CN101484224A - Target substance-extracting method and target substance-extracting device - Google Patents
Target substance-extracting method and target substance-extracting device Download PDFInfo
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- CN101484224A CN101484224A CNA2007800252706A CN200780025270A CN101484224A CN 101484224 A CN101484224 A CN 101484224A CN A2007800252706 A CNA2007800252706 A CN A2007800252706A CN 200780025270 A CN200780025270 A CN 200780025270A CN 101484224 A CN101484224 A CN 101484224A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P43/00—Drugs for specific purposes, not provided for in groups A61P1/00-A61P41/00
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
Abstract
It is intended to provide an extraction method capable of extracting a target substance selectively and effectively from a matter to be treated without resort to a multi-stage extraction process, and an extraction apparatus. The method for extracting a target substance of the invention comprises the steps of: bringing a high-pressure fluid mixture obtained by mixing a hydrophilic fluid component with a hydrophilic fluid component in a supercritical or subcritical state over their solubilities into contact with a solid matter to be treated containing a target substance, and extracting the target substance contained in the matter to be treated into at least either of the hydrophilic fluid component and the hydrophobic fluid component; fractionating the high-pressure fluid mixture into a fraction mainly containing the hydrophilic fluid component and a fraction mainly containing the hydrophobic fluid component; and isolating the target substance from at least one of the fractions.
Description
Technical field
The present invention relates to a kind of extracting method and extraction element that from solid-state object being treated, extracts target substance (targetsubstance).
Background technology
As the method for extracting useful component contained in the natural agricultural product etc. or the method for removing remains of pesticide composition contained in the natural agricultural product etc., the method (for example with reference to patent documentation 1～3) with the natural agricultural product of carbon dioxide treatment of supercriticality or subcritical state (following abbreviate these states as " critical condition " sometimes) etc. is disclosed.
For carbon dioxide,, demonstrate character as critical fluids roughly also having the character (diffusivity) of gas and the character (dissolubility) of liquid concurrently near the room temperature by regulating pressure.In addition, the carbon dioxide of critical condition can easily be removed after temperature and pressure gasifies by regulating.And carbon dioxide is chemical inertness and avirulence.Therefore, carbon dioxide is especially suitable for use as the extraction solvent that extracts useful component or remains of pesticide composition from raw-food material.
The carbon dioxide of critical condition demonstrates higher dissolubility for the lyophobic dust as low lipid of derived essential oil and molecular weight etc., and can not demonstrate sufficient dissolubility for hydroaropic substance on the other hand.What particularly point out is, contained effective component combines with hydroaropic substance such as sugar in these natural agricultural product mostly in the natural agricultural product etc., therefore is difficult to extract with high yield.In addition, for example, can not demonstrate sufficient dissolubility for the big lyophobic dust of molecular weight as carotenoids (lutein, carrotene, curcumin etc.).
As the method that addresses these problems, patent documentation 1～3 discloses following method, by in the carbon dioxide of critical condition, adding the polarity instrumentality (hereinafter referred to as " entrainer (entrainer) ") of lower alcohols such as water or methyl alcohol, ethanol and so on, change the polarity of the carbon dioxide of critical condition.
But, the method of entrainer is added in employing in the carbon dioxide of critical condition, though can improve the solubility of the carbon dioxide of critical condition to the big useful component of effective component, hydroaropic substance or molecular weight, its solubility to lyophobic dust reduces but then.Therefore, in order from natural agricultural product, to obtain the useful component of hydroaropic substance and lyophobic dust, essential other abstraction process.
Patent documentation 1: No. 3010099 communique of Japan Patent
Patent documentation 2: No. 2669304 communique of Japan Patent
Patent documentation 3: TOHKEMY 2001-8659 communique
Summary of the invention
The present invention finishes in order to solve above-mentioned existing issue, the present invention relates to extract from object being treateds such as natural agricultural product the extracting method of target substance.
An aspect of of the present present invention is a kind of extracting method of target substance, it is characterized in that, comprising:
Make the hydrophilic fluid composition mix the formation high-pressure mixing fluid in the mode that surpasses mutual solubility with the hydrophobic fluid composition of supercriticality or subcritical state, this high-pressure mixing fluid is contacted with the solid-state object being treated that contains target substance, target substance contained in this object being treated is extracted into the operation among at least one side of above-mentioned hydrophilic fluid composition or above-mentioned hydrophobic fluid composition;
Fractionation is with above-mentioned hydrophilic fluid composition cut that is principal component and the operation that is the cut of principal component with above-mentioned hydrophobic fluid composition from above-mentioned high-pressure mixing fluid; And
The operation of from least one side's above-mentioned cut, separating above-mentioned target substance.
Description of drawings
Fig. 1 is the key diagram of structure of first embodiment of example target substance extraction element of the present invention.
Fig. 2 is the key diagram of structure of second embodiment of example target substance extraction element of the present invention.
Fig. 3 is the key diagram of structure of the 3rd embodiment of example target substance extraction element of the present invention.
Fig. 4 represents the figure of composition contained in the fresh coffee beans with respect to the relative volatility of caffeol.
The specific embodiment
The target substance extracting method of the embodiment that the present invention relates to, comprise: make the hydrophilic fluid composition mix the formation high-pressure mixing fluid in the mode that surpasses mutual solubility with the hydrophobic fluid composition of supercriticality or subcritical state, this high-pressure mixing fluid is contacted with the solid-state object being treated that contains target substance, target substance contained in the object being treated is extracted into the operation among at least one side of hydrophilic fluid composition or hydrophobic fluid composition; Fractionation is the cut of principal component with the hydrophilic fluid composition and is the operation of the cut of principal component with the hydrophobic fluid composition from high-pressure mixing fluid; And from least one side's cut the operation of isolation of target substances.Below each operation is done concrete elaboration.
Handled object being treated in the extracting method as present embodiment gets final product so long as contain the solid-state object being treated of target substance, and there is no particular limitation, specifically can enumerate following material (contained hydrophily target substance in (a) expression object being treated.(b) contained hydrophobicity target substance in the expression object being treated).
Korean ginseng root: (a) polysaccharide, ginsenoside, (b) pesticide (sterilization profit (procymidone), lindane (below be sometimes referred to as BHC));
Black ginseng: (a) anthocyanin, (b) agricultural chemicals;
Pon hesperidium aurantium skin: (a) Nobiletin, (b) agricultural chemicals (methimazole);
Milk thistle extract (マ リ ア ア ザ ミ): (a) silymarin, (b) agricultural chemicals (malathion, parathion);
Fresh coffee beans (コ-ヒ-life beans): (a) Polyphenols, (b) caffeine;
Propolis (propolis): (a) amino acid, mineral substance, organic acid, (b) terpenoid, flavonoids;
Vegetable seeds: (a) phosphatide, (b) neutral lipid;
Chinese herbaceous peony: (a) Paeoniflorin (analgesic effect), (b) liposoluble constituent (anti-inflammatory effect)
The object being treated of handling in this extracting method, preferred powder are broken to the size of regulation.By such pulverizing, can make the hydrophilic fluid composition in non-handled thing and the high-pressure mixing fluid and the hydrophobic fluid composition of critical condition keep bigger contact area.The particle diameter of object being treated is preferably more than the 20 μ m, more preferably more than the 40 μ m, more preferably more than the 50 μ m.When the particle diameter of object being treated during less than 20 μ m, the processability of object being treated worsens sometimes.In addition, the particle diameter of object being treated is preferably below the 500 μ m, more preferably below the 300 μ m, more preferably below the 250 μ m.When the particle diameter of object being treated during greater than 500 μ m, have following situation: object being treated can not contact fully with the hydrophobic fluid composition of hydrophilic fluid composition and critical condition, thereby can not extract target substance from object being treated fully.
