JPH04281801A - Extraction chamber for supercritical fluid - Google Patents

Abstract

PURPOSE:To decrease variation in extraction and to obtain uniform qualities of extracted components by allowing the height of cases for various products to correspond to each object to be treated and increasing the amount of the extracting medium fluid in contact with the objects. CONSTITUTION:Plural cases 7, 8, 9, each housing objects 6 to be treated are stacked and installed in a cylindrical extraction chamber 2. The extracting medium fluid in a supercritical state is independently introduced to each case 7-9 to dissolve and extract specified components form the objects 6. Then the extracting medium fluid is independently drained and discharged to the outside of the chamber 1.

Description

[Detailed description of the invention]

0001

[Industrial Application Fields] The present invention is applicable to the food industry (coffee, tea decaffeination, hop extraction), pharmaceutical industry (vitamins,
Extraction of medicinal herbal extracts), iron industry (recovery of mill scale, degreasing of ceramics and powder metallurgy, etc.), coal industry (extraction of coal liquefied oil), chemical industry (separation of aromas and paraffin naphthenes), petroleum industry (petroleum residue oil) The present invention relates to a supercritical fluid extraction vessel that is widely applied to the perfume industry (extraction of natural fragrances), and other industries (regeneration of adsorbents).

0002

[Prior Art] Supercritical fluid extraction technology is a type of separation technology along with membrane and organic solvent extraction, distillation, adsorption, chromatography, etc. It is an application of the properties of the state, which is approximately intermediate between gas and liquid, that ``the density is close to that of a liquid, and the diffusion coefficient and clay are close to those of a gas.'' Since extraction can be performed under mild temperature conditions, deterioration and decomposition of heat-labile natural products can be avoided, and the temperature and pressure can be arbitrarily selected for the extract, so there is no worry about solvent residue in the product. The solvent has characteristics such as low viscosity, high diffusivity, fast extraction and separation speed, and the process is anoxic, so there is no oxidation of the extract.

A typical fluid extraction flow involves supplying an extraction solvent (typically carbon dioxide) into the system, a compression pump,
A solvent fluid that has become supercritical by a heat exchanger is supplied to an extraction container, and the soluble components are extracted from the processed product in the extraction container.The solvent fluid is taken out from the extraction container and separated by changing the pressure or temperature. The solvent fluid and soluble components are separated in the tank, and the solvent fluid from which the soluble components have been separated is circulated and reused through the heat exchanger and the compression pump.

[0004] Conventionally, as this type of extraction container, the one illustrated in FIG.
(Refer to Publication No. 03 and Japanese Unexamined Patent Publication No. 63-285176)
. This extraction container 41 includes a cylindrical container main body 42, a constant temperature jacket 43 fitted around the outer periphery of the container main body 42,
An upper lid 44, a lower lid 45, and a cylindrical processing product case 4 disposed within the main body 42 and containing a processing target 46 therein.
Filters 48 and 49 are provided at the upper and lower ends of the processed product case 47 and are held within the press frame 50. The solvent fluid, that is, the extraction medium fluid in a supercritical state is introduced into the container body 42 from the port 51 of the upper lid 44, enters the processed product case 47 through the upper filter 48, passes through the processed product 46, and extracts the extracted material. pass through the lower filter 49 while dissolving the
2 and led to a separately provided separation tank (not shown), where the extractant is separated from the extractant fluid.

[0005]

[Problems to be Solved by the Invention] In the above-mentioned prior art, the diameter of the processed product case 47 cannot be increased significantly because the extraction efficiency decreases when the extraction medium fluid flowing inside the processed product case 47 becomes uneven. Since the extraction container 41 is a pressure container, increasing its diameter will increase the cost, and there is also a limit to increasing the height of the container 1 and the processed product case 47 due to solubility. . Further, there is a problem in that uneven extraction occurs at the upper and lower parts of the processed product case 47.

The present invention has been made in view of the above-mentioned circumstances, and its purpose is to make the height of each product case correspond to the product to be processed, and to reduce the It is an object of the present invention to provide a supercritical fluid extraction vessel that increases the amount of extraction medium fluid in a critical state, reduces uneven extraction, and uniformizes the degree of extraction, and has an optimal structure both technically and economically.

[0007]

[Means for Solving the Problems] In order to achieve the above object, the present invention takes the following technical measures. That is, the present invention according to Claim 1 arranges a processed product case containing a processed product in a cylindrical extraction container main body, introduces a fluid in a supercritical state, and uses the fluid to remove the processed product from the processed product. A supercritical fluid extraction container that dissolves and extracts a specific component and leads out of the extraction container a fluid in a supercritical state in which the specific component is dissolved, which includes a plurality of the processed product cases, and the plurality of processed product cases are The container is characterized by being loaded vertically.

