KR20240000799A - apparatus for extracting effective ingredient using carbon dioxide - Google Patents

Abstract

The present invention is intended to provide an extraction device that can extract active ingredients very efficiently in a relatively short time by placing a stirrer and pulse electric field processing devices inside a reactor main body that extracts active ingredients from raw materials using carbon dioxide. In the active ingredient extraction device using carbon dioxide for extracting the active ingredient from the raw material by inserting liquid carbon dioxide, a reactor main body providing an internal space for extracting the active ingredient from the raw material by introducing the raw material and the liquid carbon dioxide and a stirrer that extends along the center of the inner space of the reactor body and includes a stirrer shaft rotatably supported on the reactor body and a stirring blade provided on the stirrer shaft, and an insulator provided on the inner peripheral surface of the reactor body. It is characterized by comprising a first electrode for pulse electric field processing and a second electrode for pulse electric field processing that are separately arranged.

Description

Apparatus for extracting effective ingredient using carbon dioxide}

The present invention relates to an extraction device that extracts active ingredients from raw materials using carbon dioxide.

As the aging society and the increase in chronic diseases require increased prevention and safety of medicinal products, medicinal plants have expanded from being used through simple processing to being used as materials for pharmaceuticals, health functional foods, cosmetics, etc. through extraction of pharmacological ingredients and ingredient research. Utilization is increasing.

In particular, in Korea, various medicinal plants exhibit unique pharmacological effects depending on various climates and soil conditions, and research and standardization studies on new effects are being conducted, and various medicinal products are being studied using these.

In particular, many studies are being conducted to identify new efficacy using new native plants, and research is being actively conducted to identify and utilize the effective ingredients of these medicinal plants, whether by using native plants alone or composite materials. .

As the industrialization of medicines and health functional foods made from natural ingredients using medicinal plants accelerates, the global health food market increases from $233.94 billion in 2016 to an average annual growth rate of 6.03%, reaching $313.56 billion in 2021. It is expected that this will happen, and approximately 50% of domestic and foreign pharmaceuticals in functional foods are reported to be single substances derived from natural products.

Domestic medicinal plants are being actively studied based on long-standing experience in use. Due to the diversity of climate and terrain, there are 8,458 species of native plants and 438 species of exotic plants, and 1,253 species of plants that can be used as medicinal resources include 826 species for medicinal purposes and 826 species for food. A total of 2,104 species are known to be growing naturally, and all chemicals naturally produced by these plants are major components of natural products. These organic compounds are collectively referred to as phytochemicals, and plants contain a wide variety of chemicals. Secondary metabolites are abundant, and can be classified into carotenoids, phenols, alkaloids, nitrogen-containing compounds, and organosulfur compounds based on their biosynthetic origin.

In the conventional method of extracting active ingredients, the dried raw materials are first pulverized and immersed in a solvent, causing expansion and hydration, and then the soluble components in the raw materials move to the solvent by diffusion and osmotic pressure, that is, the soluble components contained in the plant cell structure are extracted. A mass transfer phenomenon occurs in which components move into the solvent and eventually maintain equilibrium, which is called extraction.

Active ingredients, secondary metabolites, or bioactive ingredients are synthesized in the cytoplasm and ultimately stored in an insoluble structure surrounded by the vacuole or lipoprotein bilayer of plant cells. It is not easy to extract because it is contained. Therefore, in order to increase the extraction yield of a certain ingredient from a herbal medicine, it is important to increase the mass transfer rate of that ingredient. As the mass transfer rate increases, cell permeability and diffusion of secondary metabolites increase, and this mass transfer can be improved by changes in the concentration of components, heating or high pressure, ultrasound, and pulsed magnetic fields.

Meanwhile, supercritical fluid extraction technology is a technology that uses fluids above critical temperature and pressure, and can replace existing processes in extraction and purification-related fields such as pharmaceuticals, food processing, and petrochemical refining. It is attracting attention as a new environmentally friendly clean technology.

In particular, for the past 30 years, developed countries have been using traditional processes to produce gases or liquids due to the rising price of energy resources, the environmental damage caused by traditional separation processes, and the growing demand for special-purpose new materials that cannot be manufactured through gas or liquid processes. Breaking away from the concept of using supercritical fluid technology, we have been focusing on the development of new process fluid technology that uses supercritical fluid technology as the process fluid. As a result, technology using supercritical fluid as a process fluid is rapidly spreading across various industries such as fine chemistry, energy, environment, and new materials, replacing various traditional separation technologies with new technologies using supercritical fluid processes.

In the early days, supercritical fluid technology was mainly applied to natural product extraction and purification, which was limited to non-polar substances such as spices, cosmetics, fats, etc., and low-cost food or flavoring ingredients, but recently, with the development of various phenomenological characteristics and additional technologies related to this technology, It has been applied to extract and purify polar, small, and expensive natural medicines.

