CN1032041C - Microwave assisted process for extraction and apparatus therefor - Google Patents
Microwave assisted process for extraction and apparatus therefor Download PDFInfo
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- CN1032041C CN1032041C CN 91110686 CN91110686A CN1032041C CN 1032041 C CN1032041 C CN 1032041C CN 91110686 CN91110686 CN 91110686 CN 91110686 A CN91110686 A CN 91110686A CN 1032041 C CN1032041 C CN 1032041C
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Abstract
There is disclosed a method and apparatus for extraction of essential and other such oils from biological matter by exposure to microwave energy. The method involves exposure of microwaves to the oil containing cellular matter of the glandular system to extract the oil into a suitable non-aqueous organic medium after disruption of the oil containing cellular matter. The apparatus includes microwave applicators, solvent and starting material, storage means and multiple stages of treatment resulting in a high quality extracted product.
Description
The present invention relates to a kind of improved method, product and equipment thereof that utilizes microwave energy from biological material, to extract the solubility natural products.
The now existing multiple method of utilizing microwave.For example Gannon is at us4, and the method for narration after the cereal fatty and oily with microwave drying, is removed the peel the extraction grease subsequently in 464,402.In addition, the method that Ganzler and salgo delivered on the z.Lebensmunters Forsch184:274-276 page or leaf in 1987, this method is utilized the microwave heating extraction medium.In these examples, microwave irradiation is mainly used in heating extractant medium.
Collins is at us4, in 554, No. 132, disclosed and used microwave drying food, utilize solvent-extracted method again, but he do not point out extraction process.
GB1,209,675 have narrated and have utilized microwave irradiation, make the enzyme deactivation in the palm fruit, and use the solvent extraction palm oil.
People such as Heitkamp are at CA987, point out in 993, and when containing certain humidity and suitable solvent, as tobacco or tealeaves etc., its in-house smell and aroma ingredients can be moved to the surface at microwave action.But they do not propose any these smells and aroma ingredients to be extracted the better method of going in the medium that is extracted.
In addition, people such as Craveiro, at Flavour and Fragrance Journal4,1989, discussed among the 43-44 that plant material is placed air stream, utilize microwave irradiation to produce the method for volatile oil then.
Ganzler, salgo and valko be at Journal of Chromatography371, and 1986, disclose the method for utilizing microwave preparation organic phosphate pesticide, anti-nutraceutical (antinutrtives) and natural fat sample among the 299-306.Dry sample raw material is suspended in the organic media after wearing into particle.People's such as Ganzler this method has just mechanically been destroyed body of gland in the dried feed and dimension pipe before microwave treatment, thereby has caused the loss of volatile oil, simultaneously, some materials that obtain also can occur not expecting.The separation of these materials will take a long time.In addition, this method is also pointed out, after the suspension cooling, reuses microwave irradiation.Like this, under the situation that volatile oil and extractant do not reclaim fully, just heat.
Steam distillation and solvent-extracted method are well-known, but adopt high temperature and dangerous organic solvent, can produce pollutant.
Therefore, need a kind of microwave induced extracting process and equipment that is not subjected to above-mentioned limitations affect, it can obtain maximum production, can reclaim volatile oil and other utilities in the cell biological material again.
The invention provides a kind of more selective, more efficiently extraction scheme that is used for extraction of natural products.
The present invention utilizes microwave energy to make with the body of gland of the contacted biological material of a certain amount of non-aqueous organic solvent or produce a rapid temperature rise sometimes in its skeleton.
One aspect of the present invention is to provide the method for extracting volatile oil from grease-contained biological material.It comprises: a kind of biological material source that comprises complete basically body of gland system is provided, and this material has enough humidity can utilize microwave energy extraction volatile oil.In the method, this material floods to obtain described volatile oil with non-water extractant earlier.The irradiation that utilizes microwave energy then produces the different temperature difference on material and extractant, therefore volatile oil is discharged from raw material and extract, simultaneously, these volatile oil that are extracted out from material will be by the low extractant cooling of temperature, therefore, oily temperature will be lower than the oil temperature that just extracts from raw material in extractant.The entire process process can comprise separates residue and reclaims described grease in the extraction oil from solvent.
The invention still further relates to a kind of equipment that is used for extracting volatile oil and other materials, comprising from biological material:
At least one microwave high-frequency heating electrode (Microwaveapplicater);
A blending tank that mixes described biological material and extractant;
From first mixture of described blending tank conveying biological material and extractant, the pump installation that the described microwave high-frequency heating of process electrode is handled;
The device that separates the extractant that includes extract liquid the mixture after handling;
The extractant of separating is recycled with pending biological material mix, and form the device of second mixture; With
Supply with the device of described second mixture to microwave high-frequency heating electrode.
The invention still further relates to a kind of method that from the biological material that contains volatile oil, obtains volatile oil, comprise the steps:
The biological material of the complete body of gland of a kind of tool system is provided, and this biological material has enough moisture to be enough to allow to adopt microwave energy to extract described volatile oil;
Surround described biological raw material to extract described volatile oil with non-water extractant;
With the described biological material of microwave energy irradiation, between described biological material and described non-water extractant, to produce the difference heating, coming together from described biological material whereby described volatile oil, comes together the volatile oil that to be lower than come together temperature when of the volatile oil that comes together from biological material from biological material with described non-water extractant cooling.