High-pressure mixing fluid in this extracting method,, object being treated extracts target substance contained in the object being treated for being contacted with this high-pressure mixing fluid, as long as its hydrophobic fluid composition by hydrophilic fluid composition and critical condition constitutes, then can form by any way.For example, the hydrophobic fluid that can mix hydrophilic liquid composition and the critical condition high-pressure mixing fluid that becomes to assign to form; Perhaps, the hydrophobic fluid composition that can mix hydrophily gas componant and non-critical state obtains fluid-mixing, to gained fluid-mixing high-pressure, make its fluid-mixing that becomes the hydrophobic fluid composition of hydrophilic liquid composition and critical condition, thereby form high-pressure mixing fluid.In addition, the hydrophobic fluid composition that can also mix hydrophily gas componant and critical condition obtains fluid-mixing, to gained fluid-mixing high-pressure, make its fluid-mixing that becomes the hydrophobic fluid composition of hydrophilic liquid composition and critical condition, thereby form high-pressure mixing fluid.Perhaps, the hydrophobic fluid composition that also can mix hydrophilic liquid composition and non-critical state obtains fluid-mixing, to gained fluid-mixing high-pressure, make its fluid-mixing that becomes the hydrophobic fluid composition of hydrophilic liquid composition and critical condition, thereby form high-pressure mixing fluid.Need to prove that " fluid " used in this specification is meant, the general name of the fluid of gas and liquid or supercriticality or subcritical state.
In this extracting method, the method that object being treated is contacted with high-pressure mixing fluid, as long as object being treated fully contacts with the hydrophilic fluid composition that constitutes high-pressure mixing fluid and the hydrophobic fluid composition of critical condition, there is no particular limitation.
As the concrete example of the method that object being treated is contacted with high-pressure mixing fluid, for example can enumerate: in preformed high-pressure mixing fluid, drop into object being treated, the method for dipping object being treated in high-pressure mixing fluid; Respectively the hydrophobic fluid composition of hydrophilic fluid composition and critical condition is supplied to simultaneously the method for object being treated; Perhaps, in a side fluid composition, flood object being treated, again to the method for the fluid composition that wherein mixes the opposing party.Especially preferably enumerate following method: object being treated is immersed in the hydrophilic liquid, obtains maceration extract, in this maceration extract, mix the method for the hydrophobic fluid of critical condition then; Perhaps, object being treated is immersed in the hydrophobic fluid of critical condition, obtains maceration extract, in this maceration extract, mix the method for hydrophilic liquid then.
In addition, when the method that object being treated is contacted with high-pressure mixing fluid adopts following method, i.e. employing is supplied to object being treated separately simultaneously with two sides' fluid composition respectively, perhaps in a side fluid composition, flood object being treated, when the method for the fluid composition that wherein mixes the opposing party, preferred both sides' fluid composition is supplied with in the mode of convection current again.This supply for example can be undertaken by following manner: supply a side fluid composition from a side of object being treated, from opposite side supply the opposing party's of object being treated fluid composition.By the way, both sides' fluid composition can mix fully in the high-pressure mixing fluid.
In addition, when the method that object being treated is contacted with high-pressure mixing fluid adopts following method, i.e. employing is supplied to object being treated separately simultaneously with two sides' fluid composition respectively, perhaps in a side fluid composition, flood object being treated, when the method for the fluid composition that wherein mixes the opposing party, preferred at least one side's fluid composition is supplied with the vesicle shape again.This supply for example can be undertaken by following manner, makes fluid composition pass through the porous scutum, perhaps accommodating fluid composition off and on.Adopt aforesaid way, can increase the contact area of both sides' fluid composition.
High-pressure mixing fluid in this extracting method can constitute in the following manner: the hydrophilic fluid composition mixes with the solubility of the hydrophobic fluid composition that surpasses critical condition, perhaps, the hydrophobic fluid composition of critical condition mixes with the solubility that surpasses the hydrophilic fluid composition.Shown in above-mentioned, mix each composition above mutual solubility, can make in the high-pressure mixing fluid state have following two-phase clearly to separate mutually: contain the hydrophobic fluid composition of dissolving, be the phase of principal component with the hydrophilic fluid composition, and contain the hydrophilic fluid composition of dissolving, be the phase of principal component with the hydrophobic fluid composition.So form by being the cut of principal component with the hydrophilic fluid composition and being two kinds of cuts that the cut of principal component constitutes with the hydrophobic fluid composition.Need to prove, with the hydrophilic fluid composition be principal component cut, be the cut of principal component with the hydrophobic fluid composition, each self-forming layer because both density is different as a rule.In addition, will be that the layer of the cut of principal component is called the hydrophilic fluid layer, will will be that the layer of the cut of principal component is called the hydrophobic fluid layer with the hydrophobic fluid composition with the hydrophilic fluid composition sometimes below.
Be the cut of principal component with the hydrophilic fluid composition in the high-pressure mixing fluid and be the ratio of the cut of principal component that as long as can extract target substance from each cut, there is no particular limitation with the hydrophobic fluid composition.Need to prove that its ratio not only changes according to the mixing ratio of hydrophilic fluid composition and hydrophobic fluid composition, and change according to the characteristic of hydrophilic fluid composition and hydrophobic fluid composition or pressure or the temperature of keeping high-pressure mixing fluid.
For example, the hydrophilic fluid composition is that continuous phase, hydrophobic fluid composition are under the situation of decentralized photo, preferably constitutes: the ratio that with the hydrophilic fluid composition is the cut of principal component is 60～99wt%, be that the ratio of the cut of principal component is 1～40wt% with the hydrophobic fluid composition; Preferred constituting: the ratio that with the hydrophilic fluid composition is the cut of principal component is 70～95wt%, be that the ratio of the cut of principal component is 5～30wt% with the hydrophobic fluid composition.When the not enough 60wt% of the ratio of cut that with the hydrophilic fluid composition is principal component, then the hydrophily target substance in the target substance contained in the object being treated can not be extracted in the hydrophilic fluid composition fully.In addition, when the ratio that with the hydrophilic fluid composition is the cut of principal component is higher than 99wt%, the ratio that with the hydrophobic fluid composition is the cut of principal component must reduce, and therefore the hydrophobicity target substance in the target substance contained in the object being treated can not be extracted in the hydrophobic fluid composition fully sometimes.In addition, continuous phase is the basic phase (matrix phase) with the expansion of the arbitrary state consistency ground in liquid phase, gas phase, supercriticality and the subcritical state; Decentralized photo be base that continuous phase constitutes mutually in, with the regional phase (domain phase) of the phase state fine dispersion different with continuous phase.