There are many different types of supercritical fluid candidates, of which carbon dioxide is the most widely used. Carbon dioxide not only exists in infinite quantities in nature, but is also a substance that is generated in large quantities in the steel industry and petrochemical industry. In addition, carbon dioxide is colorless, odorless, harmless to the human body, and is also a very chemically stable substance. In addition, carbon dioxide has a lower critical temperature (31.1°C) and critical pressure (7.38 MPa) than any other fluid, so it can be easily adjusted to supercritical conditions, which has great advantages in terms of efficient energy use as well as environmental friendliness.

Moreover, when this technology is applied in the field of separation and purification of natural biologically active substances, it addresses the problems that arise in existing processes, namely, human toxicity due to organic solvents remaining in the final product, high cost, environmental pollution due to waste solvents, and loss of target ingredients. Denaturation and low extraction selectivity can be solved or supplemented to a large extent.

However, the commercially used conventional supercritical fluid extraction technique using carbon dioxide requires very high pressure extraction conditions or must be maintained at ultra-high pressure for a long period of time, so it cannot withstand the excessive energy and ultra-high pressure required to boost the ultra-high pressure. It has the disadvantage of requiring a high cost, such as a reactor, and that the extraction process takes a long time because an ultra-high pressure environment must be maintained for a long time.

For example, Republic of Korea Patent Publication No. 10-2014-0088982, “Method for producing perilla extract using supercritical carbon dioxide extraction method” (published on July 14, 2014) uses supercritical carbon dioxide as a solvent in perilla powder and extracts perilla extract at a temperature of 30 to 70°C. It is described that the extraction is performed at a temperature of 100 to 300 bar (about 10 to 30 MPa) and a pressure of 233 bar (preferably 233 bar) for 2 to 3 hours.

Republic of Korea Patent Registration No. 10-0849156, “Lycopene Extraction Using Supercritical Carbon Dioxide” (registered on July 23, 2008), freeze-dried or undried watermelon cake was extracted at 6000~9000 psi (about 41~62 MPa) and A method for producing a lycopene-enriched extract using supercritical carbon dioxide under conditions of 40 to 70°C is described.

This conventional extraction technique using supercritical carbon dioxide has the technical prerequisite that carbon dioxide must be boosted to ultra-high pressure and maintained at ultra-high pressure for a long time in that extraction proceeds only depending on the pressure of carbon dioxide.

Meanwhile, apart from supercritical fluid extraction technology, pulse electric field processing technology is developing independently.

Pulsed Electric Field (PEF)

The innovative potential in the field of PEF is the widespread implementation of this technology for the processing of pumpable fresh food products.

While traditional heat sterilization destroys health-promoting ingredients such as vitamins and causes loss of fresh taste, PEF allows heat-sensitive products such as juices and smoothies, where fresh taste is a key quality parameter, to be preserved for long periods of time without detrimental effects on quality. can do. PEF processing technology can be easily implemented into existing production lines with continuous operation and simple equipment design with various capacity options.

For PEF treatment, micro high-voltage pulses of approximately 10 to 60 kV are applied. The applied high-voltage pulse induces micropores in the cell membrane (and cell wall), causing loss of barrier function, leakage of intracellular contents, and loss of vitality.

Liquid or semi-viscous liquids that can be pumped through a PEF treatment device or solid products that must be transported are exposed to high voltage pulses. The required processing time is less than 1 second and pulses are applied at a repetition rate of up to 500 or more times per second to sufficiently process all volume elements. In addition to electrical parameters such as electric field strength and specific energy input, product temperature and product recipe also affect processing intensity.

electroporation

PEF treatment is an effective process for preserving liquid products in the food and biotechnology fields at low temperatures by causing electroporation of biological or microbial cell membranes (and cell walls).

Similar or improved levels of microbial inactivation compared to thermal processes may contribute to increased retention of heat labile components.

However, continuous PEF processing in particular can lead to non-uniform processing conditions, and since PEF is generally highest on the inner wall of the chamber where the flow rate of the product being processed is lowest, the non-uniformity of PEF within the processing chamber and the associated non-uniform temperature conditions. appears.

For this reason, PEF processing chambers should be designed to increase processing homogeneity by achieving more homogeneous flow characteristics and reducing local temperature peaks within the processing chamber.

loss of cell membrane function

The cytoplasm is surrounded by a thin semipermeable membrane, the cell membrane, which serves as a semipermeable barrier for intracellular and extracellular transport of ions and macromolecules. This cell membrane is a phospholipid bilayer with a thickness of 5 nanometers (nm). When a cell is exposed to PEF, small holes of 50 to 100 nanometers (nm) are created in the cell membrane, which is called electroporation. , which is the loss of the cell membrane barrier function that allows access to the cell's valuable contents. This electroporation occurs in 1 microsecond (μs), and the process is fast, flexible, energy efficient, and requires minimal heat, so products processed this way can be stored longer while maintaining better nutritional value than conventional food processing techniques. There will be a period.

Cell sizes can be 20 to 100 micrometers (μm), bacterial dimensions can be 2 to 10 micrometers (μm), and pores can each be 50 to 100 nanometers (nm) in size.