One of the present invention method is preferably immersed in a kind of non-water organic extractant for the biological material that will have grease-contained described cellular material, and this material source has complete substantially body of gland system and moisture, guarantees to make in microwave processing process body of gland to break.Then, use this biological material of microwave energy irradiation again, when the material temperature rise extremely enough caused the body of gland system destruction, the volatile oil in this biomaterial will be extracted in the organic extractant.
Grease through this operation extraction will cool off with extractant.Then, in the extractant that extra biological material adds to again, at this moment, contained the grease that from the first step, comes together in these extractants.Same material and this extractant are placed under the microwave irradiation, and the material in the extractant that at this moment obtains is warming up to the degree of the body of gland system destruction that can make wherein again, around oil is wherein then come out by collection and is diffused into.This procedure can constantly repeat, and correspondingly, these greases can be separated from the extractant that obtains like this.
The benefit of Chu Liing has been to reduce common required solvent load like this, has also obtained the extract that concentrates simultaneously.
Opposite with additive method, the present invention makes material more preferably obtain processing than solvent and makes its absorption microwave energy, like this, the grease solvent around it that comes together after obtains cooling, thus the grease that can cause when having avoided microwave treatment or the thermal decomposition of some sensitive materials.
Therefore, applicant's method is one so-called " cold working ", and wherein, solvent does not absorb microwave energy, so nearly all microwave energy all is passed to processed material.The temperature difference between material and the extract has guaranteed that grease is transferred in the extractant.
Organic matter, for example hexane or other suitable non-water aliphatic series organic matters all are reasonable extractants.Usually, these materials all are " microwave transparency ", and promptly they can not absorb microwave energy in a large number owing to lack molecular dipole moment.Also can use cosolvent.The quiet dielectric constant of these extractants perhaps, should be transparent to the microwave frequency of microwave source generally between 0 to 28.
If biological material lacks moisture, before microwave treatment, in material, add solvent so with pure dipole moment, make material rehydration or dissolve in once more, these solvents with net dipole moment will be opaque for microwave, for example, and the mixture of methyl alcohol, ethanol and these solvents etc.
If use the translucent organic solvent of a kind of microwave, so, in microwave processing process, the temperature of this solvent will be lower than biological material, the temperature of the grease that especially is extracted.
In addition, the present invention also adopts the spe medium system, and for example a kind of single extractant or two or more suitable and the extractant solution that mixes are used for obtaining the oil of rectifying respectively.
Use the raw material of not pulverizing to handle to obtain than grinding to such an extent that the raw material of doing pulverized is handled and obtained much better result.With almost being whole or the material of bulk has been avoided destruction to body of gland and vascular system, thereby can obtain high-quality and more valuable desirable product.
Gland tissue is meant that mainly those secrete various secretion, mainly is the histoorgan of honey.Vascular tissue then refers to the passage of those fluid transfers.Usually, the volatile oil that extracts in the biology comprises the essential oil in the body of gland system.This grease has the taste and the fragrance of material, is usually used in doing spices and flavouring.FOR ALL WE KNOW the road is such, and volatile oil is that the main distinction of essence wet goods and expressed oi such as cottonseed oil, linseed oil or coconut oil just is that the former is not a fatty glyceride.
This notion of volatile oil also comprises in the Plants and Animals raw material, essential oil and other lipoidis for example for example, aliphatic acid, fatty wet goods material, these materials can will come together in their bodies of gland from corresponding animal-plant material or the similar system with the method for the present invention narration.
The present invention is applicable to many kinds of biological tissues, for example is used to make plant tissue or its hetero-organization of spices, as animal tissue.These plant materials comprise mentba canadensis (Canadian pepper mint), seaweeds such as Irish moss, various vegetables such as onion, garlic and some other similar plant.Those animal materials are for example liver, kidney, yolk etc. or product then, as sea anemone, sea cucumber; Shell class animal such as lobster and other shellfish are arranged, and warm water and cold water fish or the like all can be used to refine pigment, grease or the like.A very tempting purposes is from the organ such as liver of fish, extracts required grease, and these organs are as pharmacy and human source of using needed acid, and these volatile oil are for example Ω-3 and Ω-6 oil and analog thereof.
Specifically, the invention provides the equipment that from biological material, extracts essence and other materials.This equipment comprises having a microwave high-frequency heating electrode at least and carry the device of biological material and the mixture of extractant through this electrode, and the device of removal extractant the separating liquid and the liquid after filtering also is provided from processed mixture.
The microwave high-frequency heating electrode comes work by known parameter usually, rated power for example, and greatly between 200 to 10,000 watts, frequency is greatly about 800 to 30,000MHz or higher.Usually, as long as a certain component in the material has to a certain degree absorption for a certain wavelength in the microwave spectrum, the wavelength of this microwave just can use.Only need change the difference that exposure time remedies degree of absorption a little.Several different microwave high-frequencies heating electrodes can be provided simultaneously.