In addition, adopt the hydrophobic fluid composition as continuous phase, when adopting the hydrophilic fluid composition as decentralized photo, preferably constitute: the ratio that with the hydrophobic fluid composition is the cut of principal component is 60～99wt%, be that the ratio of the cut of principal component is 1～40wt% with the hydrophilic fluid composition; Preferred constituting: the ratio that with the hydrophobic fluid composition is the cut of principal component is 70～95wt%, be that the ratio of the cut of principal component is 5～30wt% with the hydrophilic fluid composition.When the not enough 60wt% of the ratio of cut that with the hydrophobic fluid composition is principal component, then the hydrophobicity target substance in the target substance contained in the object being treated can not be extracted in the hydrophobic fluid composition fully.In addition, when the ratio that with the hydrophobic fluid composition is the cut of principal component is higher than 99wt%, the ratio that with the hydrophilic fluid composition is the cut of principal component must reduce, and therefore the hydrophily target substance in the target substance contained in the object being treated can not be extracted in the hydrophilic fluid composition fully sometimes.
High-pressure mixing fluid in this extracting method preferably maintains more than the 1MPa, more preferably maintains more than the 5MPa.When being lower than 1MPa, in high-pressure mixing fluid, can not keep the critical condition of hydrophobic fluid composition sometimes.In addition, preferably maintain below the 100MPa, more preferably maintain below the 90MPa.Even be higher than 100MPa, can not improve the dissolubility of target substance with respect to hydrophilic fluid composition and/or hydrophobic fluid composition yet.
High-pressure mixing fluid in the extracting method of present embodiment preferably maintains more than 5 ℃, more preferably maintains more than 20 ℃.When being lower than 5 ℃, the speed of extracting target substance sometimes from object being treated reduces.In addition, preferably maintain below 100 ℃, more preferably maintain below 90 ℃.When being higher than 100 ℃, contained target substance causes thermal denaturation in the object being treated sometimes.
In this extracting method, when only containing the hydrophily target substance in the object being treated, contact with high-pressure mixing fluid by making object being treated, this hydrophily target substance mainly is extracted in the hydrophilic fluid composition.In addition, when only containing the hydrophobicity target substance in the object being treated, this hydrophobicity target substance mainly is extracted in the hydrophobic fluid composition of critical condition.In addition, when containing hydrophily target substance and hydrophobicity target substance in the object being treated, in the hydrophobic fluid composition that the hydrophily target substance mainly is extracted in the hydrophilic fluid composition, the hydrophobicity target substance mainly is extracted critical condition.
In this extracting method, fractionation is the cut of principal component with the hydrophilic fluid composition and is the method for the cut of principal component with the hydrophobic fluid composition that there is no particular limitation from high-pressure mixing fluid.For example can be formed in the high-pressure mixing fluid by at first taking out, the cut of the top, interface of hydrophilic fluid layer and hydrophobic fluid layer, thereby the cut of the below that obtains being left.In addition, can be by at first taking out the cut of interface below, thus the cut of the top that obtains being left.
The method of isolation of target substances from the cut of fractionation, there is no particular limitation, but preferably make the target substance of dissolving thermal denaturation not take place and the method for separating.Particularly, for example can enumerate, the decompression of the fluid composition of fractionation, heating are made its gasification, separate the fluid composition of gasification and the method for target substance again.Need to prove, fractionation is the cut of principal component with the hydrophilic composition and is this fractional method in the operation of cut of principal component with the hydrophobic fluid composition from high-pressure mixing fluid, this separation method with in the operation of isolation of target substances from the cut of fractionation can adopt identical chemical method, physical method.
In addition, handled object being treated in this extracting method is preferably handled with the state that is accommodated in the logical fluidity container.Object being treated is pulverized under the situation about using the back,, can be improved the processability of object being treated by object being treated being accommodated in the logical fluidity container.
Used hydrophilic fluid composition and hydrophobic fluid composition in this extracting method considered from carrying out fractionation operation aspect simply, preferably selects the big combination of its mutual density variation.In addition, the hydrophobic fluid composition preferably becomes the composition of critical condition under comparatively gentle condition.And, need also to consider that this extracting method handles raw-food material sometimes.
Therefore, in this extracting method, as the hydrophilic fluid composition, the preferred use is selected from least a in water, methyl alcohol, the ethanol isopolarity solvent; As the hydrophobic fluid composition, the preferred use is selected from least a in the nonpolar or low pole fluid such as carbon dioxide, nitrous oxide, propane.Especially preferably make water as the hydrophilic fluid composition, especially preferably use carbon dioxide as the hydrophobic fluid composition.Its reason is, water is harmless for raw-food material, and carbon dioxide is nontoxic and do not have combustibility and can more easily obtain critical condition (about 31 ℃, about 7.3MPa), and comparatively cheap as raw material.
In addition, in this extracting method, make water, when using carbon dioxide, mix the high-pressure mixing fluid that above-mentioned fluid composition forms and preferably maintain more than the 3MPa, more preferably maintain more than the 4MPa as the hydrophobic fluid composition as the hydrophilic fluid composition.When high-pressure mixing fluid keeps with not enough 3MPa, exist object being treated in high-pressure mixing fluid, to freeze, can not carry out the situation that desired extraction is handled.In addition, high-pressure mixing fluid preferably maintains below the 100MPa, more preferably maintains below the 90MPa.
In addition, in this extracting method, as hydrophilic fluid composition use ethanol, when using carbon dioxide as the hydrophobic fluid composition, the high-pressure mixing fluid that mixes above-mentioned fluid composition formation preferably maintains more than the 3MPa, more preferably maintains more than the 4MPa.When high-pressure mixing fluid keeps with not enough 3MPa, exist object being treated in high-pressure mixing fluid, to freeze, can not carry out the situation that desired extraction is handled.In addition, high-pressure mixing fluid preferably maintains below the 20MPa, more preferably maintains below the 15MPa.When high-pressure mixing fluid keeps with the state that surpasses 20MPa, exist the solubility of each fluid composition to rise, can not form the situation of hydrophilic fluid layer and hydrophobic fluid layer.
More than, describe the embodiment of the target substance extracting method of present embodiment in detail, but the present invention is not subjected to the restriction of above-mentioned embodiment, can implement with other mode yet.