These small pores (perforations) become more stable irreversible pores when the cell membrane receives more pulses. The required processing time for pulses is less than 1 second, up to 500 pulses per second (pulse repetition rate of up to 500 Hz) to sufficiently process all volume components.

Loss of cell membrane barrier function results in the disappearance of microorganisms, but despite this perforating effect on cell membranes, PEF treatment has no effect on vitamins, flavors or proteins, maintaining the organoleptic quality and functional value of heat-sensitive liquids. Enables decontamination.

Membrane disruption occurs when the induced membrane potential exceeds a threshold of 1 V in many cellular systems, corresponding to an external electric field of approximately 10 kV/cm for E. coli. A threshold of at least about 10 kV/cm is required to kill E. coli and reduce the microbial load of a liquid, and electroporation becomes irreversible above the minimum threshold (1 V).

It is known that the factor most closely related to treatment efficiency in PEF technology is the strength of the electric field. Here, the intensity of the electric field varies depending on the voltage and electrode spacing, as shown in the following equation (1).

E = V/d -------------Equation (1)

E: electric fields (V/cm)

V : applied voltage (V)

d : electrode gap distance (cm)

Looking at the relationship between voltage (V) and electrode spacing (d), it was confirmed that the magnitude of the externally applied voltage (V) has a greater effect than the spacing (d) between electrodes.

In other words, it was confirmed that increasing the intensity of the electric field by increasing the applied voltage or reducing the electrode gap was more effective in increasing extraction efficiency.

PEF, or electroporation, is a processor that punctures cell membranes regardless of cell size. It dramatically increases production, preserves pigments, antioxidants, and vitamins, and makes products fresh and healthy for a long time. It can also be applied at relatively low temperatures for pasteurization of food with minimal impact on freshness characteristics such as color, taste and nutrients of the food, and the process itself has limited effect on the deactivation of enzymes.

Republic of Korea Patent Publication No. 10-2014-0088982 “Method for producing perilla extract using supercritical carbon dioxide extraction method” (published on July 14, 2014) Republic of Korea Patent Registration No. 10-0849156 “Lycopene extraction using supercritical carbon dioxide” (registered on July 23, 2008)

The present invention was developed to solve the problems of the prior art as described above, and is very effective in a relatively short time by placing a stirrer and pulse electric field processing devices inside the reactor body that extracts active ingredients from raw materials using carbon dioxide. We would like to propose an extraction device that can extract ingredients.

In order to solve the above problem, the present invention provides an active ingredient extraction device using carbon dioxide for extracting an active ingredient from the raw material by inputting the raw material and liquid carbon dioxide. A stirrer comprising a reactor body providing an internal space for extracting components, a stirrer shaft extending along the center of the inner space of the reactor body and rotatably supported on the reactor body, and a stirring blade provided on the stirrer shaft. and a first electrode for pulse electric field treatment and a second electrode for pulse electric field treatment arranged to be separated from each other by an insulator provided on the inner peripheral surface of the reactor main body.

In the above, it is preferable that a heater provided at the bottom of the reactor body to induce boiling of the liquid carbon dioxide and a cooler provided at the top of the reactor body to induce condensation of the boiled carbon dioxide are further provided.

In the above, the reactor main body includes a cylindrical body in the form of a vertical cylinder, and both the first electrode for pulse electric field treatment and the second electrode for pulse electric field treatment have a cylindrical shape with the top and bottom open, and the pulse electric field treatment It is preferable that the first electrode for processing the pulse electric field and the second electrode for processing the pulse electric field are alternately arranged in the vertical direction along the center of the internal space of the reactor main body.

In the above, a stirrer head for connection to external power may be formed at the upper end of the stirrer shaft.

In the above, a filter support plate is provided at the lower part of the internal space of the reactor main body, having a bearing seating groove with an open top, and a plurality of through holes extending in the vertical direction and arranged in a form surrounding the bearing seating groove. , a first bearing rotatably supporting the lower end of the agitator shaft is inserted into the bearing seating groove, and a filter having a shaft through hole formed in the center for the agitator shaft to pass through is preferably provided on an upper part of the filter support plate. do.

In the above, the reactor body includes a cylindrical body in the form of a vertical cylinder, an upper cover that closes the open upper part of the cylindrical body and has a material inlet and a carbon dioxide inlet, and closes the open lower part of the cylindrical body. For this purpose, it is preferable to include a lower cover that is detachably coupled to the cylindrical body and has an outlet port.

As described above, the present invention provides an extraction device that can extract active ingredients very efficiently in a relatively short time by placing a stirrer and pulse electric field treatment devices inside the reactor main body for extracting active ingredients from raw materials using carbon dioxide. .

1 is a schematic diagram of an active ingredient extraction system using carbon dioxide to which an active ingredient extraction device using carbon dioxide according to an embodiment of the present invention is applied;
Figure 2 is a separate view showing only the active ingredient extraction device using carbon dioxide of Figure 1;
Figure 3 is an exploded cross-sectional view of Figure 2;
Figure 4 is a perspective view of the first electrode for pulse electric field processing and the second electrode for pulse electric field processing of Figure 3;
Figure 5 is a diagram conceptually showing the state of pulse electric field processing in Figure 2;
Figure 6 is a plan view of the filter support plate in a state in which the first bearing of Figure 2 is seated.