Solvent reservoir and colvent inlet and sample inlet device that this equipment also provides the material that adapts with organic solvent to make.Available proper device such as pump are sent into mixture or process microwave high-frequency heating electrode.In order to remove residual plant material, make mixture continuously by filter, as filter paper or polytetrafluoroethylene (PTFE) sieve etc.In addition, these equipment also comprise the device of removing moisture content from the sample that desire is handled, and this device can comprise and can be added in the filter as separation phase, and for this purpose and the drier that uses.
Described material preferably pump is separated solvent to separator such as rotary evaporator etc. from described oil-containing material.Solvent then can be by in addition condensation of condenser.
Use the suitable connecting line that is used for microwave treatment, as glass tube, polytetrafluoroethylene (PTFE), quartzy or other microwave equipment is connected to each other described equipment, and in addition, described pipeline comprises suitable valve, for example, glass or polytetrafluoroethylene (PTFE) pipe close or the like.
To illustrate optimum implementation below, wherein;
Fig. 1 is the schematic diagram of present device;
According to the present invention, be generally: microwave radiation is the spe medium by microwave freely, (the microwave medium can determine it is that those quiet dielectric constants are less usually to reach interior body of gland of biological material and skeleton, that is do not have a material of net dipole moment, quiet dielectric constant as hexane is 1.9, and the quiet dielectric constant of carbon tetrachloride is 2.2, liquid carbon dioxide, when the pressure of 0 ℃ and 50atm, quiet dielectric constant is 1.6).And the bigger material of those quiet dielectric constants, water for example, quiet dielectric constant reaches 80.4.In extraction process, material has absorbed a part of microwave radiation, and absorption coefficient then depends on the water content (or the absorption microwave component of adding what) of material widely.After such processing, material inside will produce rapid temperature rise, and this temperature rise is particularly evident in body of gland and skeleton.This temperature rise will last till always when intracellular pressure has surpassed the expanding ability of cell membrane that therefore cell membrane breaks.Material in the cell flow out cell arrive around in the medium of lower temperature, separate and dissolve described oil.Solid material is separated, and the solution of gained can be with handling with the identical mode that other natural products extractions are adopted.
The consumption that is used to contact the extractant of dipping material can change in a big way.Common consumption is to make it to be enough to all to come together from biological material with physics mode all required compositions, and extractant can be 1: 1 to 20: 1 with the ratio (liter/kilogram) of used material.
The plant material that newly is extracted is found when electron microscopy, with the mentba canadensis is example, behind 20 seconds microwave-induced extraction, the degree of breaking of its body of gland is suitable with degree behind 2 hours conventional steam distillation and 6 hours the Soxhlet extractron (soxhlet extraction procsses).Electron microscope has also been explained relatively and has been changed as extraction in 2 to 3 minutes through the short time, obtained the high-quality situation of extract.So just can adjust penetration power, to obtain best effect according to spe medium.If make solvent with hexane, from peppermint, extract volatile oil, short time extraction and raw material are fresh and complete, and the pigment and other composition of not expecting that just do not have in the solvent in the plant material occur.Conventional steam distillation and other extracting process use the raw material after the pulverizing usually, compare with the present invention, and the last size of using is quite crucial in these methods, therefore, has increased extra step again.Macroscopic examination confirms, the respective substance that the contained pigment composition of the material that utilizes the present invention to extract obtains far below steam distillation.
The present invention uses the spe medium system, and this system can be single extractant or two or more extractant solution.In order to obtain the fractional extraction thing as early as possible, can be on same equipment fractional extraction sequentially.And prior art needs the substep distilation steps, and not only expense is high and time-consuming for it, and needs a variety of equipment, and therefore the amount of investment that needs is very big.The present invention then make manufacturer can be in same place, same equipment, use and compare the less time than prior art and carry out a series of extraction and rectifying.
Extracting the required exposure time of described grease generally changes with plant or other biological material difference.Typical case's time is between about 10 to 100 seconds.The water content difference of raw material, exposure time also should be different.The raw material water content should be between 25% to 90%.This extracting process can be applicable to be produced in batches and produces continuously.
Product can reclaim from extractant (after the residual solids plant material that sieve in week, filtration or centrifugation goes out) with suitable known recovery technology, separates later extractant and can recycle mutually, need not purifying once more.
The following describes the example that some utilize microwave-induced extraction method of the present invention.Wherein, all improve for the body of gland and the skeleton of the various different materials that break with this paper unique mode.These comprise with the conventional extraction processes comparison, the quality of productive rate, extract for example, the reduction of induction time and producing cost, expense of raw materials reduces owing to having reduced the processing expense of raw materials, reduce operating procedure, reduce the damage of caused by operations, also have some comprehensive improvement people and equipment.
Embodiment 1
Monarda fistulosa (Monarda fistulosa) is new varieties in the peppermint, also is a kind of novel manufacturing flavouring and the parent material of spices, contains in its essential oil than the much higher geraniol in other kind of U.S. menthol spp.For comparison purpose, extract the essential oil of Monarda fistulosa in this way.In the present embodiment, 30 gram fresh plant raw materials are torn into suitable bulk (deal same with steam distillation), and it is placed in 400 milliliters the beaker, with 175 milliliters of hexane submergence materials, note the temperature of mixture.Be subjected at mixture (500 watts of power, frequency 2450MHz) behind 15 seconds the microwave irradiation, write down the temperature of medium again, final step is that above-mentioned steps is repeated twice, needn't do further temperature survey (that is total microwave irradiation time is 45 seconds, carries out four temperature surveys altogether) again.During irradiation, data show that the inside plants temperature begins to raise, thereby have set up temperature required gradient, and this thermograde has guaranteed grease is extracted in the lower hexane of temperature expeditiously.Because passive heat transfer, solvent is at microwave irradiation 0,15, and temperature only reaches 15,29,44 and 57 ℃ respectively in the time of 30,45 seconds, and its productive rate is 1.49%.