The extracting method of present embodiment, can be at official hour, in the fractionation operation, do not carry out with the hydrophobic fluid composition is the fractionation of the cut (following abbreviate as sometimes " cut of hydrophobic fluid composition ") of principal component, only fractionation is the cut (following abbreviate as sometimes " cut of hydrophilic fluid composition ") of principal component with the hydrophilic fluid composition, in high-pressure mixing fluid, supply new hydrophilic fluid composition simultaneously, can upgrade the hydrophilic fluid composition in the high-pressure mixing fluid thus on one side, carry out on one side the extraction of target substance in the hydrophilic fluid composition and the fractionation of the cut of hydrophilic fluid composition, the cut of the last composition of fractionation hydrophobic fluid again.Perhaps, can not carry out the fractionation of the cut of hydrophilic fluid composition, the hydrophobic fluid composition of only fractionation critical condition, in high-pressure mixing fluid, supply the hydrophobic fluid composition of new critical condition simultaneously, can upgrade the hydrophobic fluid composition in the high-pressure mixing fluid thus on one side, carry out on one side the extraction of target substance in the hydrophobic fluid composition and the fractionation of the cut of hydrophobic fluid composition, the cut of the last composition of fractionation hydrophilic fluid again.In addition, can also be in the fractionation operation, the cut of the cut of fractionation hydrophilic fluid composition and the hydrophobic fluid composition of critical condition, the hydrophobic fluid composition of hydrophilic fluid composition that while supply in high-pressure mixing fluid is new and new critical condition, upgrade on one side hydrophilic fluid composition and hydrophobic fluid composition in the high-pressure mixing fluid thus, Yi Bian carry out the extraction of target substance in the hydrophilic fluid composition and the fractionation of the cut of hydrophilic fluid composition, and carry out the extraction of target substance in the hydrophobic fluid composition and the fractionation of the cut of hydrophobic fluid composition.Thus, can prevent that the hydrophilic fluid composition and the target substance concentration in the hydrophobic fluid composition that constitute high-pressure mixing fluid from rising, can prevent that therefore the ability of extracting target substance contained in the object being treated in fluid composition from reducing.
Perhaps, the extracting method of present embodiment can be carried out in the following manner, does not forward the either party at least of the cut of the fluid composition of institute's fractionation to separation circuit, and it directly is conducted in the high-pressure mixing fluid again.For example, do not forward at least a portion of the cut of the hydrophilic fluid composition of institute's fractionation to separation circuit, and directly be conducted in the high-pressure mixing fluid again it, though the extractability of hydrophilic fluid composition reduces sometimes thus, can improve the target substance concentration of the cut of hydrophilic fluid composition.In addition, can reduce the consumption of hydrophilic fluid composition in the extracting method of present embodiment.And, can in the hydrophilic fluid composition, dissolve, the hydrophobic fluid of the critical condition that inhibition disappears from high-pressure mixing fluid in the cut of fractionation hydrophilic fluid composition becomes component.
The extracting method of present embodiment is so long as the method for in the high-pressure mixing fluid that hydrophilic fluid composition and hydrophobic fluid composition mix object being treated being handled gets final product.Therefore, according to extracting purpose, can also add the modifier of this fluid-mixing of modification in this high-pressure mixing fluid.
Then, describe for the target substance extraction element that can carry out the target substance extracting method of present embodiment suitably.
Fig. 1 is the key diagram of structure of first embodiment of example target substance extraction element of the present invention.In addition, Fig. 2 is the key diagram of structure of second embodiment of example target substance extraction element of the present invention.In addition, Fig. 3 is the key diagram of structure of the 3rd embodiment of example target substance extraction element of the present invention.
According to Fig. 1, the structure of the target substance extraction element 10a of first embodiment comprises: accommodate object being treated, extract the extraction tank 12 of target substance from object being treated; Store the hydrophilic fluid composition storagetank 14 of hydrophilic fluid composition; Store the hydrophobic fluid composition storagetank 16 of hydrophobic fluid composition; One end and the hydrophilic fluid composition supply passageway 18 that hydrophilic fluid composition storagetank 14 is connected, the other end is connected with extraction tank 12; One end and the hydrophobic fluid composition supply passageway 20 that hydrophobic fluid composition storagetank 16 is connected, the other end is connected with extraction tank 12; One end is connected with extraction tank 12, and fractionation is the hydrophilic fluid fractionation path 22 of the cut of principal component with the hydrophilic fluid composition; One end is connected with extraction tank 12, and fractionation is the hydrophobic fluid fractionation path 24 of the cut of principal component with the hydrophobic fluid composition; Is first separator 26 of isolation of target substances the cut of principal component from institute's fractionation with the hydrophilic fluid composition; Is second separator 28 of isolation of target substances the cut of principal component from institute's fractionation with the hydrophobic fluid composition.
Below, with reference to the process of Fig. 1 explanation extraction target substance from object being treated.Need to prove that the used hydrophilic fluid composition and the combination of hydrophobic fluid composition select to form at least the combination of the density of an interface and hydrophilic fluid composition greater than the density of hydrophobic fluid composition here in extraction tank 12.Therefore, the upper portion in extraction tank 12 forms the hydrophobic fluid layer, forms the hydrophilic fluid layer at following quadrate part.
At first, the object being treated that is accommodated in the logical fluidity container (not shown) is accommodated in the extraction tank 12.Then, in extraction tank 12, supply with the hydrophilic fluid composition, and in extraction tank 12, supply with the hydrophobic fluid composition from hydrophobic fluid composition supply passageway 20 from hydrophilic fluid composition supply passageway 18.Herein, the hydrophobic fluid composition from hydrophobic fluid composition supply passageway 20 is supplied with becomes critical condition at least in extraction tank 12.In addition, the hydrophilic fluid composition from hydrophilic fluid composition supply passageway 18 is supplied with becomes hydrophilic liquid at least in extraction tank 12.
There is no particular limitation hydrophobic fluid to be become be divided into the method for critical condition.As its concrete example, for example can enumerate following method: the hydrophobic fluid composition of in extraction tank 12, supplying with non-critical state, and to pressurizeing in the extraction tank 12, regulate temperature in the extraction tank 12 by the temperature-adjusting device 30 that is equipped with in the extraction tank 12 then, thereby become the method for critical condition; Perhaps, utilize in the hydrophobic fluid composition supply passageway 20 booster 32 and the heater 34 that are provided with, the hydrophobic fluid composition of the non-critical state that will supply with from hydrophobic fluid composition supply passageway 16 is conducted to method in the extraction tank 12 etc. with pre-critical condition.In addition, as preferred method, can enumerate following method: utilize in the extraction tank 12 temperature-adjusting device 30 that is equipped with to regulate temperature in the extraction tank 12 in advance, hydrophobic fluid composition with non-critical state is fed in the extraction tank 12 simultaneously, and, then the hydrophobic fluid composition is conducted to method in the extraction tank 12 with critical condition to pressurizeing in the extraction tank 12.
From the hydrophilic fluid composition that hydrophilic fluid composition supply passageway 18 is supplied with, as long as be hydrophilic liquid in extraction tank 12, there is no particular limitation to its form, can be liquid condition or gaseous state.In addition, supply with the hydrophilic fluid composition, preferably in hydrophilic fluid composition supply passageway 18, be equipped with booster 36 in order inwardly to press in the extraction tank 12 that increases.In addition, in order to keep the critical condition of the hydrophobic fluid composition of accommodating in the extraction tank 12, preferred version is, with the adjustment in the extraction tank 12 to the situation of specified temp, the heater (not shown) is set in hydrophilic fluid composition supply passageway 18 does not change the temperature in the extraction tank 12, after the hydrophilic fluid composition is heated to specific temperature, be fed in the extraction tank 12.
