JP2019150825A - Extract manufacturing apparatus - Google Patents

Abstract

To provide an extract manufacturing apparatus.SOLUTION: An extract manufacturing apparatus 30 comprising: (a) closed ring system 10 which can hold a fluid which behaves as a gas; (b) a driven machine 15 which circulates the fluid in the closed ring system 10; (c) a raw material vessel 12 which is provided in the closed ring system, and through which the fluid passes; (d) a feeder 11 which feeds vapor of an extractant having an extraction temperature, which is a standard boiling point or less, into the closed ring system 10; (e) a discharger 18 which discharges at least a gas other than vapor from the closed ring system 10; (f) a controller 40 which monitors a pressure in the closed ring system 10, and thus, causes the discharger 18 to discharge the gas until at least a pressure in the closed ring system 10 is an equilibrium vapor pressure or les of the extractant at the extraction temperature; and (g) a distributor having a bubbling unit which obtains extract from the fluid.SELECTED DRAWING: Figure 2

Description

  The present invention relates to an apparatus for producing an extract, and particularly relates to an apparatus suitable for extracting components from biological materials.

  Patent Document 1 discloses an apparatus for extracting components from plants and animals. FIG. 1 cited from the patent document shows a closed circulation path 90 of the apparatus. In the circulation path 90, a generation tank 91, an extraction device 92, a condensing device 93, a storage tank 94, and a blower 95 are provided in this order. The generation tank 91 generates water atomized fine particles by ultrasonic vibration. The atomized fine particles are sent to the extraction device 92 by the air flow created by the blower 95.

  The extraction device 92 can be filled with crushed pieces of raw material. Within the extraction device 92, atomized microparticles pass between the fragments. The fragment pieces packed in the extraction device 92 resist the air flow created by the blower 95. For this reason, a decompression space is generated in the extraction device 92. In the reduced pressure space, the active ingredient is sucked out from the crushed pieces toward the atomized fine particles. The condensing device 93 generates water containing the active ingredient by condensing the atomized microparticles holding the active ingredient. Water is transferred to storage tank 94.

  The apparatus described in Patent Document 1 can efficiently extract components from a raw material by using a reduced pressure space. Therefore, it is possible to extract active ingredients that could not be extracted by the conventional distillation method or solution extraction method (paragraphs [0002]-[0004] and [0009]).

JP 09-248138 A JP 2011-000515 A Special table 2011-508034 gazette

  As described above, the apparatus of Patent Document 1 uses the air flow to generate a decompressed space. Thus, the raw material is exposed to a large amount of air flow as well as atomized microparticles. For this reason, the extracted component may be altered by air.

[1] (a) a ring-closing system containing a vapor of an extractant and a drain formed by changing the phase of the vapor into a liquid and capable of holding a fluid that behaves as a gas;
(B) a driven machine for circulating the fluid in the closed system;
(C) a raw material container provided in the ring-closing system and through which the fluid passes;
(D) a supply device for supplying the steam having an extraction temperature below the normal boiling point of the extractant into the ring-closing system;
(E) a discharge device that discharges at least a gas other than the vapor from within the ring-closing system;
(F) By monitoring the pressure in the closed system, the gas is discharged to the discharge device until at least the pressure in the closed system is equal to or lower than the equilibrium vapor pressure of the extractant at the extraction temperature. A control device,
(G) A distribution device that collects an extract by separating drainage having a high density from the fluid by selecting the fluid by density, and returns the remainder containing the drainage and vapor having a low density to the closed system;
An extract production apparatus comprising:

[2] The distributor has a cyclone separator,
The cyclone separator sorts the fluid by density,
[1] The manufacturing apparatus.

[3] The control device weakens or stops the discharge of the gas by the discharge device when the pressure in the closed system becomes equal to the saturated vapor pressure of the extractant.
[1] or [2] manufacturing apparatus.

[4] The supply device includes a heater for heating the liquid phase extractant,
The control device monitors the temperature of the fluid and causes the heater to heat the liquid phase extractant until the temperature of the fluid reaches at least the extraction temperature.
The manufacturing apparatus in any one of [1]-[3].

[5] The supply device further includes a pot that forms part of the ring-closing system,
The raw material container is disposed in the pot, and the space in the pot is configured as a vapor reservoir and surrounds the raw material container, so that the raw material container is separated from the outside world,
The pot further comprises a reservoir for the extractant in the liquid phase,
The heater is provided in the reservoir;
The extractant is released into the vapor reservoir;
[4] The manufacturing apparatus.

A method for producing an extract using the production apparatus according to any one of [1] to [5],
(A) Air-tightening the closed system filled with a gas other than the vapor in a state where the raw material is installed in the raw material container,
(B) While supplying the steam into the closed system by the supply device, at least gas other than the steam is discharged from the closed system, and the fluid is circulated in the closed system by the driven machine. Thus, the gas in the closed ring system is replaced with the vapor,
(C) By allowing the gas to be discharged by the control device and the discharge device, the inside of the closed system is filled with the steam,
(D) removing a component in the raw material from the raw material by bringing the fluid having the extraction temperature into contact with the raw material;
(E) The distribution device collects the extract by separating the high-density drain from the fluid by selecting the fluid according to the density, and the remainder containing the low-density drain and vapor is added to the ring-closing system. Circulating the remainder again in the closed system by returning;
Method.

Increasing the extraction temperature step by step for a predetermined time,
Collecting the extract individually for each extraction temperature;
The method of [6].

The extractant is water;
The steam is water vapor;
The extract contains an aromatic component,
[6] or [7].

  In the production apparatus of the present invention, components are extracted from the raw material in an environment filled with steam, so that the extracted components can be prevented from being altered by air.