Plant material is because moisture, in the cell temperature up to 100 ℃ about.Though ICW can infiltrate the minor variations that causes the hexane temperature in the hexane, this changes with respect to oily temperature is quite low.
After the cooling of the mixture of extractant medium and grease, removing the moisture content of trace, and wash with 50 milliliters of fresh hexane with a spot of sodium sulphate filtering mixt.Utilize the gas-chromatography bond quality to select detector analytical extraction liquid and definite productive rate (mass spectrometric data can compare with the normal data in library).The results are shown in the Table I.
Experiment above repeating is filtration step to the last.Just extract is used as spe medium in other two groups of experiments, that is: the plant material of coextraction 90 grams (90 gram raw materials are divided into three parts, every part 30 gram, every part of irradiation three times, each 15 seconds), but only use a hexane.All extracts all pass through a small amount of sodium sulphate and filter, with other 50 milliliters fresh hexane wash.Same methods analyst content and definite productive rate above utilizing.In experimental error, productive rate (1.54%) is consistent with above-mentioned conclusion with the sample composition.The analysis knot that Table I is summed up shows because microwave auxiliary extraction method has the advantage that increases geraniol content in the extract, therefore to have very big commercial value.
Table I composition relative concentration
Microwave treatment steam distillation octene-3-alcohol (octen-3-o1) 0.23 0.28 laurene 0.59 p-cymene 0.12 α-terpinenes (0.21 0.96 linalool (Linalool), 0.37 0.62 neral (Neral), 0.57 0.33 geraniol (Geraniol), 98.48 94.83GermacreenD, 0.14 14.7 total amount 100.00 99.20 of α-Terpinene)
Repeat, use microwave auxiliary extraction continuously, use appropriate solvent simultaneously, the productive rate (0.94%) the when productive rate of extract will use separately greater than the steam distillation of routine.Simultaneously, time of being spent of evaporate to dryness extract also has only 1/3rd of common process.This method has not only improved treatment effeciency, and has reduced manpower cost, energy consumption; In fact, the committed step of decision speed just is the minimizing or the evaporation of solvent in the microwave extraction process.In the superincumbent experiment, only need just can finish three extractions less than ten minutes, and will finish same work, steam distillation then needs at least 8 hours.
Embodiment 2
With water content is that 30% complete garlic clove is immersed in 250 milliliters the carrene.At 625 watts, the microwave power of 2450MHz is irradiation 30 seconds next time with the sample that soaks.Use quite complete sample to confirm that resulting extract contains those compositions of not expecting hardly, quality is fairly good.Contain 22.2% diallyl sulfide in the product, 28.4% 3-vinyl-1,2-two thiophenes-5-alkene, 49.4% 2-vinyl-1,3-two thiophenes-4-alkene.Here utilize the analysis result of the product that this method obtains to be referred to as " microwave-2 " (μ-wave
2).
In order to compare, garlic samples is handled with following already known processes respectively: water diffusion (Hydrodiffusion) (HD
1); Steam distillation (HD
2) (hydrodistillation); Carbon dioxide supercritical extraction (CO
2) and use the impregnated garlic of solvent (carrene) to carry out (four times) irradiation 125 seconds (microwave-1, μ-wave with microwave
1).
Table II composition HD1 HD2 CO2 microwave-1 microwave-2 allyl methyl sulfide 12.3 dimethylsulphides 1.41 diallyl sulfides 1.33 3.89 allyl methyl disulfide compounds 3.05 5.32 5.58 8.12 methyl-prop-1-thiazolinyl disulphide 5.41 methyl-prop-2-thiazolinyl disulphide 1.26 dimethyl trisulfides 1.12 diallyl disulfides 31.2 30.7 16.7 17.7 22.2 dipropyl disulfide compounds 1.38 1.83 third-2-thiazolinyl disulphide 4.76 6.88 1.41 allyl methyl trisulfide compounds 11.2 12.4 7.383-vinyl-1; 2 two thiophenes-5-alkene, 23.3 4.47 28.42-vinyl 1,3-two thiophenes-4-alkene 1.84 46.5 34.3 49.4 diallyl trisulfides 33.8 22.4 dipropyl trisulfides 2.29 triallyl tetrasulfides 1.04 dipropyl tetrasulfides 4.24 1.32
In the table, HD
1Represent the hydrogenation diffusion; HD
2Represent the hydrogenation way of distillation; CO
2Representative CO
2Supercritical fluid extraction; Microwave-1 expression is carried out totally 125 seconds microwave irradiation four times with the impregnated garlic of carrene; Complete garlic clove in the microwave-2 expression carrene carries out one time 30 seconds microwave irradiation.