Among the target substance extraction element 10a, in extraction tank 12, supply with the method for the hydrophobic fluid composition of hydrophilic fluid composition and critical condition, as long as target substance contained in the object being treated can be extracted among at least one side in the cut of the cut of the hydrophilic fluid composition in the high-pressure mixing fluid and hydrophobic fluid composition, there is no particular limitation.For example, can be respectively the hydrophobic fluid composition of hydrophilic fluid composition and critical condition be fed in the extraction tank 12 simultaneously; Also can be in advance a side fluid composition be fed in the extraction tank 12, obtain the maceration extract of object being treated after, again to the fluid composition of wherein supplying with the opposing party.
Two kinds of fluid compositions supplying with in extraction tank 12 preferably mix fully and contact.By two kinds of fluid compositions being mixed fully and contacting, can accelerate the processing in the abstraction process as mentioned above.
For two kinds of fluid compositions being mixed fully and contacting, preferred hydrophilic fluid composition supply passageway 18 is connected with the upper portion of extraction tank 12, hydrophobic fluid composition supply passageway 20 is connected with the following quadrate part of extraction tank 12.Two kinds of fluid compositions are contacted in the mode of convection current.
In extraction tank 12, the contact area of preferred two kinds of fluid compositions is bigger.In order to increase the contact area of two kinds of fluid compositions, for example can porous scutum 38 be set in extraction tank 12, making at least, either party's fluid composition passes through porous scutum 38.Fluid composition can be separated into little blister thus.
The cut of the cut of fractionation hydrophilic fluid composition and hydrophobic fluid composition from extraction tank 12, can be following structure: hydrophilic fluid fractionation path 22 is connected with the following quadrate part of extraction tank 12, and hydrophobic fluid fractionation path 24 is connected with the upper portion of extraction tank 12.Thus, for example: the cut that at first takes out the hydrophilic fluid composition from the hydrophilic fluid fractionation path 22 that is connected with the following quadrate part of extraction tank 12, obtain the cut of the hydrophobic fluid composition of critical condition residual in the extraction tank 12 then, thereby can fractionate out each cut.Perhaps, the hydrophobic fluid fractionation path 24 that is connected from the upper portion with extraction tank 12 is discharged the cut of the hydrophobic fluid composition of critical conditions, take out the cut of hydrophilic fluid composition by hydrophilic fluid fractionation path 22 from the following quadrate part of extraction tank 12 then, thereby can fractionate out each cut.
The method of isolation of target substances is not special from the cut of institute's fractionation limits, but preferred version is, after the hydrophobic fluid composition gasification with critical condition, when hydrophobic fluid composition that separates this gasification and target substance, between the hydrophobic fluid fractionation path 24 and second separator 28, pressure-regulating valve 40 and heater 42 are set.
As first separator 26, for example can enumerate evaporimeter.In addition, in first separator 26, during the hydrophobic fluid composition of the critical condition of in the cut that separates the hydrophilic fluid composition in the lump, dissolving, preferably between the hydrophilic fluid fractionation path 22 and first separator 26, pressure-regulating valve and heater (not shown) are set.
More than, with reference to Fig. 1 the leaching process of present embodiment has been described, but target substance extraction element of the present invention is not subjected to the qualification of above-mentioned embodiment.
Target substance extraction element 10a can also be equipped with condenser 44, is used for that the hydrophobic fluid composition that first separator 26 separates with second separator 28 is recycled to hydrophobic fluid composition storagetank 16 and recycles.
Target substance extraction element 10a, while upgrade hydrophilic fluid composition and/or hydrophobic fluid composition in the extraction tank 12, carry out target substance contained in the object being treated in each fluid layer extraction and during the fractionation of each fluid layer, in order to control from the quantity delivered of each fluid composition of supply passageway 18,20 or from the fractionation amount of fractionation path 22,24, for example preferably be provided with the liquid level meter 46 of measuring the liquid level of hydrophilic fluid layer in extraction tank 12 (for example differential pressure transmitter etc.).
In addition, another embodiment as the target substance extraction element, target substance extraction element 10b as shown in Figure 2, can be equipped with high-pressure circulation pump 48, at least a portion of the cut of the hydrophilic fluid composition that described high-pressure circulation pump 48 will take out from the following quadrate part of extraction tank 12 does not forward first separator 26 to, and it directly is conducted to the upper portion of extraction tank 12 once more.Need to prove that the mode among Fig. 2 except that above-mentioned can be identical with Fig. 1, its explanation of Therefore, omited.
In addition, as the another embodiment of target substance extraction element, target substance extraction element 10c as shown in Figure 3, its structure can comprise: the high-pressure mixing fluid drain passageway 50 that is connected with the upper portion of extraction tank 12; The temporary transient mixed high-voltage fluid of discharging from high pressure mixing drain passageway 50 of storing is separated into the high-pressure separator 52 of cut (that is, hydrophilic fluid layer and hydrophobic fluid layer) of the hydrophobic fluid composition of the cut of hydrophilic fluid composition and critical condition; Be connected the hydrophobic fluid fractionation path 24 of the cut of fractionation hydrophobic fluid composition with the upper portion of high-pressure separator 52.Thus, even discharge high-pressure mixing fluid from extraction tank 12, the cut that still can prevent the hydrophilic fluid composition flows into hydrophobic fluid fractionation path 24, therefore do not need the hydrophilic fluid layer in the extraction tank 12 and the interface of hydrophobic fluid layer are remained on certain altitude, thereby can increase the amount of accommodating of object being treated in extraction tank 12.
In addition, when hydrophilic target substance is extracted in the cut of the hydrophilic fluid composition that separates with high-pressure separator 52, the preferred outfit: the cut of hydrophilic fluid composition is fed to the hydrophilic fluid fractionation path (not shown) of first separator 26 after high-pressure separator 52 fractionation, separates the hydrophily target substance in the cut of the hydrophilic fluid composition from high-pressure separator 52.
Need to prove that the mode among Fig. 3 except that above-mentioned can be identical with Fig. 1 or Fig. 2, its explanation of Therefore, omited.
Fig. 1～target substance extraction element 10a～10c shown in Figure 3, combination according to hydrophilic fluid composition and hydrophobic fluid composition, can increase suitable design alteration and use, so that the fluid composition that the big side's of density fluid composition is supplied with (then from quadrate part discharge) down, a side that density is little from the upper portion of extraction tank is supplied with (discharging from upper portion then) from the following quadrate part of extraction tank.
In addition, the present invention is in the scope that does not break away from above-mentioned purport, and the mode that can increase various improvement, modification, distortion according to the knowledge based on those skilled in the art is implemented.
Embodiment
Below, more specifically describe the present invention by embodiment, but the present invention is not subjected to the qualification of these embodiment.
Embodiment 1
(contained useful component is with respect to the relative volatility of caffeol in the fresh coffee beans)
To accommodate as the fresh coffee beans 100g of object being treated in the extraction tank of capacity 300ml, as the hydrophilic fluid composition, behind the airtight extraction tank, will be heated to 60 ℃ in the extraction tank to the water that wherein adds specified quantitative (5g, 10g, 30g, 50g, 70g, 90g).Then, in extraction tank, charge into carbon dioxide, regulate that to make in the extraction tank be 60 ℃, 30MPa.