Below, with reference to the attached drawings, embodiments of the present invention will be described in detail so that those skilled in the art can easily implement the present invention. However, the present invention may be implemented in many different forms and is not limited to the embodiments described herein. In order to clearly explain the present invention in the drawings, parts that are not related to the description are omitted, and similar parts are given similar reference numerals throughout the specification.

Throughout the specification, when a part is said to “include” a certain element, this means that it may further include other elements rather than excluding other elements, unless specifically stated to the contrary.

Figure 1 is a schematic diagram of an active ingredient extraction system using carbon dioxide to which an active ingredient extraction device using carbon dioxide according to an embodiment of the present invention is applied, and Figure 2 is a separate diagram showing only the active ingredient extraction device using carbon dioxide of Figure 1. , FIG. 3 is an isolated cross-sectional view of FIG. 2, FIG. 4 is a perspective view of the first electrode for pulse electric field processing and the second electrode for pulse electric field processing in FIG. 3, and FIG. 5 conceptually shows the state of pulse electric field processing in FIG. 2. It is a drawing, and FIG. 6 is a plan view of the filter support plate in a state in which the first bearing of FIG. 2 is seated.

First, a carbon dioxide storage unit 10 is provided for this extraction device 100.

The carbon dioxide storage unit 10 is used to supply liquid carbon dioxide and gaseous carbon dioxide to the extraction device 100.

Liquid carbon dioxide and gaseous carbon dioxide of 7.4 MPa are stored in the carbon dioxide storage unit 10, and 7.4 MPa of liquid carbon dioxide and gaseous carbon dioxide can be continuously provided to the extraction device 100.

Liquid carbon dioxide stored in the carbon dioxide storage unit 10 is supplied to the main extraction device 100 through the liquid carbon dioxide supply pipe 11, and gaseous carbon dioxide stored in the carbon dioxide storage unit 10 is main extracted through the gaseous carbon dioxide supply pipe 12. is supplied to the device 100.

The gaseous carbon dioxide used in this extraction device 100 (including the gaseous carbon dioxide generated after the liquid carbon dioxide discharged from the carbon dioxide storage unit 10 is used) has a small amount of use and can be purged into the atmosphere without a separate recovery device. .

The present extraction device 100 will be described.

This embodiment consists of a reactor main body 110, a heater 120, a cooler 130, first and second electrodes 141 and 142 for pulse electric field treatment, and a stirrer 150.

In this embodiment, the raw materials to be extracted are preferably fresh animal and plant raw materials, and fresh plant raw materials are presented as a specific example, but are not limited thereto.

The reactor body 110 provides an internal space for extracting active ingredients from raw materials.

The reactor main body 110 of this embodiment includes a cylindrical body 113 in the form of a vertical cylinder with the top and bottom open, a lower cover 114 that closes the open lower part of the cylindrical body 113, and a cylinder. It includes an upper cover 115 that closes the open upper part of the mold body 113.

Since the reactor body 110 operates at a pressure of approximately 7.4 MPa or more, it is desirable to make the diameter of the cylindrical body 113 as small as possible for economical and safe operation.

In this embodiment, the upper cover 115 covers the open upper part of the cylindrical body 113 and has a structure integrated with the cylindrical body 113.

A through hole 115a for shaft coupling is formed in the center of the upper cover 115, and a material inlet 115b and a carbon dioxide inlet 115c are formed around the through hole 115a for shaft coupling.

The through hole 115a for shaft coupling consists of a small diameter second bearing seating hole 115a-1 at the bottom and a large diameter cap mounting female screw hole 115a-2 at the top.

The second bearing (115d) is seated in the second bearing seating hole (115a-1).

The second bearing 115d rotatably supports the upper end of the agitator shaft 151, which will be described later, and the agitator head 151a protrudes from the top.

The male thread portion 115e-1 of the stirrer head cap 115e is screwed into the female thread hole 115a-2 for mounting the cap.

The stirrer head cap 115e is detachably coupled to the cap mounting female screw hole 115a-2 to cover or expose the stirrer head 151a to the outside.

A gasket 115f is inserted into the lower part of the cap 115e to enable airtightness between the cap 115e and the upper cover 115.

Animal and plant raw materials can be introduced into the internal space of the reactor main body 110 through the material inlet 115b, and an inlet lid 115b-1 is coupled to the material inlet 115b to close the material inlet 115b. .

Liquid carbon dioxide or gaseous carbon dioxide can be injected into the reactor main body 110 through the carbon dioxide inlet 115c.

That is, the carbon dioxide inlet 115c is connected to both the liquid carbon dioxide supply pipe 11 and the gaseous carbon dioxide supply pipe 12, and liquid carbon dioxide or gaseous carbon dioxide can be injected into the internal space of the reactor main body 110 through any one of them. .