Data in the Table II clearly illustrate that, just 30 seconds microwave irradiations and colder medium are used to extract various compositions simply; The present invention has also surpassed widely such as conventional methods such as water diffusion method, vapor distillation method, supercritical extractions.The more important thing is the microwave abstracting of the longer time irradiation that has surpassed the impregnated mistake of sample.
Embodiment 3
The pectoral fin of fresh rainbow salmon (salmon galrdneri), dorsal fin and head are promptly as the raw material that extracts for the first time (38.5 gram).On one's body same fish, internal organ are partly told, can be as the raw material (34.9 gram) of extraction for the second time.
According to the present invention, every kind of these raw material uses same extractant, places (3 * 15 seconds) under a series of microwave abstracting processes.Identical among equipment and the embodiment 1, the extractant of use is hexane (60 milliliters every part), and these hexanes are with the complete submergence of raw material.Must be noted that these raw materials all are the states of not pulverizing.In addition, the temperature maintenance of extractant is at the grease that the extractant cooling is extracted from these materials.
The grease that extracts in the initiation material is then separated from hexane with the method that the front was described, and analyzes the product that reclaims and understands its content of fatty acid.
Disclose on the agricultural handbook 8-15 (United States Department of Agriculture, 1987) and utilized conventional method extruding rainbow salmon, its essential oil and edible have partly been separated, about like this lipoid of 3.4% that can obtain altogether.Usually, extrusion technique is quite time-consuming.Utilizing the present invention, is raw material with fin and a spot of flesh of fish only, resulting essential oil just with routine techniques suitable (3.9%), and in routine techniques, always all edibles with fish partly are raw material.On the other hand, when being raw material with the internal organ of fish, the content (16.1%) of essential oil that the present invention obtains almost is five times of commonsense method (3.4%).
Fig. 1 shows equipment used in the present invention.The holder 10 that tool inlet 11 and inlet 12 are wherein arranged, wherein entering the mouth 11 is used to add biological raw material and enters the mouth and 12 be used to add above-mentioned solvent, and solvent can be stored in the solvent reservoir 13.Valve 14 control solvents are to holding vessel 10 feed.The mixture of solvent and biological raw material stirs with agitator 15.Pump 16 passes microwave high-frequency heating electrode 17 with the solvent and the plant material conveying that mix, and the typical calibration power of this microwave high-frequency heating electrode is 200 to 10,000 watts, and typical operating frequency is 800 to 30,000MHz.Pump 18 is sent into raw material and the solvent handled in the filter 19.Also microwave source can be contained in the feeder sleeve and with it and be enclosed in the feeder sleeve.So just can use metal tube (as steel pipe), only need the fixed cover of strengthening simultaneously.After microwave acts directly on the raw material,, cell rupture goes cooling in the extractant thereby being released into grease or other materials.The various piece that is appreciated that this equipment is connected with suitable pipeline, and these pipelines can be polyfluortetraethylene pipes, the pipe that glass tube and other suitable material well known to those skilled in the art are made.Be typically, the described diameter that is used to connect the pipeline of this system's each several part is about 1 to about 10cm, it is desirable to be about 2 to 5cm.
The invention still further relates to a kind of extraction equipment of being made up of a plurality of microwave high-frequencies heating electrodes, its described microwave high-frequency heating electrode is installed with following a kind of form, (a) be installed in series, and b) parallel installation, or (a) and (b) combination installation;
Act on each microwave high-frequency heating electrode of diameter for mixture mobile in about pipeline of 1 to 10cm;
The device of mixed extractant and pending material; With
This mixture is supplied with the device of each pipeline.
In a kind of form of the present invention, equipment comprises a plurality of microwave high-frequency heating electrodes 17, and each electrode is control separately all.Applicator 17 can in series be installed between pump 16 and 18, perhaps install in parallel to each other, or further both combines.Like this, a large amount of materials of each holding vessel 10 can be handled simultaneously, or a charging reprocessing.
In addition, the invention still further relates to a kind of equipment that is used for extracting volatile oil and other material, comprising from biological raw material:
The microwave dielectric heating electrode of a plurality of arranged in series;
Borrow little cross section container or pipeline that biological material and extractant mixture are carried the feeding device that passes described a plurality of microwave high-frequency heating electrodes; With
The EGR of the biological material after recycling described extractant and handling.
Being installed in series of the described applicator 17 that specially refers to, it has many benefits.If the material of preparing to be extracted is contained in the different compartments, as the capsule bag, cell, subcellular structure, and these spaces are surrounded by different structure, its effect as " wall " that build up, these spaces need continuous series to handle like this and just can be extracted into required material just like the chorista of different media, film or other different densities, thickness or swelliong power.Comprise in the water in the aforesaid various example or protein (meat) in adipose capsule, and the content in the plant chlorophyll vacuole.