Then, in with extraction tank, keep under 60 ℃, the state of 30MPa, supply with supercritical carbon dioxide (the about 10g/ of flow minute) from the following quadrate part of extraction tank, discharge the cut of supercritical carbon dioxide layer simultaneously from the upper portion of extraction tank, in extraction tank, make supercritical carbon dioxide stream 3 hours thus.
Cut to the supercritical carbon dioxide layer of discharging from extraction tank reduces pressure, and makes the supercritical carbon dioxide gasification and removes, and obtains liquid extract.
Adopt high performance liquid chromatography (using the system ODS of (strain) Shimadzu Seisakusho Ltd. post) to analyze the liquid extract of gained, caffeine contained in the extract and Polyphenols are carried out quantitatively, remaining liquid extract is caffeol.Calculate caffeine amount and Polyphenols amount, try to achieve relative volatility with respect to caffeol with respect to the coffee oil mass.Its result as shown in Figure 4.
By the result of Fig. 4 as can be known, by increasing the addition of water, thereby optionally improve the relative volatility of caffeine with respect to caffeol with respect to fresh coffee beans.In addition we know, Polyphenols is with respect to the volatility of caffeol, even the addition increase of water is also almost constant.From this result as can be known, for the situation that the coexistence of hydrophobic fluid composition and hydrophilic fluid composition is extracted, and only with (promptly as the supercritical carbon dioxide of hydrophobic fluid composition, with respect to fresh coffee beans, the addition of water is the situation of 0wt%) situation about extracting, extracting operation has bigger difference, when the hydrophilic fluid composition when specified quantitative is above, improve the extraction efficiency of target component especially.
Embodiment 2
To put in the basketry as the fresh coffee beans 100g of object being treated, under this state it is contained in the extraction tank of volume 300ml, the water 200g to wherein supplying with as the hydrophilic fluid composition is immersed in fresh coffee beans in the water, behind the airtight extraction tank, will be heated to 60 ℃ in the extraction tank.Then, in extraction tank, supply with carbon dioxide and pressurization, regulate that to make in the extraction tank be 60 ℃, 30MPa.
Then, in with extraction tank, keep under 60 ℃, the state of 30MPa, supply with water (flow 2.5g/ minute) from the upper portion of extraction tank, following quadrate part from extraction tank, supply with supercritical carbon dioxide (flow 10g/ minute) while using the porous scutum that is provided with in the extraction tank to be separated into the vesicle shape, simultaneously from the cut of the following quadrate part discharge water layer of extraction tank, discharge the cut of supercritical carbon dioxide layer from the upper portion of extraction tank, water and supercritical carbon dioxide were circulated 3 hours, each cut of fractionation simultaneously in extraction tank.
Need to prove that in this case, water layer is made of the water of about 94.5wt% and the supercritical carbon dioxide of about 5.5wt%.In addition, the supercritical carbon dioxide layer is made of the water of about 0.3wt% and the supercritical carbon dioxide of about 99.7wt%.
Cut to the gained water layer reduces pressure, heats, and heats up in a steamer and anhydrates, and obtains liquid extract.Adopt high performance liquid chromatography (using the system ODS of (strain) Shimadzu Seisakusho Ltd. post) to analyze the extract of gained, caffeine contained in the extract and Polyphenols are carried out quantitatively, remaining liquid extract is caffeol.Its result is as shown in table 1.
[table 1]
As shown in Table 1, from the cut of water layer, optionally remove caffeine, can extract caffeol and Polyphenols with high concentration (high yield) simultaneously.
In addition, the result of embodiment 1 and the result of embodiment 2 are compared, can draw following result.Promptly, among the embodiment 1, by with the carbon dioxide being the Polyphenols that the hydrophobic fluid layer of principal component can extract denier, and extract the caffeine of several times to the 50 times amount of Polyphenols, on the other hand, among the embodiment 2, by can extracting the caffeine of denier, and extract the Polyphenols more than 3800 times of caffeine based on the hydrophilic fluid layer of water.By this result as can be known, according to the method described above, can distinguish optionally and extract: utilize the material of hydrophobic fluid extraction and the material that utilizes hydrophilic fluid to extract with high concentration.
Embodiment 3
Accommodate ginseng 100g that particle diameter is distributed as 50～250 μ m sizes and replace fresh coffee beans among the embodiment 2 in extraction tank, in addition operation is similarly to Example 2 handled ginseng with the high-pressure mixing fluid of water and supercritical carbon dioxide.
Afterwards, the cut of the cut of fractionation water layer and supercritical carbon dioxide layer, decompression, heating remove and to anhydrate or carbon dioxide, obtain being extracted the liquid extract in the water layer cut and are extracted liquid extract in the supercritical carbon dioxide layer cut.Adopt high performance liquid chromatography (using the system ODS of (strain) Shimadzu Seisakusho Ltd. post) to analyze extract, ginsenoside is carried out quantitatively from the water layer cut.Need to prove that remaining liquid extract is a polysaccharide.In addition, analyze the extract from supercritical carbon dioxide layer cut with gas chromatography (GL Sciences (ジ-エ Le サ イ エ Application ス) (strain) system DB1701 post), (sterilization profit, BHC) carries out quantitatively to agricultural chemicals.Its result is as shown in table 2.
[table 2]
As shown in Table 2, can from the cut of water layer, optionally remove agricultural chemicals, simultaneously can be with the ginsenoside and the polysaccharide of high concentration (high yield) extraction as saponins.
The present invention for the above-described is summarized as follows.
One aspect of the present invention is a kind of target substance extracting method, it is characterized in that, comprise following operation: make the hydrophilic fluid composition mix the formation high-pressure mixing fluid in the mode that surpasses mutual solubility with the hydrophobic fluid composition of supercriticality or subcritical state, this high-pressure mixing fluid is contacted with the solid-state object being treated that contains target substance, target substance contained in this object being treated is extracted into the operation among at least one side of above-mentioned hydrophilic fluid composition or above-mentioned hydrophobic fluid composition; Fractionation is with above-mentioned hydrophilic fluid composition cut that is principal component and the operation that is the cut of principal component with above-mentioned hydrophobic fluid composition from above-mentioned high-pressure mixing fluid; The operation of from least one side's above-mentioned cut, separating above-mentioned target substance.According to this method, when extracting target substance from object being treateds such as natural agricultural product, the extraction operation by single can separate hydrophily target substance contained in the object being treated and hydrophobicity target substance respectively, can extract with high extracting efficiency simultaneously.In addition, owing to can in an extraction tank, utilize high-pressure mixing fluid to extract operation, thereby device is oversimplified.And then the needed time of abstraction process also shortens.As mentioned above,, do not need other abstraction process, promptly can from object being treated, distinguish and high-purity ground extraction hydrophily target substance and hydrophobicity target substance according to extracting method of the present invention.
In addition, in the above-mentioned target substance extracting method, from the cut that is principal component with above-mentioned hydrophilic fluid composition, extract the hydrophily target substance, from the cut that is principal component with above-mentioned hydrophobic fluid composition, extract the hydrophobicity target substance simultaneously, by single extraction operation, can distinguish hydrophily target substance contained in the separation and Extraction object being treated and hydrophobicity target substance like this.