Block diagram of manufacturing equipment of background art Block diagram of the manufacturing apparatus of the embodiment Schematic diagram of the manufacturing apparatus of the example 1 Block diagram of extract device of comparative example Schematic diagram of the manufacturing apparatus of the example 2 Analysis result 1 of gas chromatography Analysis result of gas chromatography 2 Analysis result of gas chromatography 3 Schematic diagram of comparative example extraction device Schematic diagram of the manufacturing apparatus of the example 3

[1. Extract liquid manufacturing equipment]

  The configuration of the manufacturing apparatus of the present embodiment will be described with reference to the block diagram of FIG. FIG. 2 shows an extract manufacturing apparatus 30. The manufacturing apparatus 30 includes a closed ring system 10. The closed ring system 10 has a structure capable of holding a fluid that behaves as a gas. The ring-closing system 10 is formed by connecting the devices including the supply device 11 through paths 21, 22, 24 and 25.

  In this specification, “fluid” is a fluid that behaves as a gas. The fluid is mainly composed of the gas phase. There is some liquid phase in the fluid. The liquid phase becomes, for example, a mist and does not strongly harm the behavior of the gas phase. In other words, the liquid phase and the gas phase coexist. The liquid phase and the gas phase are preferably made of the same extractant. The extractant will be described later.

  The manufacturing apparatus 30 includes a driven machine 15 provided in the closed ring system 10. The driven machine 15 circulates the fluid in the ring-closing system 10 in the direction of the arrow in the figure. The driven machine 15 forms a part of the closed ring system 10.

  As used herein, “driven machine” is a machine that converts mechanical energy into fluid energy. An example of a “driven machine” is a blower. Examples of blowers are fans and blowers. A fan refers to a blower having a pressure ratio of 1.1 or less. A blower refers to a blower having a pressure ratio of about 1.1-2. Another example of a “driven machine” is a pump.

  The manufacturing apparatus 30 illustrated in FIG. 2 includes a supply apparatus 11 and a path 21. The path 21 is connected to the supply device 11. The supply device 11 sends the fluid to the path 21. The supply device 11 forms part of the closed ring system 10.

  The supply device 11 shown in FIG. 2 supplies the extractant vapor into the closed ring system 10. In the supply device 11, the steam is mixed with the fluid. The circulating fluid contains such steam and drain derived from the steam. Vapor is a gas. “Vapor” as used herein is the gas phase of the extractant and is not a liquid phase such as so-called mist or drain.

  The supply device 11 shown in FIG. 2 does not actively supply the liquid phase of the extractant. However, it is not excluded from the scope of the present invention that the liquid phase inevitably supplied is mixed with steam due to the characteristics of the supply device 11 that supplies steam.

  In this specification, “drain” is a state in which vapor, which is a gas, has undergone a phase change to a liquid. Drain is a form in which the extractant, which was originally in the liquid phase, recondenses from the gas phase and returns to the liquid phase. In the closed ring system, the drain may evaporate again and return to the liquid phase. The drain includes those in which the molecules of the extractant are clustered. The drain may behave like a gas in the fluid in the closed system. The drain may behave as a mist that is an aggregate of particles in the fluid in the closed ring system.

  In the present specification, the “extractant” is a substance that becomes a vapor-liquid equilibrium in a standard state. In this specification, “vapor-liquid equilibrium” means that the evaporation and vaporization reaction from liquid to gas is the same as the condensation and liquefaction reaction from gas to liquid, and as a result, the amount of liquid and gas does not change. It is a state that seems to be.

  In other words, the saturated vapor pressure of the extractant is less than the standard pressure (101.325 kPa) at a temperature of 25 ° C. Further, the extractant does not coagulate in an environment where the temperature is 25 ° C. and less than the standard atmospheric pressure. The normal boiling point of the extractant is the boiling point at normal atmospheric pressure.

  Examples of extractants are water, ethanol, methanol, 1,3-butylene glycol (BG), 1-butanol, hexane and ethyl acetate. A preferred extractant is water. The extractant may be a single substance or a mixture thereof. The extractant serves as a medium for extracting components from the raw material. An additive may be added to the extractant. The additive may act on the component extracted from the raw material or may protect the component.

  Unless otherwise specified, the “component” in the present specification includes substances contained in the raw material and substances extracted from the raw material. New substances produced by changing the chemical structure of these substances in the process of producing the extract are included in the components. A new substance produced by spontaneously changing the chemical structure of a substance extracted from the raw material after the extract is produced in the extract is included in the components. In this specification, the “extract” is a product that contains a so-called (active) component. For example, distilled water or purified water that does not contain a specific (active) component is not an extract in this specification. These are rather examples of what can be used as an extractant or an extraction solvent.

  Some of the components may contain active ingredients. As used herein, “active ingredient” refers to a substance having physiological activity. The component may contain a substance having a weak physiological activity or a physiological activity that cannot be confirmed. For example, a substance that emits a scent but is unclear whether it has a specific physiological activity is a kind of component. A component may refer to a collection of these substances.

  After producing the extract, the components may or may not remain in the raw material. After producing the extract, the components are preferably contained in the extract. The component may be hydrophilic or lipophilic. The component may be dissolved or dispersed in the extract.

  The temperature of the vapor of the extractant supplied by the supply device 11 shown in FIG. 2 is preferably a predetermined extraction temperature. The extraction temperature is a temperature set for extracting a component from the raw material 50 a arranged in the raw material container 12. The extraction temperature is preferably below the normal boiling point of the extractant. The extraction temperature may be higher than the normal boiling point of the extractant. When the extractant is water, the extraction temperature is preferably 10 ° C or higher and 140 ° C or lower. The extraction temperature may be any of 20, 30, 40, 50, 60, 70, 80, 90, 100, 110, 120, and 130 ° C.

  The supply device 11 shown in FIG. 2 may supply steam having a temperature not higher than the extraction temperature. By heating such steam in the closed ring system 10, the temperature may be set as the extraction temperature. The supply device 11 may supply steam having a temperature equal to or higher than the extraction temperature. By cooling such steam in the closed ring system 10, the temperature may be set as the extraction temperature.

