-04-24 | 2017-06-20 | 贵州省仁怀市茅台镇永泰酒业股份有限公司 | A kind of Quick production method of Chinese chestnut wine |
| CN114849275A (en) * | 2022-05-18 | 2022-08-05 | 郑州远洋油脂工程技术有限公司 | Ethanol extraction process of powdery material |
| CN115487536A (en) * | 2022-10-25 | 2022-12-20 | 湖南农业大学 | Large Soxhlet extraction equipment and method for extracting materials |
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