In addition, consider from the aspect that operation becomes more easy, above-mentioned object being treated is immersed in the fluid composition of the either party in above-mentioned hydrophilic fluid composition and the above-mentioned hydrophobic fluid composition, obtain maceration extract, in this maceration extract, mix the opposing party's fluid composition, above-mentioned object being treated is contacted with above-mentioned high-pressure mixing fluid.
In addition, consider from the aspect that the contact area that can make both sides' fluid composition becomes bigger, preferably supply the opposing party's fluid composition in the fluid composition of the either party in above-mentioned hydrophilic fluid composition and above-mentioned hydrophobic fluid composition with the vesicle shape, thereby form above-mentioned high-pressure mixing fluid.
In addition, consider, preferably supply with above-mentioned hydrophilic fluid composition and above-mentioned hydrophobic fluid composition and form above-mentioned high-pressure mixing fluid in the mode of convection current from the aspect that each fluid composition is mixed fully and contact.
In addition, from the density contrast of hydrophilic fluid composition and hydrophobic fluid composition than the easy fractionation of die, and the hydrophobic fluid composition can relatively mild condition be issued to critical condition aspect consider, preferably:, use to be selected from least a in water, methyl alcohol, the ethanol as above-mentioned hydrophilic fluid composition; As above-mentioned hydrophobic fluid composition, use to be selected from least a in carbon dioxide, nitrous oxide, the propane.
In addition, the present invention relates to a kind of target substance extraction element on the other hand, it is characterized in that, described target substance extraction element is equipped with: be used to accommodate the hydrophobic fluid composition of the solid-state object being treated, hydrophilic fluid composition and supercriticality or the subcritical state that contain target substance, extract the extraction tank of target substance from described object being treated; Fractionation is with the hydrophilic fluid fractionation path of the described hydrophilic fluid composition cut that is principal component from described extraction tank; Fractionation is with the hydrophobic fluid fractionation path of the described hydrophobic fluid composition cut that is principal component from described extraction tank; From cut, separate first separator of described target substance by the fractionation of described hydrophilic fluid fractionation path institute; And, from cut, separate second separator of described target substance by the fractionation of described hydrophobic fluid fractionation path institute.
The present invention also relates to a kind of target substance extraction element on the other hand, it is characterized in that, described target substance extraction element is equipped with: be used to accommodate the hydrophobic fluid composition of the solid-state object being treated, hydrophilic fluid composition and supercriticality or the subcritical state that contain target substance, extract the extraction tank of target substance from described object being treated; Fractionation is with the hydrophilic fluid fractionation path of the described hydrophilic fluid composition cut that is principal component from described extraction tank; The fluid drain passageway that is connected with the upper portion of described extraction tank; The high-pressure separator of the fluid that storage is discharged from described extraction tank; Be connected with the upper portion of described high-pressure separator, fractionation is with the hydrophobic fluid fractionation path of the described hydrophobic fluid composition cut that is principal component; From cut, separate first separator of described target substance by the fractionation of described hydrophilic fluid fractionation path institute; And, from cut, separate second separator of described target substance by the fractionation of described hydrophobic fluid fractionation path institute.
Adopt said apparatus, when from object being treateds such as natural agricultural product, extracting target substance, the abstraction process that does not need other, by single extraction operation, can extract contained all types of target material in the object being treated with high-purity on one side, on one side all types of target material contained in the object being treated is separated into hydrophily target substance and hydrophobicity target substance respectively.
In addition, consider preferred outfit the: the hydrophilic fluid composition storagetank of storing above-mentioned hydrophilic fluid composition from the aspect that each fluid composition is mixed fully and contact; To supply with the hydrophilic fluid composition supply passageway of said extracted groove from the above-mentioned hydrophilic fluid composition in this hydrophilic fluid composition storagetank; Store the hydrophobic fluid composition storagetank of above-mentioned hydrophobic fluid composition; To supply with the hydrophobic fluid composition supply passageway of said extracted groove from the above-mentioned hydrophobic fluid composition in this hydrophobic fluid composition storagetank, be equipped with above-mentioned hydrophilic fluid composition supply passageway and above-mentioned hydrophobic fluid composition supply passageway, so that above-mentioned hydrophilic fluid composition and above-mentioned hydrophobic fluid composition are conducted in the said extracted groove in the mode of convection current.
In addition, from each fluid composition being mixed fully and contacting, and the aspect that makes fractionation become easy considers that preferred connected mode is: connect above-mentioned hydrophilic fluid composition supply passageway the hydrophilic fluid composition is supplied with from the downward quadrate part of the upper portion of extraction tank; Connect above-mentioned hydrophobic fluid composition supply passageway and make of the following quadrate part upward portion supply of hydrophobic fluid composition from extraction tank; Connect above-mentioned hydrophilic fluid fractionation path and make the cut that partly to heat up in a steamer with above-mentioned hydrophilic fluid composition from the below of described extraction tank be principal component.
In addition, consider, preferably connect above-mentioned hydrophobic fluid fractionation path and make from stating the cut that the hydrophobic fluid composition is a principal component more than the upper portion fractionation of said extracted groove from the aspect that can make fractionation become easy.
In addition, from considering by the aspect that can make the contact area of both sides' fluid composition become bigger with vesicle shape supply fluid composition, the said extracted groove preferably has the porous scutum, and this porous scutum is used for making in this extraction tank at least one side of above-mentioned hydrophilic fluid composition and above-mentioned hydrophobic fluid composition to disperse with the vesicle shape.
In addition, consider the preferred EGR of at least a portion of the cut of institute's fractionation being supplied with the said extracted groove that is equipped with from the target substance concentration aspect of the cut that can improve the hydrophilic fluid composition.
In addition, consider from the aspect that can recycle this hydrophobic fluid composition, preferably in above-mentioned second separator, be equipped with condenser, be used for the above-mentioned hydrophobic fluid composition that condensation separates with above-mentioned target substance, and this hydrophobic fluid composition is reverted in the above-mentioned hydrophobic fluid composition storagetank.
Utilizability on the industry
Target substance extracting method of the present invention is applicable in optionally carrying from object being treated Get target substance.
Claims (14)
1. a target substance extracting method is characterized in that, comprises following operation:
Make the hydrophilic fluid composition mix the formation high-pressure mixing fluid in the mode that surpasses mutual solubility with the hydrophobic fluid composition of supercriticality or subcritical state, this high-pressure mixing fluid is contacted with the solid-state object being treated that contains target substance, target substance contained in this object being treated is extracted into the operation among at least one side of described hydrophilic fluid composition or described hydrophobic fluid composition;
Fractionation is with described hydrophilic fluid composition cut that is principal component and the operation that is the cut of principal component with described hydrophobic fluid composition from described high-pressure mixing fluid; And
The operation of from least one side's described cut, separating described target substance.
2. target substance extracting method as claimed in claim 1, wherein, from the cut that is principal component with described hydrophilic fluid composition, extract the hydrophily target substance, from the cut that is principal component with described hydrophobic fluid composition, extract the hydrophobicity target substance simultaneously.