  The manufacturing apparatus 30 illustrated in FIG. 2 includes a raw material container 12 and a path 22. The raw material container 12 is provided in the closed ring system. The paths 21 and 22 are connected to the raw material container 12. The fluid flows from the supply device 11 to the raw material container 12 via the path 21. The fluid passes through the raw material container 12. The raw material container 12 sends the fluid to the path 22. The raw material container 12 forms a part of the closed ring system 10. It is preferable that the ring-closing system 10 is not provided with another path that bypasses the raw material container 12.

  The manufacturing apparatus 30 shown in FIG. 2 includes a distribution apparatus 13 and paths 23 and 24. The paths 23 and 24 are connected to the distribution device 13. The fluid flows from the raw material container 12 to the distribution device 13 via the path 22. The distribution device 13 forms part of the closed ring system 10.

  The distribution device 13 shown in FIG. 2 sorts the fluid based on its density. In this specification, the “density” of the drain depends on the size of the liquid phase particles constituting the “drain”. If the drain is composed of only the extractant, there is no difference in density as a liquid between the drain particles. On the other hand, in the fluid before being sorted, it is considered that both the drain having a large density and the drain having a small density are scattered in the fluid evenly.

  In this specification, “density” represents the density as a so-called gas of the drain particles that behave as a gas. The drain has a particle size distribution. It may be considered that a drain having a relatively large particle size has a high density and a drain having a relatively small particle size has a low density.

  As shown in FIG. 2, the distributor 13 sorts the fluid into a drain 19a (large circle), a drain 19b (small circle), and a vapor (dot). The drain 19a is a drain having a relatively large density or a set thereof. The drain 19b is a drain having a relatively low density or a set thereof. The drain 19b selected in the distribution device 13 is mixed with steam. The figure schematically shows the function of the distributor 13 and does not necessarily represent a physicochemically accurate state.

  An example of the distributor 13 is a cyclone separator. Other examples of distribution device 13 are spacer columns, collision distribution devices, baffle plates, packed bed collectors, wire mesh collectors. A spacer column refers to a long vertical tube or pipe through which the vapor-liquid mixture flows vertically upwards.

  The distributor 13 shown in FIG. 2 separates the drain 19a from the fluid. The distributor 13 sends the drain 19a to the path 23. Thereby, the distribution device 13 collects the drain 19a as the extract 20.

  The manufacturing apparatus 30 shown in FIG. The path 23 connects to the collection container 14. The drain 19a, that is, the extract, flows from the distributor 13 to the collection container 14 via the path 23. The collection container 14 stores the collected extract 20. The collection container 14 may be a container that can be detachably attached to the distribution device 13.

  The remainder is obtained by separating the drain 19a from the fluid by the distributor 13 shown in FIG. The balance includes drain 19b and steam. The remainder is returned to the closed ring system 10. The distributor 13 sends the remainder as a fluid to the path 24.

  The manufacturing apparatus 30 shown in FIG. The paths 24 and 25 are connected to the driven machine 15. The fluid flows from the distributor 13 to the driven machine 15 via the path 24. The path 25 is connected to the supply device 11. The driven machine 15 sends the fluid to the path 25 while applying momentum to the fluid. The fluid is sent from the driven machine 15 via the path 25 to the supply device 11. As described above, the fluid circulates in the closed ring system 10.

  The driven machine 15 shown in FIG. 2 is preferably provided at a location downstream of the location where the steam is supplied from the supply device 11 and upstream of the location where the raw material container 12 is provided.

  The manufacturing apparatus 30 shown in FIG. The discharge device 18 is connected to the closed ring system 10. For example, the discharge device 18 is connected to the path 21. The discharge device 18 may be connected to another route. In the embodiment described later, the discharge device 18 is connected to the supply device 11. The discharge device 18 is provided for discharging a gas other than the vapor from the closed ring system 10. The discharge device 18 discharges at least a gas other than the vapor from the closed system 10.

  In one example, the gas other than steam is air. In one example, air is air that has existed in the closed system before supplying steam to the closed system, or air that has entered the closed system from the outside of the closed system.

  The manufacturing apparatus 30 shown in FIG. The control device 40 is composed of a computer, for example. Preferably, the control device 40 is connected to the discharge device 18 in a wired or wireless manner. Preferably, the control device 40 controls the discharge device 18 by sending a signal to the discharge device 18.

  The control device 40 shown in FIG. 2 monitors the pressure in the closed ring system 10. The controller 40 acquires or stores in advance the equilibrium vapor pressure of the extractant at the extraction temperature. In the present specification, the “equilibrium vapor pressure” is the pressure of the vapor phase that is in equilibrium with the liquid phase at a constant temperature. The control device 40 causes the discharge device 18 to discharge gas until the pressure in the closed ring system 10 is at least equal to or lower than the equilibrium vapor pressure of the extractant at the extraction temperature.

  The control device 40 shown in FIG. 2 preferably weakens or stops the discharge of gas by the discharge device 18 when the pressure in the closed ring system 10 becomes equal to the saturated vapor pressure of the extractant. “Saturated vapor pressure” is the vapor pressure at which a vapor of an extractant is in equilibrium with the pure liquid phase of the extractant at a certain temperature. “Saturated steam” is steam at a temperature equal to the boiling point at that pressure. The fluid preferably contains a saturated vapor of extractant at the extraction temperature.

