JP2021090928A - Extraction method and extraction device - Google Patents

Abstract

To provide an extraction device and an extraction method by which solid constituents can be recovered at normal temperature.SOLUTION: This extraction method has: an atomization process in which a liquefied gas solution, in which solid constituents are solved in a liquefied gas, is irradiated with ultrasonic wave, and the liquefied gas solution is atomized; and a recovery process in which a gas for evaporation is brought into contact with droplets, which are formed by the atomization process, to evaporate the liquefied gas, and solid constituents deposited from the droplets are recovered as fine particles. Further, this extraction device comprises: a container for holding a liquefied gas solution in which solid constituents are solved in a liquefied gas; an ultrasonic vibrator which is provided in the container, and irradiates the liquefied gas solution with ultrasonic wave; a drying container which dries droplets atomized by the ultrasonic vibrator; a gas supply device which supplies a gas for evaporation to the drying container; and a recovery device which recovers solid constituents deposited from the droplets as fine particles.SELECTED DRAWING: Figure 1

Description

The present invention relates to an extraction method and an extraction device for extracting a solid component dissolved in a liquefied gas using a liquefied gas.

Conventionally, as a technique for extracting an active ingredient from a raw material, a technique for forming droplets by ultrasonic waves is known. As an example of using ultrasonic waves, Patent Document 1 discloses an apparatus for forming droplets by ultrasonic waves to obtain metal fine particles. Patent Document 2 discloses an apparatus for extracting an object by atomizing water by ultrasonic waves.

Japanese Unexamined Patent Publication No. 2010-222182 Japanese Unexamined Patent Publication No. 09-248138

Patent Document 1 exemplifies water and alcohol as liquids in which fine particles are dispersed, and discloses that these liquids are vaporized at a high temperature after atomization. Further, Patent Document 2 exemplifies water as a liquid to be atomized, and discloses that after contact with an object, it is heated to 60 ° C. or higher in order to remove water. However, Patent Documents 1 and 2 do not disclose a method for recovering a solid component by a process at room temperature.

Therefore, an object of the present invention is to provide an extraction device and an extraction method capable of recovering a solid component at room temperature.

The present invention is configured as described in the claims of an extraction device and an extraction method in order to solve the above problems.
Specifically, the extraction method of the present invention is, for example, an extraction method for extracting a solid component from a raw material, in which a liquefied gas solution in which a solid component is dissolved in a liquefied gas is irradiated with ultrasonic waves to irradiate the liquefied gas solution. A recovery step of atomizing the liquefied gas by bringing a gas for evaporation into contact with the droplets formed by the atomization step to vaporize the liquefied gas, and recovering the solid component precipitated from the droplets as fine particles. It has a process.
Further, the extraction device of the present invention is, for example, an extraction device for extracting a solid component from a raw material, and is provided in a container for holding a liquefied gas solution in which the solid component is dissolved in a liquefied gas and a container provided in the container for liquefaction. An ultrasonic vibrator that irradiates a gas solution with ultrasonic waves, a drying container that dries droplets atomized by the ultrasonic vibrator, a gas supply device that supplies a gas for evaporation to the drying container, and the above. A recovery device for recovering the solid component precipitated from the droplets as fine particles is provided.

According to the present invention, a solid component can be recovered from a raw material at room temperature or lower.
Issues, configurations and effects other than those described above will be clarified by the description of the following embodiments.

It is a schematic diagram which shows the structure of the solid fine particle manufacturing apparatus which concerns on 1st Embodiment. It is a schematic diagram which shows the structure of the solid fine particle manufacturing apparatus which concerns on 2nd Embodiment.

Hereinafter, embodiments of a solid fine particle manufacturing apparatus and a manufacturing method according to the present invention will be described with reference to the drawings. In the description of the drawings, the same elements are designated by the same reference numerals, and duplicate description thereof will be omitted.

[First Embodiment]
FIG. 1 is a schematic view showing the configuration of the extraction device according to the first embodiment. In the present embodiment, as an extraction device and an extraction method for recovering solid components as fine particles from a raw material using a liquefied gas, fine particles of a solid component containing β cryptoxanthin in Unshuumikan are efficiently used by using a phase change of the liquefied gas. An example of collecting the particles will be described. In the following examples, dimethyl ether (DME) is used as the "liquefied gas" and β cryptoxanthin is used as the "solid component". Here, in the present specification, the liquefied gas is a gas at normal temperature and pressure, and is liquefied by cooling to 20 ° C. or lower under normal pressure.