3. target substance extracting method as claimed in claim 1, wherein, described object being treated is immersed in the fluid composition of the either party in described hydrophilic fluid composition and the described hydrophobic fluid composition, obtain maceration extract, in this maceration extract, mix the opposing party's fluid composition, described object being treated is contacted with described high-pressure mixing fluid.
4. target substance extracting method as claimed in claim 1 wherein, with vesicle shape supply the opposing party's fluid composition, forms described high-pressure mixing fluid in the fluid composition of the either party in described hydrophilic fluid composition and described hydrophobic fluid composition.
5. target substance extracting method as claimed in claim 1 wherein, is supplied with described hydrophilic fluid composition and described hydrophobic fluid composition in the mode of convection current, forms described high-pressure mixing fluid.
6. target substance extracting method as claimed in claim 1 wherein, as described hydrophilic fluid composition, is used to be selected from least a in water, methyl alcohol, the ethanol; As described hydrophobic fluid composition, use to be selected from least a in carbon dioxide, nitrous oxide, the propane.
7. a target substance extraction element is characterized in that, is equipped with:
Extraction tank is used to accommodate the hydrophobic fluid composition of the solid-state object being treated, hydrophilic fluid composition and supercriticality or the subcritical state that contain target substance, and extracts target substance from described object being treated;
Hydrophilic fluid fractionation path, the cut that fractionation is a principal component with described hydrophilic fluid composition from described extraction tank;
Hydrophobic fluid fractionation path, the cut that fractionation is a principal component with described hydrophobic fluid composition from described extraction tank;
First separator from the cut by the fractionation of described hydrophilic fluid fractionation path institute, separates described target substance; And,
Second separator from the cut by the fractionation of described hydrophobic fluid fractionation path institute, separates described target substance.
8. a target substance extraction element is characterized in that, is equipped with:
Extraction tank is used to accommodate the hydrophobic fluid composition of the solid-state object being treated, hydrophilic fluid composition and supercriticality or the subcritical state that contain target substance, and extracts target substance from described object being treated;
Hydrophilic fluid fractionation path, the cut that fractionation is a principal component with described hydrophilic fluid composition from described extraction tank;
The fluid drain passageway is connected with the upper portion of described extraction tank;
High-pressure separator is stored the fluid of discharging from described extraction tank;
Hydrophobic fluid fractionation path is connected with the upper portion of described high-pressure separator, the cut that fractionation is a principal component with described hydrophobic fluid composition;
First separator from the cut by the fractionation of described hydrophilic fluid fractionation path institute, separates described target substance; And,
Second separator from the cut by the fractionation of described hydrophobic fluid fractionation path institute, separates described target substance.
9. as claim 7 or 8 described target substance extraction elements, wherein, be equipped with:
Hydrophilic fluid composition storagetank is stored described hydrophilic fluid composition;
Hydrophilic fluid composition supply passageway will be supplied with described extraction tank from the described hydrophilic fluid composition of this hydrophilic fluid composition storagetank;
Hydrophobic fluid composition storagetank is stored described hydrophobic fluid composition;
Hydrophobic fluid composition supply passageway will be supplied with described extraction tank from the described hydrophobic fluid composition of this hydrophobic fluid composition storagetank,
Be equipped with described hydrophilic fluid composition supply passageway and described hydrophobic fluid composition supply passageway, so that described hydrophilic fluid composition and described hydrophobic fluid composition are conducted in the described extraction tank in the mode of convection current.
10. target substance extraction element as claimed in claim 9, wherein,
Connect described hydrophilic fluid composition supply passageway, so that the hydrophilic fluid composition is supplied with from the downward quadrate part of the upper portion of extraction tank;
Connect described hydrophobic fluid composition supply passageway, so that the hydrophobic fluid composition is from following quadrate part portion's supply upward of extraction tank;
Connect described hydrophilic fluid fractionation path and make the cut that partly to heat up in a steamer with described hydrophilic fluid composition from the below of described extraction tank be principal component.
11. target substance extraction element as claimed in claim 7 wherein, connects described hydrophobic fluid fractionation path, so that from the upper portion fractionation of the described extraction tank cut that is principal component with described hydrophobic fluid composition.
12. as claim 7 or 8 described target substance extraction elements, wherein, described extraction tank has the porous scutum, this porous scutum is used for making in this extraction tank at least one side of described hydrophilic fluid composition and described hydrophobic fluid composition to disperse with the vesicle shape.
13. as claim 7 or 8 described target substance extraction elements, wherein, the EGR of described extraction tank is supplied with at least a portion of the cut of institute's fractionation in outfit.
14. as claim 7 or 8 described target substance extraction elements, wherein, be equipped with condenser in described second separator, the described hydrophobic fluid composition that condensation separates with described target substance reverts in the described hydrophobic fluid composition storagetank this hydrophobic fluid composition.
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| JP2006232103A JP4113230B2 (en) | 2006-08-29 | 2006-08-29 | Target substance extraction method and target substance extraction apparatus |
| JP232103/2006 | 2006-08-29 |
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| CNA2007800252706A Pending CN101484224A (en) | 2006-08-29 | 2007-08-14 | Target substance-extracting method and target substance-extracting device |
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| JP (1) | JP4113230B2 (en) |
| KR (1) | KR20090038470A (en) |
| CN (1) | CN101484224A (en) |
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| CN106022117A (en) * | 2016-05-18 | 2016-10-12 | 北京金山安全软件有限公司 | Method and device for preventing system environment variable from being modified and electronic equipment |
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| CN101905090B (en) * | 2010-05-31 | 2012-08-15 | 中国农业大学 | Method for extracting polar or medium polar plant source natural product |
| US10016700B2 (en) | 2013-07-22 | 2018-07-10 | Yong Cao | Multifunctional continuous phase transition extraction apparatus |
| GB201707758D0 (en) | 2017-05-15 | 2017-06-28 | British American Tobacco Investments Ltd | Ground tobacco composition |
| CN113559550B (en) * | 2021-08-26 | 2022-04-05 | 山西大学 | Method and device for extracting flavone from day lily |
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| DE2827002B2 (en) * | 1978-06-20 | 1980-09-04 | Adam Dr. 8421 St Johann Mueller | Process for treating hops with CO2 as extraction agent |
| JPH0651084B2 (en) * | 1990-11-28 | 1994-07-06 | 通商産業省基礎産業局長 | How to purify alcohol |
| JP3264515B2 (en) * | 1992-05-28 | 2002-03-11 | 日本たばこ産業株式会社 | Method and apparatus for extracting soluble matter from natural solid raw material |
| JPH0910502A (en) * | 1995-06-30 | 1997-01-14 | Japan Tobacco Inc | Extraction process for object component out of natural solid raw material |
| JP3042830B2 (en) * | 1996-01-29 | 2000-05-22 | 日本炭酸株式会社 | Continuous processing equipment using supercritical fluid |
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| CN106022117A (en) * | 2016-05-18 | 2016-10-12 | 北京金山安全软件有限公司 | Method and device for preventing system environment variable from being modified and electronic equipment |
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| WO2008026446A1 (en) | 2008-03-06 |
| KR20090038470A (en) | 2009-04-20 |
| JP4113230B2 (en) | 2008-07-09 |
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