  The control device 40 shown in FIG. 2 controls the pressure and temperature in the closed ring system 10. The manufacturing apparatus 30 can extract components with water vapor even at a low temperature of about 30 ° C. The manufacturing apparatus 30 distributes low-temperature steam to the inside of the raw material placed in a reduced pressure environment. In the manufacturing apparatus 30, the alteration of the component due to heat and the destruction of the raw material structure are unlikely to occur. Therefore, the target component can be extracted without heat denaturation, and unnecessary components that are eluted by destruction of the plant tissue can be minimized. Furthermore, it can extract continuously. When extracting continuously, the temperature of the fluid circulating in the closed ring system 10 can be raised stepwise. Therefore, there is a high possibility that an extract having a unique composition is contained in the extract.

  During the operation of the manufacturing apparatus 30 shown in FIG. 2, the ring-closing system 10 is kept airtight. Here, the airtight maintenance particularly means that gas from the outside of the closed ring system 10, for example, air does not enter the closed ring system 10 as an example. As can be seen from the fact that the discharge device 18 and the distribution device 13 are provided in the manufacturing apparatus 30, airtightness does not necessarily mean that complete airtightness is maintained in the closed ring system 10. Moreover, when extracting at low temperature, since the pressure in the closed ring system 10 is not high, the large-scale apparatus for maintaining the airtightness of the closed ring system 10 is unnecessary.

[2. Extract liquid manufacturing method]

  The extraction method of this embodiment using the manufacturing apparatus of this embodiment will be further described with reference to FIG. The active ingredient is extracted from the extract by the extraction method of this embodiment. Hereinafter, an extract having an aroma component received from a raw material in particular may be referred to as an aroma extract. First, the raw material 50 a is installed in the raw material container 12. In this state, the closed ring system 10 filled with a gas other than the extractant vapor is hermetically sealed.

  As used herein, “raw material” includes a raw material derived from any organism including animals, plants, and fungi. Living organisms include natural ones or artificially grown ones. The raw material may be a living body or may not be a living body. The raw material may be part of a biological body. The component may be contained in the cells of the organism that is the raw material, or may not be contained in the cells. The raw material may be a biological secretion. The raw material may or may not be pretreated beforehand. The raw material may be previously crushed or not crushed.

  The raw material is preferably a plant body. The body of the plant may be raw, dried or fermented. The plant body may be washed in advance. Plant leaves, stems, roots, flowers, seeds, bark, and other organs are all plant bodies that can be used as raw materials. The plant may be edible or non-edible. Plants can be herbs. The plant may be suitable for fragrance production. The plant may be herbal medicine.

  Next, steam is supplied into the closed ring system 10 by the supply device 11 shown in FIG. During the supply of steam, at least gases other than the steam are discharged from the closed ring system 10. The discharging may be performed by the discharging device 18. The fluid is circulated in the closed ring system 10 by the driven machine 15 while supplying the steam and discharging the gas. Thereby, the gas in the closed ring system 10 is replaced with steam.

  Further, gas is continuously discharged by the control device 40 and the discharge device 18 shown in FIG. As the exhausted gas, for example, air newly entering the closed system through the boundary between the closed system 10 and the atmospheric environment is applicable. The state in which the closed ring system 10 is filled with steam is maintained by continuous gas discharge.

  The raw material 50a shown in FIG. 2 is continuously exposed to the full steam. A gas phase or liquid phase extractant contacts the raw material 50a. A fluid having an extraction temperature is brought into contact with the raw material 50a. Thereby, the component in the raw material 50a is taken out. When the component is taken out from the raw material 50a, the component is dissolved in the extractant.

  It is not limited whether an extractant is a gaseous phase or a liquid phase. Further, the ratio of the component taken into the gas phase and the ratio of the component taken into the liquid phase may be different depending on the temperature of the extractant. Such an extractant is extracted together with the components in a distributor.

  The fluid is selected according to the density by the distribution device 13 shown in FIG. The extract 20 is collected by separating the dense drain 19a from the fluid. Further, the low-density drain 19b and the remainder containing the steam are returned to the ring-closing system 10. As a result, the remainder is circulated again in the closed ring system 10.

  When using the manufacturing apparatus 30 shown in FIG. 2, you may use water as an extractant. When water is used, the steam to which the raw material is exposed is water vapor. The resulting extract 20 is an aroma extract.

[3. Action and Effect]

  With reference to FIG. 2, operations and effects brought about by the manufacturing apparatus and the manufacturing method of the present embodiment will be described below. Such description is not intended to limit the scope of the invention.

  In the manufacturing apparatus 30 shown in FIG. 2, a component is extracted from the raw material 50a in the environment where the closed ring system 10 is filled with steam. For this reason, it can suppress that the extracted component changes in quality by air.

  In the manufacturing apparatus 30 shown in FIG. 2, the remainder selected from the drain having a high density is circulated again in the ring-closing system 10. For this reason, during operation of the manufacturing apparatus 30, the supply apparatus 11 only needs to replenish an amount of steam corresponding to the extractant taken out from the closed ring system 10 as the extraction liquid 20.

  In the manufacturing apparatus 30, a drain having a high density is selectively collected to obtain a liquid. Rich components are dissolved in the dense drain under suitable conditions. Accordingly, an extract 20 rich in components can be obtained. The steam returned to the closed ring system 10 as the remainder is used again for extraction of components from the raw material 50a.

[4. Modified example]

  Note that the present invention is not limited to the above-described embodiment, and can be changed as appropriate without departing from the spirit of the present invention.

  For example, the manufacturing apparatus 30 shown in FIG. 2 may have a supply device 17 instead of the supply device 11 provided in the closed ring system 10. The supply device 17 does not constitute a ring of the closed ring system 10. The supply device 17 is located outside the closed ring system 10. The supply device 17 is connected to the center of the path 21 through a pipe line, for example. The supply device 17 sends steam into the path 21. The steam is mixed with the fluid at the portion where the supply device 17 and the closed ring system 10 are connected. This vapor may be water vapor or vapor of an extractant other than water.