About the control respectively of the described applicator 17 that is installed in series, can adopt short time difference irradiation so that the space structure of selecting destroys, extract the material of selection whereby.This is with using 17 radiation treatment differences of single applicator, because a radiation treatment needs the long time of staying, and carries out long irradiation and just can obtain the similar rate of recovery, and with lower selectivity.Shown among the embodiment as favourable installation arrangement described herein, with the microwave extractant and have the plant material mixture pumping of the vacuole of two or more type pass narrow tube (as, 2 to 5cm diameters), by three microwave high-frequency heating electrodes 17, sequentially carry out the short time (as 3～6 seconds) irradiation for 17 times at each electrode, compare with same mixture exposure time under single electrode, desirable in the former end product " A " component concentrations is higher.The irradiation of identical time will cause the rate of recovery low, and have different extracted components.If exposure time extended to obtain the identical rate of recovery that produces with irradiation repeatedly, it extracts component can be different greatly, and usually undesirable.This selectivity can not obtain from other method, even it is also not all right to use centrifugation apparatus simultaneously.Those of ordinary skills are that any suitable sample extraction device can be inserted in each microwave high-frequency heating electrode 17 described equipment afterwards happyly, increase selectivity, or remove those too much reluctant components effectively, thereby make these components can be owing to excessive microwave irradiation is degraded.
In the parallel installation about applicator 17, as seen its advantage for example is, make material to be processed to select flow rate to pass to be installed in little directly each applicator of (parallel installation in large quantities) in conduit, and there is the suitable time of staying, under even temperature, extract, this ability that obtains desirable productive rate is direct advantage, this parallel installation of little pipeline has avoided reducing the appearance of effect factor, for example, when handling once big capacity, the hot-spot of material or shortage of heat can produce artifact or reduce productive rate.
The another kind of advantage of a kind of installation of back comprises reducing produces and running cost, has reduced complexity of plant design or the like.In addition, this installation provide a kind of operation that can directly measure (as, if 10 applicators are installed by system, then can increase production 10%), and provide a kind of equipment that in this operating process, can be safeguarded.
With reference to aforementioned, by series connection and the parallel installation microwave high-frequency heating advantage that electrode brought, to connect and the use that mutually combines of the parallel installation high frequency generating utmost point, can have extra effect, promptly in an arranged parallel assembly, each assembly can comprise the series connection applicator with overall merit.
Let us returns described basic equipment aspect and comes, and a plurality of filters are installed in the filter, available in these filters also can be without drier, and these filter effects are identical.So just can guarantee under the situation of closing device not, from each filter, to dispose the biosolids residue termly.
Solvent that filters out from filter 19 and grease are transported to separator 21 with pump 20, perhaps through valve 51 and 52 and pipeline 50 be recycled in the microwave high-frequency heating electrode 17 with further processing.With gasifying solvent, heating is by temperature controller 23 controls by external heater 22 heating for separator 21.Material residual in separator 21 excludes from exporting 24 termly by by-pass valve control 25.
Solvent after the vaporization is by condenser 26, and the solvent of condensation is sent to main memory 27, and then, by control valve 28, solution is sent to solvent reservoir 13 again.Also can do accommodation slightly, make the solvent of condensation directly deliver to solvent reservoir 13.
In order to increase the extraction in the filter, the solvent of some condensation also can be delivered to filter 19.This by control valve 31 and 32 and pipeline 30 realize.In order to make the instrument internal pressure identical, various relief valve also is housed as 33 and 34 with atmospheric pressure.
This complete equipment obtains essential oil for the gland cell that utilizes broken microwave to contain essential oil and other materials are very useful.This complete equipment can also be used in combination with some other conventional equipment, for example between microwave high-frequency heating electrode and filter 19 flow divider 40 is installed.According to different operating positions, the mixture of biological raw material and solvent can be delivered to filter 19 by this valve, these top just described shape feelings.Also mixture can be delivered to a conventional steam distillation device by tube connector 41.And in this case, solvent for use is a water, and when the mixture of biological raw material and water was handled in microwave high-frequency heating electrode, water was heated.Change a kind of method and use, also can under pressure, add hot water with the microwave high-frequency electrode 17 that generates heat to the phase of vaporizing, water vapour condensation during by tube connector 41, and pass the biological raw material (steam distillation and diffusion of vapor) that is placed in the holder.
Be to improve operation, vacuum state this system of operation down is more satisfactory, particularly, reduces pressure and keep low relatively temperature that to come the evaporative removal solvent be very easily.Tube connector 43 and 44 can be used for being connected vacuum system.
Another kind of preferred equipment is and the use that connects together of a supercritical fluid extraction method, wherein, the connecting pipe system that microwave high-frequency heating electrode utilizes for example glass, quartz or similar material to make connects or is closed in (for example steel pipe) in the outer layer metal outer tube, microwave generator in the microwave equipment is placed in pipe vertically, radiation exposed raw material then from then on to pass through in the pipe.So just, can give play to the quantity-produced advantage.Other installation methods also can use, and as microwave generator the microwave conduit are surrounded, and use suitable material such as metallic shield microwave generating apparatus simultaneously.In this case, polytetrafluoroethylene (PTFE) and glass can be used for making transparent pipeline.
This equipment provides the extraction to the reinforcement of some essential oil that will remove or preferably will remove or other materials, and need not use the heating of heated solvent and so on.
Further advantage, sample purity checkout gear as described equipment disclosed herein can be chromatogram arrangement, particularly gas phase chromatographic device can be connected in any position of described equipment, in different processes, to control product, for example, exit in the follow-up microwave treatment of equipment, after filtration stage, perhaps after purification phase.The position of this analytical equipment is selected to depend on customer requirements.The purity detecting device can connect in addition, and like this, method disclosed herein can continuous operation under a continual situation, and all can collect sample Anywhere at described equipment.