The solid component is not limited to β cryptoxanthin, and may contain physiologically active substances such as carotenoids, flavonoids, ceramides, and glycosides thereof. Further, it may be a chemical product such as styrene or polyarylate. Furthermore, the technique of the present invention can be applied to pharmaceuticals, cosmetics, health foods, and their raw materials as long as they are solid.

Further, the liquefied gas is not limited to DME, and any gas that liquefies at 20 ° C. or lower may be used. For example, a liquefied gas having a boiling point at atmospheric pressure of −79 ° C. to 20 ° C. can be used. Specific examples thereof include hydrocarbons such as propane, normal butane, isobutane, neopentane and isopentane, and ethers such as dimethyl ether and ethyl methyl ether. Further, the liquefied gas may be a combination of these, and may be any liquefied gas capable of dissolving the target solid.

Further, in the following description, the vaporized DME may be referred to as "vaporized DME" or "DME gas", and the liquefied DME may be referred to as "liquefied DME" according to the description.

The extraction method according to the present embodiment includes an atomization step of irradiating a liquefied gas solution in which a solid component is dissolved in a liquefied gas with ultrasonic waves to atomize the liquefied gas solution, and droplets formed by the atomization step. It has a recovery step of contacting a gas for evaporation to vaporize the liquefied gas and recovering the solid component precipitated from the droplets as fine particles.

As shown in FIG. 1, the extraction device 1 of the present embodiment is a device for recovering fine particles of β cryptoxanthin using, for example, a DME capable of dissolving β cryptoxanthin. The extraction device 1 includes a container 55 that holds a liquefied gas solution in which a solid component is dissolved in a liquefied gas, an ultrasonic vibrator 56 that is provided in the container and irradiates the liquefied gas solution with ultrasonic waves, and an ultrasonic vibrator. It is provided with a drying container 53 for drying the droplets atomized by the above, a gas supply device for supplying a gas for evaporation to the drying container, and a recovery device for recovering the solid component precipitated from the droplets as fine particles. Specifically, a container 55 for storing the DME solution of β cryptoxanthin, a cooler 52 for cooling the container 55, an ultrasonic transducer 56 for generating ultrasonic waves, and a drying container for drying the atomized DME solution. 53, a blower 54 that blows air to supply latent heat to the drying container 53, a blower 57 that sends β cryptoxanthin-containing fine particles and air generated in the drying container 53, and β cryptoxanthin-containing fine particles and air are separated. Cyclone 34 and a recovery container 40 for collecting the separated β cryptoxanthin-containing fine particles are provided.

A DME solution containing β cryptoxanthin is supplied to the container 55 from the outside of the extraction device 1. Latent heat is supplied to the DME solution depending on the room temperature, and only the liquefied DME is vaporized, and the β cryptoxanthin concentration in the DME solution rises. It is connected to the. Since it is sufficient that the cooler can cool the liquefied DME, it is preferable that the cooler is installed in the container 55 or the pipe for supplying the liquefied gas. Here, the cooler 52 is not an essential component, but when the β cryptoxanthin concentration in the DME solution increases, the β cryptoxanthin concentration in the formed droplets increases, and the particle size of the precipitated solid increases. Therefore, when the purpose is to reduce the particle size and make the particle size uniform, it is preferable to cool the particles using the cooler 52 to suppress the vaporization of the DME.

An ultrasonic vibrator 56 is installed at the bottom of the container 55, and when oscillated, the DME solution is atomized, minute droplets are formed, and the droplets rise in the drying container 53. The DME solution, which has become minute droplets, absorbs the heat of the surrounding air and vaporizes, and precipitates as fine particles containing solid β cryptoxanthin. At this time, since the temperature of the ambient air continues to decrease, air is supplied by the blower 54 in order to supplement the heat absorbed. From the viewpoint of suppressing thermal deterioration of β cryptoxanthin, the evaporation gas supplied into the drying container as the evaporation gas is preferably 50 ° C. or lower. Therefore, it is preferable to provide a temperature control device capable of controlling the temperature of the gas for evaporation. In the present embodiment, the blower 54 and the blower 57 are used as the transfer means (gas supply device) in the extraction device 1, but only one of them may be used. Furthermore, although air was described as an example of a gas for drying for the purpose of supplying latent heat, since DME is flammable, it is safe to use a gas that is inert to combustion such as nitrogen, carbon dioxide, and argon. Can be improved.