  In FIG. 2, when the extract 20 is manufactured, the extraction temperature may be increased step by step every predetermined time. Moreover, you may collect the extract 20 separately for every extraction temperature. For example, a stopcock may be provided in the path 23 and the collection container 14 may be detachable from the path 23. The extract 20 at each extraction temperature can be recovered by closing the stopcock and removing the collection container 14 from the manufacturing apparatus 30 every predetermined time. That is, the container may be attached / detached / replaced for each preferable extraction temperature or for each extraction elapsed time zone. Thereby, it becomes possible to fractionate the fraction for every preferable extraction temperature or every elapsed time zone of extraction into different containers.

  Before the discharge device 18 is operated, the closed system 10 is normally filled with air. In a modification, the inside of the closed ring system 10 may be filled with an inert gas in advance. The inert gas may be nitrogen. The use of the inert gas is useful for preventing oxidation of the active component to be extracted, other components, or the extract 20 containing these components.

[5. Manufacturing equipment design]

  An example of the manufacturing apparatus 30 will be described with reference to the schematic diagram of FIG. The points to be noted about the drawings are as follows. The collection container 14 and the path 23 shown in FIG. 2 are omitted in the manufacturing apparatus 30 shown in FIG. The path 21 shown in FIG. 2 is depicted in FIG. 3 as a communication portion at the boundary between the internal space (steam reservoir 47) of the supply device 11 and the internal space of the raw material container 12.

  The supply device 11 shown in FIG. 3 includes a pot 43 that forms a part of a closed ring system. The raw material container 12 is disposed in the pot 43. An opening and a lid are provided on the top of the pot 43. The raw material is sent into the raw material container 12 through the opening. The extractant 45 is put into the pot 43 through the opening. Close the opening with the lid. Through the opening, the liquid accumulated in the tray 51 described later is taken out.

  The bottom of the space in the pot 43 shown in FIG. 3 is used as a reservoir 46 for storing the liquid phase extractant 45. A drainage port 48 is provided on the bottom surface of the pot 43. After the extraction of the components from the raw materials 50a to 50c is finished, the excess extractant 45 is discharged from the drain port 48.

The upper part of the space in the pot 43 shown in FIG. The vapor reservoir 47 surrounds the raw material container 12. The raw material container 12 is separated from the outside, that is, the outside of the pot 43 by the vapor reservoir 47. The fluid in the raw material container 12 is not easily affected by heat or cold outside the pot 43. The component can be extracted from the raw material at a stable extraction temperature.

  In FIG. 3, a ring-closing system is formed by connecting the end portion 28A to the end portion 29A and the end portion 28B to the end portion 29B. These ends will be described later. The vapor reservoir 47 forms a part of a closed ring system. The extractant that has become steam goes around the ring-closing system in the order of the path 21, the raw material container 12, the path 22, the distribution device 13, the path 24, the driven machine 15, and the path 25 in order from the steam reservoir 47, and returns to the steam reservoir 47.

  The supply device 11 shown in FIG. 3 includes a heater 44a. The heater 44 a is located in the storage unit 46. The heater 44 a is connected to the control device 40 through the network 41. The liquid phase extractant 45 becomes steam by being heated by the heater 44a. The extractant that has become vapor is discharged toward the vapor reservoir 47.

  The supply device 11 further includes a cooler 44b. The cooler 44 b is located in the storage unit 46. The heater 44 a and the cooler 44 b are connected to the control device 40 through the network 41.

  The manufacturing apparatus 30 shown in FIG. 3 includes a compound meter 34, a pressure sensor 35, and a temperature sensor 36. These devices are connected to the vapor reservoir 47 through a pipe line. The compound meter 34 displays the atmospheric pressure in the vapor reservoir 47. The atmospheric pressure in the vapor reservoir 47 is preferably 1 atm or less during the operation of the manufacturing apparatus 30.

  The pressure sensor 35 detects the pressure of the fluid in the vapor reservoir 47. The pressure sensor 35 sends information on the pressure of the fluid to the control device 40 through the network 41. The temperature sensor 36 detects the temperature of the fluid in the vapor reservoir 47. The temperature sensor 36 sends information on the temperature of the fluid to the control device 40 through the network 41.

  The network 41 shown in FIG. 3 may be wired or wireless. A connection path between the control device 40 and each device is schematically depicted as a network 41. Some or all of the connection paths may be independent of each other.

  The discharge device 18 shown in FIG. 3 includes a gas-liquid separator 38 and a vacuum pump 39. The vacuum pump 39 sucks the fluid from the closed system without distinguishing between the vapor and the gas other than the vapor. The gas-liquid separator 38 is provided between the vacuum pump 39 and the ring closing system. In this embodiment, the gas-liquid separator 38 is connected to the vapor reservoir 47.

  During operation of the vacuum pump 39 shown in FIG. 3, the gas-liquid separator 38 operates to collect drainage and mist. This prevents drain and mist from entering the vacuum pump 39. For this reason, the discharge device 18 discharges the gas in the closed ring system stably for a long time, and it becomes easy to maintain the reduced pressure state in the closed ring system.

  The control device 40 shown in FIG. 3 monitors the pressure of the fluid in the closed system. In this embodiment, the control device 40 monitors the pressure through the pressure sensor 35 and the network 41 connected to the steam reservoir 47. The control device 40 causes the vacuum pump 39 to discharge gas until the pressure in the vapor reservoir 47 is at least equal to or less than the equilibrium vapor pressure of the extractant at the extraction temperature.

  The control device 40 shown in FIG. 3 monitors the temperature of the fluid in the closed ring system. In this embodiment, the control device 40 monitors the temperature through the temperature sensor 36 and the network 41 connected to the steam reservoir 47.

