KR20210143504A - A device for extracting an active ingredient using hydrolysis in a supercritical state and a method for extracting an active ingredient using hydrolysis in a critical state using the same - Google Patents

Abstract

The present invention relates to an active ingredient extraction apparatus using hydrolysis in a supercritical state and, more specifically, to an active ingredient extraction apparatus using hydrolysis in a supercritical state, which can effectively control the temperature and pressure applied to an object to be hydrolyzed and can add a solvent depending on the object to be hydrolyzed to increase hydrolysis efficiency. According to the present invention, the active ingredient extraction apparatus comprises: a reaction vessel (110) including the sealed inside and a rotary shaft (111) provided on the outside of both end parts; a driving means (200) rotating the reaction vessel (110); a support unit (210) allowing the rotary shaft (111) and the driving means (200) to be installed thereon and controlling the load of the reaction vessel (110); a vacuum nozzle (120) to which a vacuum pump (121) can be connected from the outside of the reaction vessel (110); and a solvent nozzle (140) a solvent (141) to the reaction vessel (110). The active ingredient extraction apparatus is configured to hydrolyze chitosan on the inside of the reaction vessel (110) to produce glucosamine.

Description

An active ingredient extraction device using hydrolysis in a supercritical state, and an active ingredient extraction method using hydrolysis in a critical state using the same in a critical state using the same}

The present invention relates to an apparatus for extracting active ingredients using hydrolysis in a supercritical state and a method for extracting active ingredients using hydrolysis in a critical state using the same. Specifically, it is possible to effectively extract active ingredients hydrolyzed in a supercritical state. It relates to an active ingredient extraction device.

It is known that, in a general hydrolysis process of an object, when the object is hydrolyzed at high temperature and high pressure, the time required is significantly shortened and the hydrolysis efficiency is remarkably improved.

Hydrolysis reaction refers to a reaction that decomposes organic compounds by adding water. Specifically, H ₂ O is ionically decomposed to become H ⁺ ions and OH ^- ions, which react with specific functional groups of organic compounds to break existing bonds. is a reaction

Water is usually vaporized when the temperature reaches 100°C at a pressure of 1 atm (0.1 MPa) to become vapor in a gaseous state. However, in the closed state, when the evaporated water vapor becomes saturated, no more evaporation occurs. The temperature at this time is the saturation temperature, and the pressure at this time is the saturated water vapor pressure.

In general, the temperature and vapor pressure in a critical state in which the two states of liquid and gas cannot be distinguished from each other are called critical points, and supercritical refers to a state having conditions above the critical pressure and critical temperature. The critical pressure of water is about 22 MPa and the critical temperature is about 374 °C. Water in a state above this temperature and pressure is called supercritical water.

In the supercritical or near subcritical state, water exhibits properties that were unthinkable at room temperature. In this state, water becomes neither a liquid nor a gas, and exhibits very strong reactivity. In particular, the strongest hydrolysis action occurs characteristically in the subcritical region at 2 MPa and 200 to 300 °C. In this state, the hydrolysis reaction occurs at a reaction rate of 100 to 1,000 times that of room temperature.

In the supercritical or subcritical state, water can decompose almost all substances, including organic substances as well as inorganic substances, due to its strong reaction force. Conventionally, a strong hydrolysis reaction in such a supercritical state has been applied to a waste treatment device.

Korean Patent Application Laid-Open No. 2014-0020854 discloses a waste optimization treatment method for decomposing organic compounds contained in an aqueous effluent in a supercritical state.

However, in the existing supercritical hydrolysis apparatus, it is possible to decompose harmful substances into less harmful substances, but it is impossible or cumbersome to extract beneficial components as a result of the decomposition. First, there is a procedural inconvenience that the reaction result can be obtained only by lowering the high-temperature and high-pressure state caught in the pressure vessel to room temperature and normal pressure.

That is, in the above-mentioned prior literature, the contents can be taken out only after the completion of hydrolysis and cooling/depressurization, and the hydrolysis reaction product is discharged in a mixed state with useful components and residues, so a method for extracting useful components is urgently needed. am.

Republic of Korea Patent Publication No. 2014-0020854

The present invention was invented to solve the above problems, and its object is to extract an active ingredient using hydrolysis in a supercritical state that can effectively extract useful active ingredients from a target material using hydrolysis efficiency, and an apparatus for extracting active ingredients using the same An object of the present invention is to provide a method for extracting active ingredients using hydrolysis in a critical state.