The precipitated β cryptoxanthin-containing fine particles are discharged from the end of the drying container 53 together with the air containing the vaporized DME, and are supplied to the cyclone (cyclone type separator) 34 by the blower 57. Inside the cyclone 34, gas and β cryptoxanthin fine particles are separated by centrifugal force, the β cryptoxanthin fine particles are collected in the recovery container 40, and air and vaporized DME are discharged to the outside.

It is also possible to supply the gas discharged from the cyclone 34 to the blower 54 to form a circulating closed system (circulate without contacting the outside air). In this case, it is possible to prevent air from being mixed in the fine particle forming path, and it is possible to prevent oxidation and deterioration of the fine particles due to air mixing. At this time, in the circulation path, the temperature drops due to the latent heat of vaporization of the DME, but the drop in temperature can be compensated for by the loss of the blower 54 or the blower 57 and the invading heat from the surrounding environment. Further, if the target temperature cannot be maintained only by these losses, a heater may be used in the circulation path. Further, when the circulation is performed, the amount of DME in the circulation path becomes excessive by the amount vaporized from the minute droplets, so that the pressure in the circulation path can be made constant by flowing the liquid to the outside through the pressure adjusting valve.

In the present embodiment, the cyclone 34 is used for separating the β cryptoxanthin-containing fine particles and the gas, but solid air separation may be performed by another method such as filter filtration. Further, although air or DME gas is used as the gas for drying, the thermal deterioration of β cryptoxanthin can be suppressed by basically keeping the temperature of these gases at room temperature. Further, the drying rate can be increased by raising the temperature of these gases, but by keeping the temperatures of these gases at 50 ° C. or lower, the thermal deterioration of β cryptoxanthin can be suppressed.

Further, according to this embodiment, since the fine droplets are vaporized at room temperature, the temperature difference between the inside and outside of the drying container 53 is low, and therefore the temperature inside the drying container can be easily made uniform. Therefore, since the vaporization time of the fine particles becomes substantially uniform, the residence time in the vaporization step and the size of the drying container can be easily designed, the time required for producing fine particles can be shortened, and the entire apparatus can be miniaturized. Further, the larger the difference between the temperature of the gas introduced from the blower 54 and the boiling point of the liquefied gas, the shorter the vaporization time of the fine droplets can be. Gas may be used.

[Second Embodiment]
FIG. 2 is a schematic view showing the configuration of the extraction device according to the second embodiment. The extraction device 1A according to the present embodiment is similar to the first embodiment in that DME is used as the liquefied gas used for producing β cryptoxanthin fine particles, and is linked with a configuration for producing a DME solution of β cryptoxanthin. However, it is different from the first embodiment.
[Frozen cycle]
In the present embodiment, a heat transfer means using a refrigerant such as chlorofluorocarbon is provided in order to perform the phase change of DME required for extraction. In order to make the flow of chlorofluorocarbons (refrigerant) easier to understand, the flow of chlorofluorocarbons is shown by a broken line in FIG. As shown in FIG. 2, the downstream side of the heat transfer tube in the heat exchanger 4 through which the chlorofluorocarbons flow is connected to the compressor 5, and the chlorofluorocarbons are compressed to a high temperature and high pressure and discharged. The discharged chlorofluorocarbon is cooled by the outside air in the heat exchanger 20 as needed, and is connected to the heat transfer tube in the heat exchanger 3. In the heat exchanger 3, heat is transferred from the high-temperature freon passing through the inside of the heat transfer tube to the liquefied DME existing outside the heat transfer tube, and is used as latent heat to vaporize the DME. The chlorofluorocarbons in the heat transfer tube are liquefied here, but are further depressurized by the expansion valve 6 installed downstream of the chlorofluorocarbons, and become a low-temperature two-phase flow that flows into the heat transfer tube in the original heat exchanger 4. In the heat exchanger 4, the DME existing outside the heat transfer tube is cooled by the freon in the heat transfer tube that has become cold to take away the latent heat, and the DME is liquefied. At this time, chlorofluorocarbons vaporize and return to the downstream compressor 5, so that the overall flow constitutes a refrigeration cycle.