  In FIG. 3, if the temperature of the fluid is lower than a predetermined extraction temperature, the control device 40 operates the heater 44a. The liquid phase extractant 45 is heated by the heater 44a. The heated extractant 45 becomes high-temperature steam and mixes with the fluid in the vapor reservoir 47. For this reason, the temperature of the fluid rises. The control device 40 causes the heater 44a to perform heating until the temperature of the fluid in the closed ring system rises and at least reaches a predetermined extraction temperature. During this time, the control device 40 stops the operation of the cooler 44b.

  The control device 40 shown in FIG. 3 may monitor the temperature of the liquid phase extractant 45 in the reservoir 46. The control device 40 may perform the control when the heater 44a is heated in consideration of the result of monitoring the temperature of the liquid phase extractant 45.

  In FIG. 3, if the temperature of the fluid is lower than a predetermined extraction temperature, the control device 40 operates the cooler 44b. The liquid phase extractant 45 is cooled by the cooler 44b. Although the cooled extractant 45 continues to evaporate, the extractant 45 becomes a low-temperature vapor and mixes with the fluid in the vapor reservoir 47. For this reason, the temperature of the fluid decreases. The control device 40 causes the cooler 44b to perform cooling until at least a predetermined extraction temperature is reached as the temperature of the fluid in the ring-closing system decreases. During this time, the control device 40 stops the operation of the heater 44a.

  The control device 40 shown in FIG. 3 may monitor the temperature of the liquid phase extractant 45 in the reservoir 46. The control device 40 may perform control when the cooler 44b performs cooling in consideration of the result of monitoring the temperature of the liquid phase extractant 45.

  The heater 44a and the cooler 44b shown in FIG. 3 may be an integrated temperature controller. In the supply device 11, another heater may further heat the gas phase extractant in the vapor reservoir 47. In the supply device 11, another cooler may further cool the gas phase extractant in the vapor reservoir 47.

  As shown in FIG. 3, the path 21 is provided in the upper part of the raw material container 12. A fluid containing steam enters the raw material container 12 through the path 21. The total amount of circulating fluid passes through the raw material container 12. The raw material containers are filled with raw materials 50a to 50c. A tray 51 is provided at the bottom of the raw material container 12. Of the liquid components that have exuded from the raw material, the components that are not mixed with the circulating fluid naturally fall onto the tray 51. The saucer 51 collects components that have dropped naturally.

  As shown in FIG. 3, the path 22 is connected to the lower part of the raw material container 12. The connection part of the route 22 is closer to the tray 51 than the connection part of the route 21. The path 22 passes through the steam reservoir 47 and exits the pot 43. A stopcock 26 </ b> A is provided in the path 22. The stopcock 26A is outside the pot 43. An end portion of the path 22 on the side not connected to the raw material container 12 is defined as an end portion 28A.

  As shown in FIG. 3, the path 25 is connected to the steam reservoir 47. A stopcock 26B is provided in the path 25. The stopcock 26B is outside the pot 43. An end portion of the path 22 on the side not connected to the raw material container 12 is defined as an end portion 28A.

  The extraction unit 27 shown in FIG. 3 includes a distribution device 13, a path 24, and a driven machine 15. The extraction unit 27 includes end portions 29A and 29B. The end portion 29A is located on the distributor 13 side. The end 29B is located on the driven machine 15 side.

  The end 29A shown in FIG. 3 is detachable from the end 28A. When operating the manufacturing apparatus 30, the end portion 29A is attached to the end portion 28A. At this time, the fluid can be guided from the raw material container 12 into the extraction unit 27 by opening the stopcock 26A which has been closed in advance. The end portion 29A is removed from the end portion 28A as necessary. At this time, by closing the stopcock 26A in advance, the fluid in the raw material container 12 can be prevented from leaking from the end portion 28A.

  The end 29B is detachable from the end 28B. When the manufacturing apparatus 30 is operated, the end portion 29B is coupled to the end portion 28B. At this time, the fluid can be guided from the inside of the extraction unit 27 to the vapor reservoir 47 by opening the stopcock 26B which has been closed in advance. The end portion 29B is removed from the end portion 28B as necessary. At this time, by closing the stopcock 26B in advance, the fluid in the vapor reservoir 47 can be prevented from leaking from the end portion 28B.

  The distributor 13 shown in FIG. 3 has a cyclone separator 31. The cyclone separator 31 sorts fluids by density. The cyclone separator 31 separates dense drain from the fluid. The cyclone separator 31 returns the low-density drain 19b and the remainder containing steam to the closed ring system 10.

  Volatile components are contained in the fluid flowing in the closed ring system of the manufacturing apparatus 30 shown in FIG. Such volatile components are derived from the raw materials 50a-c. The distributor 13 further has a condenser 32. The condensing device 32 collects volatile components in the fluid by condensation by cooling the remainder generated by separating dense drainage from the fluid.

[6. Experimental example]

  FIG. 5 shows a manufacturing apparatus 63 used in this experimental example. The manufacturing apparatus 70 has the characteristics of the manufacturing apparatus 30 (FIG. 2) described above. The manufacturing apparatus 70 includes a distribution device 63 instead of the distribution device 13. The distribution device 63 includes a cyclone separator 31, a condensing device 32, and a bubbling device 33. These are arranged in this order from upstream to downstream. It is a part of the closed system of the manufacturing apparatus 70. The aspect of the present embodiment is an exemplification, and the order of each element in the distribution device 63 may be changed. In the drawing, a heater for heating the extractant 45 is not shown.

  As shown in FIG. 5, purified water was poured into the reservoir 46 as the extractant 45. In addition, leaves of Tasmanian blue gum (Eucalyptus globulus) known as so-called eucalyptus were used as raw materials. The extraction temperature was changed in steps of 5 ° C from 45 ° C to 55 ° C.