The present invention for achieving the above technical problem is a reaction vessel 110 having a closed inside and a rotating shaft 111 on the outside of both ends; a driving means 200 for rotating the reaction vessel 110; The rotation shaft 111 and the driving means 200 are installed, the support portion 210 for controlling the load of the reaction vessel (110); a vacuum nozzle 120 to which a vacuum pump 121 can be connected from the outside of the reaction vessel 110; a steam nozzle 130 to which a boiler 131 for supplying saturated steam from the outside of the reaction vessel 110 can be connected; and a solvent nozzle 140 for supplying the solvent 141 for extracting the active ingredient to the reaction vessel 110, wherein the solvent nozzle is also used as a discharge nozzle of the extract.

In one embodiment, the reaction vessel 110, it characterized in that it further comprises a plurality of stirring projections 150 protruding toward the center on the inside.

In one embodiment, a speed reducer is coupled to the driving means 200 to control the rotational speed of the reaction vessel 110 .

The present invention also provides a method of extracting an active ingredient using a hydrolysis reaction in a supercritical state using the extraction device, a process of injecting raw materials into a closed reaction vessel, vacuuming the reaction vessel and injecting saturated steam The process, the process of pressurizing the reaction vessel to a pressure of 1.5 to 2.0 MPa and heating it to a temperature of 150 to 300 ℃, a process of stirring the inside of the reaction vessel to cause the hydrolysis reaction, the process of injecting a liquid extraction solvent, and extracting the extract It provides an extraction method comprising the step of discharging.

According to the apparatus for extracting active ingredients using hydrolysis in the supercritical state of the present invention, the resultant hydrolyzed in the supercritical state can be easily extracted without releasing the high temperature and high pressure state.

1 is a schematic diagram schematically showing an apparatus for extracting active ingredients using hydrolysis in a supercritical state of the present invention.
2 is a temperature-pressure dependent state diagram of water.
3 is a schematic diagram showing the extraction method proceeding process of the present invention in time series.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, a detailed description of preferred embodiments of the present invention will be described with reference to the accompanying drawings. It should be noted that like elements in the drawings are denoted by like numerals wherever possible. Specific specific details are set forth in the following description, which are provided to help a more general understanding of the present invention. In the description of the present invention, if it is determined that a detailed description of a related known function or configuration may unnecessarily obscure the gist of the present invention, the detailed description thereof will be omitted.

The terms used in this specification have been selected as currently widely used general terms as possible while considering the functions in the present invention, which may vary depending on the intention or precedent of a person skilled in the art to which the present invention belongs, the emergence of new technology, etc. have. In addition, in specific cases, there are also terms arbitrarily selected by the applicant, and in this case, the meaning will be described in detail in the corresponding description of the present invention. Therefore, the terms used in this specification should be defined based on the meaning of the term and the content throughout the present specification, rather than the simple name of the term.

Terms such as first or second may be used to describe various elements, but the elements should not be limited by the terms. The above terms are used only for the purpose of distinguishing one component from another, for example without departing from the scope of the inventive concept, a first component may be termed a second component and similarly a second component A component may also be referred to as a first component.

When a component is referred to as being “connected” or “connected” to another component, it may be directly connected or connected to the other component, but it is understood that other components may exist in between. it should be On the other hand, when it is said that a certain element is "directly connected" or "directly connected" to another element, it should be understood that the other element does not exist in the middle. Other expressions describing the relationship between components, such as "between" and "immediately between" or "neighboring to" and "directly adjacent to", etc., should be interpreted similarly.

The terms used herein are used only to describe specific embodiments, and are not intended to limit the present invention. The singular expression includes the plural expression unless the context clearly dictates otherwise. In the present specification, terms such as "comprise" or "have" are intended to designate that a feature, number, step, operation, component, part, or combination thereof described herein exists, but one or more other features It is to be understood that it does not preclude the possibility of the presence or addition of numbers, steps, operations, components, parts, or combinations thereof.

Unless defined otherwise, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in a commonly used dictionary should be interpreted as having a meaning consistent with the meaning in the context of the related art, and should not be interpreted in an ideal or excessively formal meaning unless explicitly defined in the present specification. does not

Hereinafter, an apparatus for extracting active ingredients using hydrolysis in a supercritical state of the present invention will be described in detail by describing a preferred embodiment of the present invention with reference to the accompanying drawings.