The lower cover 114 is for covering the open lower part of the cylindrical body 113 and is detachably coupled to the cylindrical body 113.

That is, the cylindrical body 113 and the lower cover 114 are flanged to each other by bolts after a gasket is inserted therebetween.

A disk-shaped filter support plate 116 is mounted on the upper part of the lower cover 114.

A bearing seating groove 116a with an open top is formed in the center of the filter support plate 116, and a plurality of through holes 116b extending in the vertical direction are formed to surround the bearing seating groove 116a. .

The first bearing 116c is inserted and seated in the bearing seating groove 116a.

The first bearing 116c is for rotatably supporting the lower end of the stirrer shaft 151.

In order to stably support the filter support plate 116, a plurality of supports 114a are provided on the lower cover 114.

A filter 117 is mounted on the upper surface of the filter support plate 116.

The filter 117 is provided to pass through a solution in which the active ingredient is dissolved (liquid carbon dioxide from which the active ingredient has been extracted) from the extracted mixed raw material (raw material and liquid carbon dioxide) and filter out the residue. Residue and filter 117 can be removed by separating lower cover 114 from cylindrical body 113.

A shaft penetration hole 117a is formed in the center of the filter 117 through which the stirrer shaft 151 passes.

The lower cover 114 is provided with an outlet port 114b through which the solution in which the extracted active ingredient is dissolved is discharged.

The outlet port 114b is provided with an outlet opening/closing valve 114b-1.

The essential oil recovery unit 20 is connected to the outlet port 114b.

A heater 120 is attached to the lower outer peripheral surface of the cylindrical body 113, and a cooler 130 is attached to the upper outer peripheral surface of the cylindrical body 113.

The heater 120 is used to heat carbon dioxide to induce boiling of liquid carbon dioxide, and is preferably equipped with a thermometer and automatically controlled.

The cooler 130 is used to cool carbon dioxide and induce condensation of boiling carbon dioxide, and is preferably equipped with a thermometer and automatically controlled.

The cooler 130 is a pad-type cooler that absorbs ambient heat through evaporation of liquid carbon dioxide.

Accordingly, a liquid carbon dioxide supply pipe 131 and a gaseous carbon dioxide discharge pipe 132 are respectively connected to the cooler 130.

The liquid carbon dioxide supply pipe 131 is a pipe branching from the liquid carbon dioxide supply pipe 11 of the carbon dioxide storage unit 10, and is provided with a control valve 131a (solenoid valve) and an expansion valve 131b.

Therefore, the liquid carbon dioxide supplied through the liquid carbon dioxide supply pipe 131 expands while passing through the expansion valve 131b and changes into a state in which it is easy to evaporate, and as it evaporates in the cooler 130, the surrounding heat (specifically, the reactor main body 110) It absorbs the heat of condensation of gaseous carbon dioxide at the top of the gaseous carbon dioxide and is then discharged to the outside (specifically, into the atmosphere) through the gaseous carbon dioxide discharge pipe 132.

By using liquid carbon dioxide, the cooler 130 can simplify the overall extraction system by using the same raw material as the carbon dioxide of the mixed raw material.

Meanwhile, depending on the embodiment, a separate refrigerator may be provided to supply cold heat to the cooler 130, and the refrigerator may recover gaseous carbon dioxide and supply liquid carbon dioxide through compression and condensation processes. Since the cooling process of a refrigerator is a generally well-known technology, detailed explanation is omitted here.

An insulator 143 is provided in a form that covers the inner peripheral surface of the reactor main body 110, specifically the inner peripheral surface of the cylindrical body 113, and a first electrode for pulse electric field treatment ( 141) and a second electrode 142 for pulse electric field processing are provided.

In this embodiment, a plurality of first electrodes 141 for pulse electric field processing and second electrodes 142 for pulse electric field processing are provided, and each first electrode 141 for pulse electric field processing and a plurality of second electrodes 142 for pulse electric field processing are provided. The second electrode 142 is formed in a cylindrical shape with both top and bottom open, as shown in FIG. 4 .

The first electrode 141 for pulse electric field processing and the second electrode 142 for pulse electric field processing are part of the pulse electric field processing device.

That is, a pulse generator (not shown) capable of generating a predetermined pulse is further connected to each of the first electrode 141 for pulse electric field processing and the second electrode 142 for pulse electric field processing. This constitutes a pulse electric field processing device.

Figure 5 shows the wiring state of the first electrode 141 for processing a plurality of pulse electric fields and the second electrode 142 for processing a plurality of pulse electric fields, and also shows the wiring state of the first electrode 141 for processing a pulse electric field and the second electrode 142 for processing a pulse electric field. This conceptually illustrates the pulse electric field generated from the second electrode 142 for processing.

By operating the pulse generator, a PEF of about 10 to 60 kV/cm, preferably 25 to 50 kV/cm, is generated between the first electrode 141 for pulse electric field processing and the second electrode 142 for pulse electric field processing. .