Further, in this embodiment, chlorofluorocarbons have been described as an example of the refrigerant, but chlorofluorocarbons do not necessarily have to be used, and any substance such as isobutane that can form a refrigeration cycle may be used.

[Extraction process]
The extraction device 1A according to the present embodiment includes a treatment tank 2 that dissolves a solid component in the liquefied gas by bringing the liquefied gas into contact with an organism. The treatment tank 2 is filled with Satsuma mandarin, which is a raw material containing β cryptoxanthin, or a squeezed residue of Satsuma mandarin. The liquefied DME is injected into the treatment tank 2 by the pump 10, dissolves β cryptoxanthin in the raw material, becomes a DME solution containing β cryptoxanthin, and is sent to the heat exchanger 3. In the heat exchanger 3, only the liquefied DME is vaporized to become DME gas and sent to the heat exchanger 4. In the heat exchanger 4, the latent heat of condensation is deprived, the DME gas becomes liquefied DME, and the liquid is sent by the pump 10, and the extraction cycle of liquefied DME is configured as an overall flow. When the operation of the extraction cycle is continued, the β cryptoxanthin concentration in the treatment tank 2 decreases, and the β cryptoxanthin concentration in the heat exchanger 3 increases. After reaching the desired concentration, the extraction cycle is stopped.

[Process of micronization]
When the valve 31 is opened, the high concentration β cryptoxanthin DME solution is cooled to the boiling point of DME at substantially atmospheric pressure by the first cooler 51 and injected into the container 55.

A cooler 52 for cooling below the boiling point of the DME is connected to the container 55 in order to prevent vaporization of the DME. An ultrasonic vibrator 56 is installed at the bottom of the container 55, and when oscillated, the DME solution is atomized, minute droplets are formed, and the droplets rise in the drying container 53. The DME solution, which has become minute droplets, absorbs the heat of the surrounding DME gas and vaporizes, and precipitates as solid fine particles containing β cryptoxanthin. At this time, since the temperature of the surrounding DME gas continues to decrease, DME gas at substantially room temperature, which will be described later, is supplied through the valve 36 in order to supplement the endothermic heat. The precipitated β cryptoxanthin fine particles are discharged together with the DME gas from the end of the drying container 53, and are supplied to the cyclone 34 by the blower 57. Inside the cyclone 34, DME gas and β cryptoxanthin-containing fine particles are separated by centrifugal force, and the β cryptoxanthin-containing fine particles are recovered in the recovery container 40, and the DME gas is supplied to the second compressor 35. The DME gas is compressed to high temperature and high pressure by the second compressor 35 and sent to the cooler 30. In the cooler 30, the DME gas is cooled by a fan as needed, and an excess amount of the liquefied DME as a vaporizing gas is liquefied. The amount liquefied here is the amount in which the droplets generated by atomization are phase-changed into DME gas. The supply amount of the liquefied DME liquefied by the cooler 30 is adjusted by the valve 37, merges with the other liquefied DME by the pump 10, and is used again in the extraction step. On the other hand, the DME gas that remains in a gaseous state without being liquefied by the cooler 30 is supplied to the drying container 53 while the supply amount is adjusted by the valve 36, and serves as a latent heat source for the liquefied DME that constitutes fine droplets. It will be used.

Further, although the cooler 51 and the cooler 52 are shown as coolers for cooling the liquefied gas, only one of them may be provided because the purpose is to prevent the vaporization of the liquefied gas in the container 55. .. Further, when the valve 31 is opened, the DME in which β cryptoxanthin is dissolved flows into the container 55, and the operation at this time may be continuous or intermittent.

Further, although the inside of the drying container 53 has been described as being substantially atmospheric pressure, the process of producing fine particles can also be carried out in a pressure system by using a pressure resistant container and a pressure resistant pipe as the circulation path of the DME gas including the drying container 53 and the container 55. it can. When a pressurized system is used, the compression rate in the compressor 35 is reduced, so that the running cost required for producing fine particles can be reduced. Further, in this case, if the pressure in the pressurizing system is lower than the saturated vapor pressure of the DME at room temperature, fine particles can be produced.