1 is a schematic diagram schematically showing an active ingredient extraction device using hydrolysis in a supercritical state of the present invention.

Referring to Figure 1, the present invention, the active ingredient extraction apparatus using hydrolysis in a supercritical state, the inside is sealed, the reaction vessel 110 is provided with a rotating shaft 111 is provided outside both ends. The reaction vessel 110 is used as a stirring device, and a plurality of stirring protrusions 150 protruding toward the center are formed on the inner surface, so that more efficient stirring of the contents can be performed.

On the other hand, the reaction vessel 110 is provided with a rotation shaft 111 in the center, the rotation shaft 111 is supported by a support member 112 having a bearing or the like therein is configured to rotate in place. Here, the rotating shaft 111 is connected to the driving means 200 to rotate the rotating shaft 111 by power generated from the driving stem 200 , and through this, the reaction vessel 110 also rotates at the same time.

On the other hand, the rotation shaft 111 and the driving means 200 are installed, and the support part 210 for controlling the load of the reaction vessel 110 is provided. The support part 210 may be configured in various forms, for example, a frame using a metal material other than those shown in the drawings may be applied.

On the other hand, the reaction vessel 110 has a vacuum nozzle 120 to which a vacuum pump 121 can be connected to draw out internal air to the outside, and steam to which a boiler 131 can be connected to supply saturated steam. The nozzle 130 and the solvent nozzle 140 for supplying the solvent 141 to the reaction vessel 110 may be configured. The vacuum nozzle 120 , the steam nozzle 130 and the solvent nozzle 140 cannot be connected to the vacuum pump 121, the boiler 131 and the solvent 141 reservoir from the outside when the reaction vessel 110 is driven. Therefore, each nozzle must be blocked. Therefore, before the reaction vessel 110 is driven, the vacuum pump 121, the boiler 131, and the solvent 141 storage must be separated from the vessel to take a separate action.

After the raw material containing the component to be extracted is put into the reaction vessel, it is preferable to operate a vacuum pump to remove air from the inside of the reaction vessel to almost a vacuum. Temperature rise due to residual air can be prevented, and gaps can be created as the gas contained in the raw material expands by vacuum, thereby helping the saturated water vapor injected afterward to penetrate efficiently into the raw material.

After vacuum operation, saturated steam is injected. The injection of saturated water vapor is preferably performed so that the internal pressure of the reaction vessel is about 1.5 to 2.0 MPa and the temperature is about 150 to 300°C, and more preferably, the pressure is about 2.0 MPa and the temperature is about 200 to 300°C.

The saturated water vapor thus introduced becomes a supercritical state or a similar subcritical state in the reaction vessel, and hydrolysis of the raw material occurs rapidly. The components after hydrolysis of the components included in the raw materials are, for example, as shown in Table 1 below.

[ Table 1 ]

Take chitosan as an example. When chitosan is added to the inside of the reaction vessel 110, it is hydrolyzed to produce glucosamine. Chitosan and glucosamine are well known as health foods, and since chitosan is a polymer of glucosamine, hydrolysis of chitosan produces glucosamine. Specifically, the ether bond (-O-) of the chitosan molecule is hydrolyzed by water to break the polymer chain to produce a small molecule, glucosamine.

Here, the ether bond is difficult to hydrolyze with only water. So, usually hydrochloric acid (HCl) or sulfuric acid (H ₂ SO ₄ ) is used as a catalyst, in which case glucosamine is obtained as hydrochloride or sulfate. However, according to the present invention, since the help of a catalyst such as hydrochloric acid or sulfuric acid is not required, it is possible to obtain intact glucosamine only with pure water.

After injecting saturated steam, the reaction vessel is driven (stirred) to cause hydrolysis. The driving (stirring) time of the reaction vessel is preferably about 50 minutes to 1 hour.

After the hydrolysis reaction is sufficiently proceeded, the operation is stopped and a solvent capable of dissolving the target active ingredient is added. After injecting the extraction solvent in the liquid state into the reaction vessel 110 (spraying, etc.), the extract is obtained by discharging the solvent collected at the bottom. For example, the solvent is injected through the solvent nozzle 140 , and the solvent 141 is injected into the solvent nozzle 140 after rotating and fixing the injected solvent nozzle 140 to be positioned on the upper part. This is to spread the solvent injected into the reaction vessel 110 to be sprayed relatively evenly. In this case, an appropriate extraction solvent capable of dissolving the active ingredient is used.