Claims (25)
1, a kind of method that obtains volatile oil from the biological material that contains volatile oil comprises the steps:
A kind of biological material that complete basically body of gland system is arranged is provided, and this biological material has enough moisture to make and can extract described volatile oil with microwave energy;
Surround described biological material with the nonaqueous solvents that is used for obtaining volatile oil;
With the described biological material of microwave energy irradiation, described solvent is transparent or semitransparent to this microwave, between described biological material and described nonaqueous solvents, produce the difference heating, from described biological material, discharge and extract described volatile oil, and cool off the volatile oil that from described biological material, the extracts temperature when being lower than the volatile oil that extracts and from biological material, extracting with described nonaqueous solvents.
2, the method for claim 1 may further comprise the steps:
The biological material that will have the body of gland system of closing described grease is immersed in the non-water organic extractant, and described raw material has complete basically body of gland system and the moisture that when microwave treatment described system is broken;
With the described raw material of microwave energy irradiation, described solvent is transparent or semitransparent to this microwave, the temperature of described biological material is raise be enough to make described body of gland system to be broken, and described volatile oil is discharged and is extracted in the described organic extractant;
Reclaim the described volatile oil in the organic extractant in first extraction step;
In the extractant of the volatile oil that extracts from containing of first extraction step, add extra biological material;
Biological material that mixes with microwave energy irradiation and the extractant that obtains improve the temperature of described biological material, and the body of gland system in the biological material in the described extractant that obtains is broken, and discharge, extract and diffuse out volatile oil; With
From the extractant that further obtains, separate described volatile oil.
3, the method for claim 1, further comprise the described oil extraction in the described biological material to the step of comparing with first organic extractant in the second non-water organic extractant that different extraction character are arranged, and again with the described biological material of microwave energy irradiation and produce second product.
4, the method for claim 1, wherein said biological material is a plant tissue.
5, the method for claim 1, wherein the extractant that evaporates in extraction and separation process is cooled and circulates as the feeding extraction agent.
6, the method for claim 1, wherein said volatile oil comprises essential oil.
7, method as claimed in claim 6, wherein said volatile oil comprises aliphatic acid.
8, the method for claim 1 further comprises the extractant circulation that contains the volatile oil that extracts, and makes the step of the concentration rising of the grease that extracts in the extractant.
9, method as claimed in claim 8, wherein said extraction process is realized with supercritical liq.
10, a kind of composition by described any method of claim 1 to 9 microwave abstracting from biological material.
11, a kind of described composition of claim 10 of pressing is characterized in that described biological material is the garlic plant, and the composition of described microwave abstracting comprises:
A large amount of 2-vinyl-1,3-two thiophenes-4-alkene;
A spot of 3-vinyl-1,2-two thiophenes-5-alkene and diallyl sulfide.
12, a kind ofly it is characterized in that as composition as described in the claim 10 described biological material is a Monarda fistulosa, the composition of described microwave abstracting comprises:
A large amount of geraniols and a spot of octene-3-alcohol, α-terpinenes, linalool, neral and GermacreenD.
But 13, a kind of equipment that extracts extracted component from biological material comprises:
Blending tank with described biological material and extractant mixing;
First mixture of biological material and extractant is carried the pump that passes described microwave high-frequency heating electrode and handle from described blending tank;
From the mixture of handling, isolate the device of the extractant that includes extract liquid;
The extractant circulation of separating is mixed the device that forms second mixture again with biological material to be processed; With
Carry the device of second mixture to microwave high-frequency heating electrode.
14, equipment as claimed in claim 13 comprises a plurality of microwave high-frequency heating electrodes.
15, equipment as claimed in claim 13, wherein said microwave high-frequency heating electrode is an applicator that can comprise the supercritical liq extractant.
16, equipment as claimed in claim 13 is included in described device and connects continuous tubing system between the device of vacuum source.
17, equipment as claimed in claim 13 further comprises:
An extractant storage tank;
Controllably carry the valve of extractant to described blending tank;
The mixture that microwave treatment is crossed circulates, with the further EGR of handling of described at least one applicator; With
The device that from the mixture that microwave treatment is crossed, separates volatile oil.
18, equipment as claimed in claim 17, the device of described separation volatile oil comprises the filter of the mixture that filtration treatment is crossed.
19, equipment as claimed in claim 18 further comprises the separator that described fluid separation applications is become volatile oil and extractant.
20, a kind of extraction equipment comprises:
Adopt (a) to be installed in series, (b) the parallel installation, (c) in conjunction with a plurality of microwave high-frequencies heating electrodes of (a) and a kind of form (b), it is mobile mixture in 1 to 10cm the pipeline that each applicator acts at diameter;
The mixing arrangement of mixed extractant and the raw material that will extract; With
These mixtures are delivered to the device of each pipeline.
But 21, a kind of equipment that extracts extracted component from biological material comprises:
The microwave high-frequency heating electrode that a plurality of orders are installed;
Carry the mixture of biological material and extractant to pass a plurality of microwave high-frequencies heating electrodes and be not more than the device of handling in the container of 5cm or the pipeline at cross-sectional diameter;
The EGR of the biological material that circulates described extractant and handled.