In this example, the production of β cryptoxanthin-containing fine particles has been described using Satsuma mandarin as a raw material as an example, but it can be applied to other than citrus fruits, and fine particles of the target component can be produced from other plants, animals, and microorganisms. ..

Although the embodiments of the present invention have been described in detail above, the present invention is not limited to the above-described embodiments, and various designs are designed without departing from the spirit of the present invention described in the claims. You can make changes.

1, 1A Extractor 2 Processing tank 3, 4 Heat exchanger 5 Compressor 6 Expansion valve 10 Pump 30 Cooler 34 Cyclone 51, 52 Cooler 53 Drying container 55 Container 56 Ultrasonic transducer

Claims (20)

It is an extraction method that extracts solid components from raw materials.
An atomization step of irradiating a liquefied gas solution in which a solid component is dissolved in a liquefied gas with ultrasonic waves to atomize the liquefied gas solution.
An extraction method comprising a recovery step of bringing a gas for evaporation into contact with the droplets formed by the atomization step to vaporize the liquefied gas and recovering the solid component precipitated from the droplets as fine particles. The extraction method according to claim 1.
An extraction method characterized in that, in the recovery step, a gas for evaporation at 50 ° C. or lower is brought into contact with the droplets. The extraction method according to claim 1.
An extraction method characterized by recovering the fine particles with a cyclone in the recovery step. The extraction method according to claim 1.
An extraction method comprising cooling the liquefied gas solution in the atomization step. The extraction method according to claim 1.
An extraction method characterized in that, in the recovery step, the gas for evaporation is supplied to a space in which the droplets are present by using a blower. The extraction method according to claim 3.
An extraction method characterized in that the exhaust gas discharged from the cyclone is compressed by using a compressor and used as a gas for evaporation at 50 ° C. or lower for supplying latent heat of the droplets. The extraction method according to claim 1.
An extraction method characterized by circulating the liquefied gas without contacting the outside air. The extraction method according to claim 1.
An extraction method characterized in that the boiling point of the liquefied gas at atmospheric pressure is −79 ° C. to 20 ° C. The extraction method according to claim 8.
The extraction method, wherein the liquefied gas contains any one of propane, normal butane, isobutane, neopentane, isopentane, dimethyl ether, and ethyl methyl ether. The extraction method according to any one of claims 1 to 9.
The extraction method, wherein the liquefied gas solution is an extraction solution from which a target solid component is extracted by bringing the liquefied gas into contact with an organism. An extraction device that extracts solid components from raw materials.
A container that holds a liquefied gas solution in which solid components are dissolved in liquefied gas,
An ultrasonic vibrator provided in the container and irradiating the liquefied gas solution with ultrasonic waves,
A drying container for drying the droplets atomized by the ultrasonic vibrator, and
A gas supply device that supplies a gas for evaporation to the drying container,
An extraction device including a recovery device for recovering solid components precipitated from the droplets as fine particles. The extraction device according to claim 11.
An extraction device further comprising a temperature control device for adjusting the temperature of the gas for evaporation to 50 ° C. or lower. The extraction device according to claim 11.
The recovery device is an extraction device characterized by being a cyclone type separator. The extraction device according to claim 11.
An extraction device, wherein the container or a pipe for supplying the liquefied gas includes a cooler for cooling the liquefied gas. The extraction device according to claim 11.
The gas supply device is an extraction device including a blower for supplying the gas for evaporation. The extraction device according to claim 13.
An extraction device including a compressor that compresses the exhaust gas discharged from the cyclone type separator as a gas having a temperature of 50 ° C. or lower. The extraction device according to claim 11.
An extraction device characterized in that the liquefied gas or the vaporized gas circulates without coming into contact with the outside air. The extraction device according to claim 11.
An extraction device characterized by using a liquefied gas having a boiling point at atmospheric pressure of −79 ° C. to 20 ° C. as the liquefied gas. The extraction device according to claim 18.
An extraction device, wherein the liquefied gas contains any one of propane, normal butane, isobutane, neopentane, isopentane, dimethyl ether, and ethyl methyl ether. The extraction device according to claim 11.
An extraction device comprising a treatment tank for dissolving a target solid component in the liquefied gas by bringing the liquefied gas into contact with an organism.

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