In this embodiment, as shown in FIG. 5, a first electrode 141 for pulse electric field processing and a second electrode for pulse electric field processing are installed along the center of the internal space of the cylindrical body 113 (that is, along the vertical direction). 142) are alternately inserted into the surface of the insulator 143, so a relatively very large PEF effective treatment area (surface area of the electrode) can be secured, thereby increasing PEF treatment efficiency.

A stirrer 150 is provided inside the reactor body 110.

In this embodiment, the stirrer 150 consists of a stirrer shaft 151 and a stirring blade 152.

In this embodiment, the stirrer 150 is driven by connecting external power, but the present invention is not limited to this, and the stirrer may be equipped with a motor for rotating the stirrer shaft 151.

The stirrer shaft 151 extends along the inner center of the reactor body 110 and is rotatably supported on the reactor body 110.

That is, the stirrer shaft 151 is rotatably supported by the first bearing 116c and the second bearing 115e.

A stirrer head 151a in the form of a hexagonal column is formed at the top of the stirrer shaft 151.

An external power source (tabletop drill machine, hand drill, etc.) can be connected to the stirrer head 151a to rotate the stirrer shaft 151.

The stirrer head 151a can be transformed into various shapes such as a square column and a pentagonal column in addition to a hexagonal column.

A stirring blade 152 is provided on the stirrer shaft 151.

The unexplained symbol 30 is a control unit.

The operation of this embodiment will be described.

(1) Raw material input step

Fresh biological raw materials (eg, animal and plant raw materials) are introduced into the internal space of the reactor main body 110 through the material inlet 115b.

In this way, when fresh biological raw materials, preferably fresh plant raw materials, are directly added, it is possible to prevent the volatile aroma substances, that is, essential oils, of the fresh plant raw materials from being lost.

Fresh here means that it has not been dried. If the dried raw materials are ground in a conventional grinder, most of the essential oil will be lost to the atmosphere and the volatile aroma substances will not be recoverable.

Therefore, the quality and quantity of the extracted active ingredients can be increased by introducing fresh raw materials into the reactor main body 110 and immediately pulverizing them.

After the input of the raw materials is completed, the inlet lid 115b-1 of the material inlet 115b is closed to seal the reactor main body 110.

(2) Raw material grinding step

After the raw material input step, the stirrer head cap 115e is opened and external power is connected to the stirrer head 151a to rotate the stirrer shaft 151, thereby rotating the stirring blade 152 of the stirrer 150 to mix the raw materials. Crush.

At this time, the external power source may be a tabletop drill machine or hand drill.

If the stirrer 150 is not connected to external power but has a motor, etc., it is sufficient to simply operate the stirrer.

(3) Pulsed electric field processing step

After the raw material grinding step, power is supplied to the first electrode 141 for pulse electric field treatment and the second electrode 142 for pulse electric field treatment to process the pulverized raw material with a pulse electric field (PEF).

The innovative potential in the field of PEF is the widespread implementation of this technology for the processing of pumpable fresh food products. While traditional heat sterilization destroys health-promoting ingredients such as vitamins and causes loss of fresh taste, PEF allows heat-sensitive products such as juices and smoothies, where fresh taste is a key quality parameter, to be preserved for long periods of time without detrimental effects on quality. can do. PEF processing technology can be easily implemented into existing production lines with continuous operation and simple equipment design with various capacity options.

For PEF treatment, micro high-voltage pulses of approximately 10 to 60 kV are applied. The applied high-voltage pulse induces micropores in the cell membrane, causing loss of barrier function, leakage of intracellular contents, and loss of vitality.

Liquid or semi-viscous liquids that can be pumped through a PEF treatment device or solid products that must be transported are exposed to high voltage pulses. The required processing time is less than 1 second and pulses are applied at a repetition rate of up to 500 or more times per second to sufficiently process all volume elements. In addition to electrical parameters such as electric field strength and specific energy input, product temperature and product recipe also affect processing intensity.

Meanwhile, at the same time as the pulse electric field (PEF) treatment, the stirrer 150 is operated to send the pulverized raw material from the inner center of the cylindrical body 113 to the inner peripheral surface of the cylindrical body 113, and the pulse electric field is generated from the electrode surface of the pulse electric field (PEF). This extraction device (100) ensures that the treatment is performed evenly and also removes the tendency to stick to the electrode for pulse electric field treatment due to the viscosity of the pulverized raw material due to the turbulence of the pulverized raw material by the stirrer (150). Pulverized raw materials can be efficiently treated with pulsed electric field (PEF).

In addition, in this extraction device 100, the cylindrical first electrode 141 for pulse electric field processing and the second electrode 142 for pulse electric field processing are alternately arranged in the vertical direction along the inner peripheral surface of the insulator 143, so that the By securing a large PEF effective treatment area (surface area of the electrode), PEF treatment efficiency can be increased.

In addition, the present extraction device 100 performs pulse electric field treatment while operating the stirrer 150, thereby making it possible to perform pulse electric field treatment while spreading the raw material or forming a vortex.