[0008] Further, in the present invention according to claim 2, a pipe for introducing a fluid in a supercritical state and a pipe for leading out the fluid are independently connected to each of the plurality of processing product cases. It is characterized by the presence of Furthermore, in the present invention according to claim 3, each of the processed product cases includes a bottomed cylinder;
It consists of an upper opening and upper and lower filters disposed at the lower part of the cylindrical body, and is characterized in that supercritical fluid is introduced from either one of the upper and lower filters and extracted from the other.

[0009] The present invention according to claim 4 is characterized in that each cylindrical body of the processed product case is provided with another tube that passes through the cylindrical body in the vertical direction and is disposed below or above the processed product case. A flow path that independently introduces the fluid into each of the processed product cases, and a flow path that vertically penetrates the cylinder and is independent from each of the other processed product cases that are disposed above or below the processed product case. It is characterized in that a flow path for leading out the fluid is provided.

0010

[Operation] According to the present invention, the extractant fluid in the supercritical state is
It is introduced into the extraction container 1, flows individually into each of the plurality of processing product cases 7, 8, 9, and efficiently contacts the processed product 6 to dissolve and extract the extractant components. The extractant fluid in which the components are dissolved flows out from each of the treated product cases 7, 8, and 9 individually, is led out of the extraction container 1, and is sent to a separation tank. And each processed product case 7, 8, 9
Since the permeation distance of the extractant fluid within the container is short and equal, the amount of fresh extractant fluid that comes into contact with the workpiece 6 increases, and the unevenness of extraction is reduced, resulting in a uniform extraction degree.
Extraction work can be done efficiently. Furthermore, when the processed material is used after the components have been extracted, the quality can be made uniform and the quality can be improved.

[0011]

Embodiments Hereinafter, embodiments of the present invention will be explained based on the drawings. In the drawings, the extraction container 1 includes a cylindrical container body 2, a pedestal and constant temperature jacket 3 fitted around the outer periphery of the container body 2, and an upper lid 4 and a lower lid 5 of the container body 2.
It is divided into three parts in the vertical direction, and each part has a workpiece 6 inside.
It consists of the same cylindrical processed product cases 7, 8, and 9 in which are housed, and is held within the press frame 10.

The upper lid 4 is provided with an introduction port 11 for supercritical extraction medium fluid, and is removably fitted in a sealed manner to the upper end opening of the container body 2 via a packing 12. Further, the lower lid 5 is provided with a discharge port 13 for an extractant fluid in which extractant components in a supercritical state are dissolved, and is removably fitted in a sealed manner to the lower end opening of the container body 2 via a packing 14. equipped.

Each of the processed product cases 7, 8, and 9 has a cylindrical bottomed cylinder 15, 16, 17, and an upper filter made of sintered metal disposed in the upper opening of each cylinder. 18,19
, 20, and lower filters 24, 25, 26 made of sintered metal are disposed at the bottom of each of the cylindrical bodies 15-17 with required fluid discharge spaces 21, 22, 23 between them and the bottom plate. The cylindrical body 15 of the upper processing product case 7 has the parts shown in Figs.
As shown in FIG. 2, fluid introduction channels 27 and 28 to the intermediate and lower processing product cases 8 and 9 are provided vertically penetratingly, and a fluid outlet channel 29 communicating with the fluid discharge space 21 is provided at the outer periphery of the lower surface. ing. In addition, the processed product case 8 in the middle
As shown in FIGS. 4 and 5, the cylindrical body 16 is provided vertically penetratingly so that a fluid introduction path 30 to the lower processing product case 9 can be connected to the fluid introduction path 28. The fluid outlet path 31 of the processed product case 7 is connected to the upper processed product case 7.
A fluid outlet passage 32 is provided vertically penetratingly so as to be connected to the fluid outlet passage 29 of the cylindrical body 16 , and is provided at the outer peripheral edge of the lower surface to communicate with the fluid discharge space 22 . is the fluid introduction path 27 of the upper processing product case 7.
A fluid introduction path 33 is provided which connects to. moreover,
The cylindrical body 17 of the lower processed product case 9 is provided with a fluid introduction passage 34 on its upper edge so as to be connected to the fluid introduction passage 30 of the cylindrical body 16, and a fluid discharge space 23 on the outer peripheral edge of its lower surface. A communicating fluid outlet port 35 is provided,
Fluid outlet path 3 of the upper and middle processing product cases 7 and 8
Fluid lead-out passages 36 and 37 connected to 1 and 32 are provided in a vertically penetrating manner.