22, equipment as claimed in claim 21, wherein said microwave high-frequency heating electrode is installed in series.
23, equipment as claimed in claim 21, wherein said microwave high-frequency heating electrode is parallel the installation.
24, equipment as claimed in claim 21, wherein said microwave high-frequency heating electrode comprises the applicator of series connection in conjunction with being installed in series and walking abreast installation in parallel every row applicator of installing.
25, equipment as claimed in claim 21, wherein said a plurality of microwave high-frequency heating electrodes are the applicators that comprise the supercritical liq extractant.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP02310139A JP3095241B2 (en) | 1990-11-15 | 1990-11-15 | Microwave extraction of volatile oil and apparatus therefor |
| JP310139/90 | 1990-11-15 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1061729A CN1061729A (en) | 1992-06-10 |
| CN1032041C true CN1032041C (en) | 1996-06-19 |
Family
ID=18001637
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91110686 Expired - Lifetime CN1032041C (en) | 1990-11-15 | 1991-11-14 | Microwave assisted process for extraction and apparatus therefor |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JP3095241B2 (en) |
| CN (1) | CN1032041C (en) |
| BR (1) | BR9104967A (en) |
| CA (1) | CA2055390C (en) |
Families Citing this family (35)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5853726A (en) * | 1992-09-16 | 1998-12-29 | Chevereau; Pierre | Method for extracting and fixing aromas on non-aqueous substrate, machine for implementing the method, and product thereby |
| FR2694300B1 (en) * | 1992-09-16 | 1994-10-14 | Pierre Chevereau | Process for extracting and fixing aromas on a non-aqueous substrate, machine for implementing the process and product obtained according to the process. |
| AT397464B (en) * | 1992-10-07 | 1994-04-25 | Koch Heinrich P Dr | METHOD FOR OBTAINING A THERAPEUTIC PLANT EXTRACT |
| CN1041943C (en) * | 1995-10-16 | 1999-02-03 | 李晓鸣 | Technology for production of Hippophae rhmnoides seed oil |
| CN1101237C (en) * | 1998-07-30 | 2003-02-12 | 吕胜一 | Multifunctional rapid extracting fusion equipment |
| CN1112953C (en) * | 1999-10-29 | 2003-07-02 | 汤大卫 | Process for liquid/sodid extraction |
| KR100388110B1 (en) * | 2000-05-04 | 2003-06-18 | 해태제과식품주식회사 | Process for extracting astaxanthin pigment from yeast and extracted pigment thereof |
| JP2006035078A (en) * | 2004-07-26 | 2006-02-09 | National Institute Of Advanced Industrial & Technology | Method and apparatus for extracting/separating objective substance by using supercritical fluid and irradiating with microwave |
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| RU2382669C1 (en) * | 2008-12-29 | 2010-02-27 | ЗАО "Твин Трейдинг Компани" | Method of extracting materials and device to this end |
| DE102009007402A1 (en) * | 2009-02-04 | 2010-08-05 | VLB Berlin e. V. Institut für Mikrobiologie | Biosynthesis and extraction of substances from cells |
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| CN106221921A (en) * | 2016-08-26 | 2016-12-14 | 广西灏源盛世生物科技有限公司 | A kind of Geranium Essential extracting method |
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| JP2020203958A (en) * | 2017-08-18 | 2020-12-24 | ライオン株式会社 | Labiatae menta plant-derived extract and method for manufacturing the same |
| CN110025968B (en) * | 2018-01-12 | 2021-08-27 | 湖北民族大学 | Rotary evaporator for vacuum automatic extraction continuous feeding |
| CN108753439A (en) * | 2018-05-30 | 2018-11-06 | 无限极（中国）有限公司 | A kind of oil plant squeezes the method for grease and the application of the grease |
| CN110801643B (en) * | 2019-11-19 | 2021-10-19 | 四川丁点儿食品开发股份有限公司 | Device and method for removing bitter taste of pepper extract |
| CN111676097A (en) * | 2020-06-01 | 2020-09-18 | 蓝彤生物科技(吉林)有限公司 | Extraction method of ginseng essential oil |
| CN112760166A (en) * | 2021-01-08 | 2021-05-07 | 四川轻化工大学 | Rattan pepper oil production facility |
| CN115449434B (en) * | 2022-10-13 | 2023-11-17 | 江西安邦药业有限公司 | Method for continuous fractional distillation of eucalyptus oil |
-
1990
- 1990-11-15 JP JP02310139A patent/JP3095241B2/en not_active Expired - Lifetime
-
1991
- 1991-11-13 CA CA002055390A patent/CA2055390C/en not_active Expired - Lifetime
- 1991-11-14 CN CN 91110686 patent/CN1032041C/en not_active Expired - Lifetime
- 1991-11-14 BR BR9104967A patent/BR9104967A/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| CA2055390C (en) | 2006-12-05 |
| CA2055390A1 (en) | 1992-05-16 |
| JP3095241B2 (en) | 2000-10-03 |
| JPH04183796A (en) | 1992-06-30 |
| BR9104967A (en) | 1992-06-23 |
| CN1061729A (en) | 1992-06-10 |
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