When the pulse electric field treatment is completed, the operation of the stirrer 150 is also stopped, external power is separated from the stirrer head 151a, and the stirrer head cap 115e is closed.

(4) Liquid carbon dioxide injection step

After the pulse electric field treatment step, that is, high-pressure liquid carbon dioxide is injected into the pulverized and PEF-treated raw material in the extraction device 100, and the raw material is mixed with the liquid carbon dioxide to form a pressurized mixed raw material.

Specifically, by opening the first opening/closing valve 11a of the liquid carbon dioxide supply pipe 11, liquid carbon dioxide in the carbon dioxide storage unit 10 flows through the liquid carbon dioxide supply pipe 11 and the carbon dioxide inlet 115c to the reactor main body 110. ) is injected into the inside, thereby forming a mixed raw material of the pulverized raw material and liquid carbon dioxide, and the mutual pressure is balanced at 7.4 MPa (i.e., after the pulverized raw material is pressurized), the first opening/closing valve (11a) is opened. Close.

The purpose of injecting liquid carbon dioxide into the pulverized raw materials in this way is to increase the fluidity of the mixed raw materials and facilitate the formation of diffusion flow or vortex around the critical temperature and critical pressure of the mixed raw materials in the active ingredient separation process described later. , the mixed raw material pressurized by liquid carbon dioxide at 7.4 MPa causes the cell membrane (and cell wall) to self-destruct as the high-pressure carbon dioxide penetrates the cell wall where irreversible and reversible micropores have already been formed as a result of the pulse electric field treatment, turning into irreversible micropores. This is to increase the efficiency of extracting active ingredients.

When the water solvent and carbon dioxide of fresh animals and plants themselves penetrate through these micropores, the reversible micropores change into irreversible micropores and the cell membrane (and cell wall) is destroyed. As a result, the reversible micropores change into irreversible micropores, and the cell membrane (and cell wall) destroys itself, spilling out the raw cell fluid, thereby increasing the efficiency of electroporation (or extraction).

As described above, the present extraction device 100 injects liquid carbon dioxide immediately after the pulse electric field treatment step, thereby selectively destroying only the cell membrane (and cell wall) without destroying the active ingredient through short-term administration of electric energy, thereby producing the desired active ingredient (or Not only is it possible to increase the productivity of active substances and enhance other useful activities, but because the extraction is performed at low temperatures, there is no risk of destruction of the active ingredients of fresh animals or plants, so extracts can be obtained stably.

Meanwhile, the temperature and pressure of liquid carbon dioxide are between subcritical and supercritical, with a critical temperature of 31.1℃ and a critical pressure of 7.4 MPa. This temperature and pressure significantly lowers the pressure compared to conventional technology, drastically reducing the price of the overall equipment. It is very effective and economical by reducing energy consumption.

(5) Extraction (heating and cooling)

After liquid carbon dioxide is injected, the extraction process begins.

When the mixed raw materials in a subcritical state are heated by the operation of the lower heater 120, the pressure of the mixed raw materials inside the reactor main body 110 rapidly rises above the critical pressure of carbon dioxide, entering a supercritical state, and liquid carbon dioxide As it boils, a rapid vortex accompanied by a large amount of bubbles and buoyancy occurs from the bottom to the top inside the reactor main body 110, generating a turbulent flow, which forcibly mixes the mixed raw materials, allowing the active ingredient to be quickly separated from the raw materials. You can.

Meanwhile, if only the heater 120 is maintained in operation, the overall pressure of the reactor body 110 will increase over time, and the generation of bubbles and vortices will gradually decrease.

To prevent this, the upper cooler 130 is operated together with the lower heater 120.

When the cooler 130 is operated, condensation occurs at the upper part of the reactor main body 110, that is, the high-temperature gas carbon dioxide rising to the upper part of the reactor main body 110 is cooled and condensed, and then moves back to the lower part of the reactor main body 110, thereby forming the reactor. While a large amount of bubbles and rapid swirling are continuously maintained inside the main body 110, operation like a thermal siphon is possible, allowing a large amount of useful components to be extracted from pulverized animal and plant raw materials.

As described above, the mixed raw materials inside the reactor main body 110 operate in the temperature and pressure ranges of subcritical and supercritical (critical temperature 31.1°C and critical pressure 7.4 MPa), thereby significantly reducing the overall cost of equipment and reducing energy consumption. It is very effective and economical by reducing consumption.

(6) Extraction solution discharge

After extracting useful components from the pulverized animal or plant raw materials for a certain period of time, the operation of the heater 120 and cooler 130 is stopped.