  As shown in FIG. 5, the fluid was circulated through the cyclone separator 31, the condenser device 32, and the bubbling device 33 in this order. The condenser device 32 is a so-called cooling device. In this experimental example, the condensing device 32 operates at 4 ° C. Purified water is stored in the bubbling device 33 in advance. The fluid is blown out toward the supply device 11 by the driven machine 15. Part of the fluid passes through the raw material container 12. The fluid takes components from the raw material and then goes to the distributor 13 again. Part of the fluid returns as a liquid in the reservoir 46.

  As an actual operation, 10 to 30 g of eucalyptus leaves are first placed in the raw material container 12 as a raw material. In this experimental example, 10 g of raw material was placed. An aroma extract was obtained for each temperature from 45 ° C to 55 ° C. At this time, the temperature was raised stepwise from 45 ° C. → 50 ° C. → 55 ° C. By performing the extraction operation at each temperature for 30 minutes to 1 hour, the extract is collected in a separate collection container for each time zone. In this experimental example, an extraction time of 30 minutes was used in each temperature zone. The extraction itself was performed continuously without a break. Here, the inside of the closed system rises by 5 ° C. every 30 minutes, and keeps the specified temperature for the next 30 minutes.

  In FIG. 5, the extract 1 obtained in the cyclone separator 31 contains the extract 1. The extract 2 obtained by the condenser 32 contains the extract 2. The extract 3 obtained in the bubbling device 33 contains the extract 3.

  Extract 3 was analyzed with a trace aroma component analyzer. The scent component in the extract 3 was adsorbed for 30 minutes to a metal piece called a twister. Gas chromatography (GC) analysis was performed using the twister trapped in this manner as a sample. The purpose of the analysis is to confirm whether the component ratios of the extract 3 obtained in each temperature zone are different from each other by performing continuous extraction while changing the temperature.

  Eucalyptus leaves contain major scent components such as 1,8-cineole (70-90%), limonene (-10%) and α-pinene (10-20%). 1,8-cineole and limonene give off a refreshing fragrance. α-Pinen emits a unique scent similar to that of pine.

  FIG. 6 shows the results of GC analysis in the 45 ° C. temperature zone, FIG. 7 shows the 50 ° C. temperature zone, and FIG. 8 shows the 55 ° C. temperature zone. C1 represents the main scent component of eucalyptus leaves. C1 is a highly aromatic part. C2 represents components other than the main scent component. The composition ratio of the components in the extract 3 gradually changed as the extraction temperature increased by 5 ° C. When the experienced tester confirmed the scent, it was found that each extraction unit 3 emitted a different scent. As the temperature increases, C1 decreases and C2 increases.

  The above experimental results show that the production apparatus used in this experimental example is suitable for continuously and easily obtaining extracts having different scent characteristics.

[7. Comparative Example 1]

  The extraction device 80 shown in FIG. 4 is a non-circulating vacuum steam distillation device. In the extraction device 80, fresh steam is continuously supplied from the production steam supply system 85 to the raw material 50 d in the extraction container 81, for example, coffee beans. The extract in the raw material 50d is extracted with steam under an oxygen-free or low oxygen concentration. Most of the steam is condensed in the condenser 82, so that a large amount of the fraction 88 is obtained in the storage tank 83. The storage tank 83 is depressurized by the vacuum pump 84.

  Patent Document 2 discloses a non-circulating extract extraction device (summary of Patent Document 2). When a large amount of steam is used in such a non-circulating apparatus, the concentration of the raw material-derived component in the fraction may decrease. If the amount of steam is limited, the amount of components extracted from the raw material may decrease.

  In contrast, in the above examples and experimental examples, the vapor is not condensed unless a special operation is performed. Since the steam circulates in the system again, the concentration of the components in the fluid is further increased by the contact of the steam or drain with the raw material again. In the above embodiment, an extraction liquid rich in components can be obtained by carrying out circulation, extraction and separation over a long period of time.

[8. Comparative Example 2]

  Paragraphs [0045]-[0047] of Patent Document 3 show that a liquid contaminant separator including a cyclone separator is used to separate liquid contaminants from steam containing tea aroma components. As a result, liquid contamination in the vapor can be reduced (paragraph [0035]).

  In contrast, in the above examples and experimental examples, a cyclone separator is used to intentionally recover the liquid phase to obtain an extract. Even if the component is not taken into the extract by one cycle, the component circulates in the system again, so that it is not discharged out of the system unless special operation is performed. In the above embodiment, an extraction liquid rich in components can be obtained by carrying out circulation, extraction and separation over a long period of time.

[9. Comparative Example 3]

  FIG. 9 shows a Soxhlet extractor as a comparative example. A Soxhlet extractor is a device for solid-liquid extraction of ingredients from raw materials. When the bottom flask of the Soxhlet extractor is heated, the solvent evaporates (I). The evaporated solvent condenses in the uppermost cooling tube and drops down toward the solid sample (II). Ingredients are dissolved in the increasing solvent (III). Eventually the solvent reaches the height of the side tube (IV). The solvent returns to the flask according to the siphon principle (V). By repeating this cycle, the concentration of the component in the solvent increases.

  As shown in FIG. 9, in the Soxhlet extractor, a large amount of solvent condenses and the siphon is operated by the flow. Therefore, it is necessary to heat a large amount of solvent with a sufficient amount of heat. As a result, heat denaturation of raw materials, components and solvents is likely to occur. In the Soxhlet extractor, the pressure is also increased by the vapor of the solvent, so that the raw material structure itself is destroyed. For this reason, the contamination component in an extract increases.

  On the other hand, in the above embodiment, the flow of condensed liquid is not essential. In the above embodiment, the fluid acting as gas plays the role of extraction. Condensation of the extractant is not essential for fluid circulation or component extraction from raw materials. The extract is collected from the fluid by devices such as cyclone separators, condensers, and bubbling devices. In the above embodiment, heating of the extractant to cause heat denaturation can be avoided. It is also possible to avoid using high-pressure steam that causes tissue destruction. The apparatus of the said Example is suitable for obtaining the extract of the original composition which cannot be obtained unless low temperature extractant vapor | steam is used.