The solvent may be preferably added in a liquid state, and polar/non-polar solvents and organic/inorganic solvents may be appropriately used according to the desired physical properties of the extraction target. For example, if the active ingredient to be extracted is water-soluble, water or an aqueous solvent may be used as the solvent, and if the active ingredient is an organic substance, an organic solvent may be used. The liquid solvent is preferably sprayed, but the present invention is not limited thereto.

After adding the solvent for extraction, the extraction efficiency may be increased by further driving the reaction vessel. The injected solvent serves to dissolve and elute the target component from the hydrolysis residue of the raw material.

After driving or leaving the reaction vessel to sufficiently extract the desired component, the extraction solvent in which the target component is dissolved, that is, the extract solution is easily discharged immediately. In the case of a conventional hydrolysis processor, there was an inconvenience that the temperature and pressure of the reaction vessel had to be lowered to room temperature/normal pressure to take out the result from the inside after hydrolysis was completed, Although it was necessary to go through a separate process for extracting components, according to the present invention, the extract solution collected on the floor can be easily discharged simply by opening the solvent nozzle 140 at the bottom of the reaction vessel regardless of the temperature and pressure of the reaction vessel. There is a point.

On the other hand, the drive means 200 is coupled to a speed reducer is configured to control the rotational speed of the reaction vessel (110). That is, by controlling the rotation speed of the reaction vessel 110, it is possible to control the hydrolysis time and efficiency.

According to the present invention, it takes only about 1 hour to extract the active ingredient.

The embodiment of the apparatus for extracting active ingredients using hydrolysis in the supercritical state of the present invention described above is merely exemplary, and those of ordinary skill in the art to which the present invention pertains have technical ideas or essential features of the present invention It will be understood that it can be easily transformed into another specific form without changing the . Therefore, it should be understood that the embodiments described above are illustrative in all respects and not restrictive. For example, each component described as a single type may be implemented in a dispersed form, and likewise components described as distributed may be implemented in a combined form.

The scope of the present invention is indicated by the following claims rather than the above detailed description, and all changes or modifications derived from the meaning and scope of the claims and their equivalent concepts should be interpreted as being included in the scope of the present invention. something to do.

110: reaction vessel
111: axis of rotation
112: support member
120: vacuum nozzle
121 vacuum pump
130: steam nozzle
131: boiler
140: solvent nozzle
141: solvent
150: stirring protrusion
200: driving means
210: support

Claims (4)

The inside is sealed, the reaction vessel 110 is provided with a rotation shaft 111 on the outside of both ends;
a driving means 200 for rotating the reaction vessel 110;
The rotation shaft 111 and the driving means 200 are installed, the support portion 210 for controlling the load of the reaction vessel (110);
a vacuum nozzle 120 to which a vacuum pump 121 can be connected from the outside of the reaction vessel 110;
a steam nozzle 130 to which a boiler 131 for supplying saturated steam from the outside of the reaction vessel 110 can be connected; and
A solvent nozzle 140 for supplying the solvent 141 to the reaction vessel 110;
The solvent nozzle 140 is an active ingredient extraction device using hydrolysis in a supercritical state, characterized in that it is also used as a discharge nozzle of the extract.
According to claim 1,
The reaction vessel 110,
Active ingredient extraction device using hydrolysis in a supercritical state, characterized in that it further comprises a plurality of stirring protrusions 150 protruding toward the center on the inside. According to claim 1,
An active ingredient extraction device using hydrolysis in a supercritical state, characterized in that a reduction gear is coupled to the driving means 200 to control the rotational speed of the reaction vessel 110 . The process of putting raw materials into a sealed reaction vessel,
The process of vacuuming the reaction vessel and injecting saturated water vapor,
A process of pressurizing the reaction vessel at a pressure of 1.5 to 2.0 MPa and heating it to a temperature of 150 to 300 °C;
A process of stirring the inside of the reaction vessel so that the hydrolysis reaction occurs,
A process of injecting an extraction solvent in a liquid state, and
Characterized in that it comprises a process of discharging the extract,
An active ingredient extraction method using an active ingredient extraction device using hydrolysis in a supercritical state according to any one of claims 1 to 3.

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