After the heater 120 and the cooler 130 stop operating, the second opening/closing valve 12a of the gaseous carbon dioxide supply pipe 12 is opened, thereby allowing 7.4 MPa of gaseous carbon dioxide in the carbon dioxide storage unit 10 to enter the gaseous carbon dioxide supply pipe. (12) and carbon dioxide is supplied to the upper part of the reactor main body 110 through the inlet 115c, and in this state, when the outlet opening/closing valve 114b-1 of the outlet port 114b is slowly opened, high-pressure gaseous carbon dioxide is released. The dissolved solution from which the useful components are extracted by pressing the mixed raw materials while pushing them downward passes through the filter 117 and the through hole 116b of the filter support plate 116 and is discharged through the outlet port 114b. The liquid is transferred to the essential oil recovery unit (20). In addition, residues filtered in the filter 117 can be discharged to the outside by removing the lower cover 114.

Depending on the embodiment, liquid carbon dioxide may be injected once again into the reactor main body 110 and the extraction process may be repeated again.

This device can also be used as a pilot device for extracting active ingredients.

A pilot is a process to determine whether customer needs are appropriately reflected by creating an initial model system with architectural decisions on non-functional and functional requirements in terms of the characteristics of the system to be completed in the future. This is a process to empirically review whether architectural decisions meet key quality factors. This can increase customer satisfaction, project managers can gain confidence in development productivity, and developers can have the opportunity to learn new architectures. do.

During the pilot process, if missing customer requirements or incorrect reflections of customer requests are discovered, the problem must be resolved by boldly returning to the place where the problem began (feedback). The purpose of the pilot is to provide rapid feedback between users and developers, clarify mutual opinions, and ensure that user requirements can be fully satisfied through a model system that can handle differences in abstract ideas.

The description of the present invention described above is for illustrative purposes, and those skilled in the art will understand that the present invention can be easily modified into other specific forms without changing the technical idea or essential features of the present invention. will be. Therefore, the embodiments described above should be understood in all respects as illustrative and not restrictive. For example, each component described as single may be implemented in a distributed manner, and similarly, components described as distributed may also be implemented in a combined form.

The scope of the present invention is indicated by the claims described below rather than the detailed description above, and all changes or modified forms derived from the meaning and scope of the claims and their equivalent concepts should be construed as being included in the scope of the present invention. do.

100: extraction device
110: reactor body
113: cylindrical body
114: lower cover
115: upper cover
115a: Penetration hole for shaft coupling 115a-1: Second bearing seating hole
115a-2: Female thread hole for cap mounting
115b: material inlet 115c: carbon dioxide inlet
115d: second bearing 115e: stirrer head cap
116: Filter support plate 116a: Bearing seating groove
116b: Through hole 116c: First bearing
117: filter
120: heater
130: cooler
141: First electrode for pulse electric field processing
142: Second electrode for pulse electric field processing
143: insulator
150: stirrer
151: Agitator shaft 151a: Agitator head
152: stirring wing

Claims (6)

In an active ingredient extraction device using carbon dioxide for extracting active ingredients from raw materials by adding raw materials and liquid carbon dioxide,
A reactor body providing an internal space into which the raw materials and the liquid carbon dioxide are added to extract active ingredients from the raw materials;
A stirrer extending along the center of the inner space of the reactor body and including a stirrer shaft rotatably supported on the reactor body and a stirring blade provided on the stirrer shaft;
An active ingredient extraction device using carbon dioxide, comprising a first electrode for pulse electric field treatment and a second electrode for pulse electric field treatment arranged to be separated from each other by an insulator provided on the inner peripheral surface of the reactor main body.
According to claim 1,
An active ingredient extraction device using carbon dioxide, characterized in that it further includes a heater provided at the bottom of the reactor body to induce boiling of the liquid carbon dioxide, and a cooler provided at the top of the reactor body to induce condensation of the boiled carbon dioxide.
The method of claim 1 or 2,
The reactor body includes a cylindrical body in the form of a vertical cylinder,
The first electrode for pulse electric field processing and the second electrode for pulse electric field processing are both cylindrical in shape with the top and bottom open,
An active ingredient extraction device using carbon dioxide, characterized in that the first electrode for pulse electric field treatment and the second electrode for pulse electric field treatment are alternately arranged in the vertical direction along the center of the internal space of the reactor main body.
The method of claim 1 or 2,
An active ingredient extraction device using carbon dioxide, characterized in that a stirrer head for connection to external power is formed at the upper end of the stirrer shaft.
The method of claim 1 or 2,
A filter support plate is provided at the lower part of the internal space of the reactor main body, which has a bearing seating groove with an open top and a plurality of through holes that extend in the vertical direction and are disposed in a form surrounding the bearing seating groove,
A first bearing rotatably supporting the lower end of the agitator shaft is inserted into the bearing seating groove,
An active ingredient extraction device using carbon dioxide, characterized in that a filter having a shaft penetration hole formed in the center for the agitator shaft to pass through is provided on an upper part of the filter support plate.
The method of claim 1 or 2,
The reactor body includes a cylindrical body in the form of a vertical cylinder, an upper cover formed with a material inlet and a carbon dioxide inlet to close the open upper part of the cylindrical body, and a cylindrical body to close the open lower part of the cylindrical body. An active ingredient extraction device using carbon dioxide, characterized in that it is detachably coupled to the body and includes a lower cover having an outlet port.