[10. Other uses of manufacturing equipment]

  The other usage of a manufacturing apparatus is demonstrated using FIG. A manufacturing apparatus 60 can be obtained by replacing the extraction unit 27 of the manufacturing apparatus 30 shown in FIG. 3 with an injection unit 57 shown in FIG. The injection unit 57 is also detachable from the end portion 28A and the end portion 28B. By switching and connecting to the injection unit 57 in this way, the manufacturing apparatus 30 can be easily converted to the manufacturing apparatus 60. Or you may enable it to switch an extraction unit and an injection | pouring unit by providing a three-way cock in the end part 28A and the end part 28B.

  An injection unit 57 shown in FIG. 10 includes an injector 53, a path 54, and a driven machine 55. The extraction unit 27 includes end portions 59A and 59B. The end portion 59A is located on the injector 53 side. The end 59B is located on the driven machine 55 side. The driven machine 55 pushes the fluid toward the injector 53.

  The circulation of the fluid in the ring-closed system shown in FIG. 10 is the reverse of the above embodiment. That is, the injectant supplied from the injector goes around the ring-closing system in the order of the path 22, the raw material container 12, the path 21, the vapor reservoir 47, the path 25, the driven machine 55, and the path 54 in order from the injector 53. Return to 53.

  The end portion 59A shown in FIG. 3 is detachable from the end portion 28A. When the manufacturing apparatus 30 is operated, the end portion 59A is attached to the end portion 28A. At this time, the injection agent can be introduced into the raw material container 12 from the injection unit by opening the stopcock 26A which has been closed in advance. The end portion 59A is removed from the end portion 28A as necessary. At this time, by closing the stopcock 26A in advance, the fluid in the raw material container 12 can be prevented from leaking from the end portion 28A.

  The end portion 59B is detachable from the end portion 28B. When the manufacturing apparatus 30 is operated, the end portion 59B is coupled to the end portion 28B. At this time, the fluid can be guided from the vapor reservoir 47 into the injection unit by opening the stopcock 26B which has been closed in advance. The end portion 59B is removed from the end portion 28B as necessary. At this time, by closing the stopcock 26B in advance, the fluid in the vapor reservoir 47 can be prevented from leaking from the end portion 28B.

  The manufacturing apparatus 60 shown in FIG. 10 can be used as follows. It is possible to gradually inject the extractant from the injector 53 to the supply device 11 while processing the raw materials 50a to 50c put in the manufacturing device 60 in the manufacturing device 60. This mode of use is effective when an extraction object such as a plant is selected as the raw materials 50a to 50c. According to this mode of use, an extractant other than the extractant 45 previously placed in the storage unit 46 can be injected into the supply device 11.

  In FIG. 10, the extractant used for the injector 53 may be selected according to the characteristics of the component to be extracted from the raw materials 50a to 50c. In the manufacturing apparatus 60, the extraction temperature and time can also be set freely. For this reason, a very specific extract is obtained. Further, the extractant injected from the injector 53 can be recovered immediately as necessary. Further, components may be continuously extracted from the raw materials 50 a to 50 c while injecting the extractant from the injector 53.

DESCRIPTION OF SYMBOLS 10 Ring closure system, 11 Supply apparatus, 12 Raw material container, 13 Distribution apparatus, 14 Collection container, 15 Driven machine, 17 Supply apparatus, 18 Discharge apparatus, 19a Drain, 19b Drain, 20 Extract liquid, 21 path, 22 path, 23 path , 24 routes, 25 routes, 26A stopcock, 26B stopcock, 27 extraction unit, 28A end, 28B end, 29A end, 29B end, 30 manufacturing equipment, 31 separator, 32 condensing device, 34 compound meter, 35 Pressure sensor, 36 Temperature sensor, 38 Gas-liquid separator, 39 Vacuum pump, 40 Control device, 41 Network, 43 pot, 44a Heater, 44b Cooler, 45 Extractant, 46 Reservoir, 47 Vapor reservoir, 48 Drain 50a raw material, 50b raw material, 50c raw material, 50d raw material, 51 saucer, 53 injector 54 path, 55 driven machine, 57 injection unit, 59A end, 59B end, 60 manufacturing equipment, 80 extraction equipment, 81 extraction container, 82 condenser, 83 storage tank, 84 vacuum pump, 85 steam supply system, 88 distillation Minute, 90 circulation path, 91 generation tank, 92 extraction device, 93 condensing device, 94 storage tank, 95 blower

Claims (4)

(A) a ring-closing system that contains a vapor of the extractant and a drain formed by changing the phase of the vapor into a liquid and can hold a fluid that behaves as a gas;
(B) a driven machine for circulating the fluid in the closed system;
(C) a raw material container provided in the ring-closing system and through which the fluid passes;
(D) a supply device for supplying the steam having an extraction temperature below the normal boiling point of the extractant into the ring-closing system;
(E) a discharge device that discharges at least a gas other than the vapor from within the ring-closing system;
(F) By monitoring the pressure in the closed system, the gas is discharged to the discharge device until at least the pressure in the closed system is equal to or lower than the equilibrium vapor pressure of the extractant at the extraction temperature. A control device,
(G) a distributor having a bubbling device for obtaining an extract from the fluid;
An extract production apparatus comprising: The distribution device separates the high-density drain from the fluid by selecting the fluid according to the density, and returns a device containing the low-density drain and vapor to the closed system. Further provided upstream of the bubbling device,
The manufacturing apparatus according to claim 1. The device for sorting the fluids by density is a cyclone separator;
The manufacturing apparatus according to claim 2. A condensing device for condensing volatile components in the fluid in the closed ring system downstream of the device for selecting the fluid by density and upstream of the bubbling device;
The manufacturing apparatus according to claim 2.

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