Note that between the lower lid 5 and the bottom plate of the lower processing product case 9 , there is formed a space 38 for leading out the extraction medium fluid from each case 7 , 8 , 9 , and communicates with the discharge port 13 . . In the above embodiment, the supercritical extractant fluid (e.g. carbon dioxide gas) is introduced into the upper space of the upper processing product case 7 from the introduction port 11 of the upper lid 4, and a part of it is introduced from the upper filter 18 into the processing product. The other part passes through the fluid introduction channels 27 and 33 to reach the upper space of the middle-stage processing product case 8 and flows into the case 8 from the upper filter 19, and the other part flows into the case 8. It passes through the introduction channels 28, 30, and 34 to reach the upper space of the lower processed product case 9, and flows into the case 9 from the upper filter 20. Then, in the upper processing product case 7, the product to be processed 6
The extractant fluid in which the extractant components have been dissolved in contact with
9, 31, and 36, and the extraction medium fluid that has come into contact with the product to be processed 6 in the intermediate processing product case 8 and dissolved the extractant components passes through the lower filter 25 and is transferred between the fluid discharge chambers. 22, the extraction medium fluid is led to the fluid derivation space 38 through the fluid derivation paths 32, 37, and furthermore, the extractant fluid that has come into contact with the product to be processed 6 in the lower process product case 9 and dissolved the extractant components is passed through the lower filter. 26 to the fluid discharge space 23, the fluid is guided from the fluid discharge path 35 to the fluid discharge space 38, and is taken out of the extraction container 1 from the discharge port 13 of the lower lid 5. The extraction medium fluid thus derived is transferred to a separation tank (
(not shown), the extractant components are separated from the extractant fluid, and the extractant fluid is again fed into the extraction vessel 1 and used for circulation.

[0015] According to the above embodiment, since the cylindrical bodies 15 to 17 of the upper, middle and lower processing product cases 7 to 9 are provided with the fluid inlet passage and the fluid outlet passage, separate piping is not required. It has a simple structure, is easy to handle, and can be obtained economically. In addition, the fluid transmission distances of each case 7 to 9 are equal and short, and the amount of fresh extraction medium fluid that comes into contact with the product 6 is increased.

The present invention is not limited to the above-mentioned embodiments; for example, the bottom plates of each of the processed product cases 7 to 9 may have a separate structure and be stacked on top of each other;
It can have a square or triangular cross section, and furthermore, fluid can be introduced from port 13 of the lower lid 5 and port 1 of the upper lid 4.
It can be discharged from 1.

[0017]

[Effects of the Invention] As mentioned above, the processing product case inside the extraction container main body is divided into a plurality of parts in the vertical direction, so the height of the case is set to the optimum length according to the processing material, thereby improving extraction efficiency. The structure is technically and economically optimal, and the height of the processed product case can be lowered, allowing fresh supercritical extractant fluid to be supplied and reducing the amount of contact with the processed product. Since it is possible to increase the amount of water and reduce unevenness in extraction, it is possible to make the extract quality components uniform in foods.

[0018] Furthermore, since the fluid in the supercritical state is independently introduced into and taken out of each of the processing product cases,
The quality of the extracted components can be made more uniform, and the extraction efficiency can be improved. Furthermore, the present invention provides for each cylinder of the processing product case to be independently connected to each other processing product case that vertically passes through the cylinder and is disposed below or above the processing product case. a channel for introducing the fluid;
A channel is provided that vertically penetrates the cylindrical body and leads out the fluid independently from each of the other processing product cases arranged above or below the processing product case. Therefore, there is no need to separately provide fluid inlet/outlet piping for the processed product case, and the structure is simple and easy to handle.

According to the present invention, since the processed product case is composed of the bottomed cylinder and the upper and lower filters, each processed product case can be constructed independently by simply stacking the processed product cases.

[Brief explanation of the drawing]

FIG. 1 is a longitudinal sectional view showing an embodiment of the present invention.

FIG. 2 is a central sectional view of the upper processing product case.

FIG. 3 is a plan view of FIG. 2;

FIG. 4 is a central vertical cross-sectional view of the middle-stage processing product case.

FIG. 5 is a plan view of FIG. 4;

FIG. 6 is a central vertical sectional view of the lower processed product case.

FIG. 7 is a bottom view of FIG. 6;

FIG. 8 is a central vertical sectional view of a conventional example.

[Explanation of symbols] 1 Extraction container 2 Extraction container main body 6 Processed products 7, 8, 9 Processed product cases 15, 16, 17 Bottomed cylinders 18, 19, 20 Upper filters 21, 22, 23 Fluid discharge space 24, 25,
26 Lower filter 27, 28, 30, 33, 34 Channel (fluid introduction channel) 29, 31, 32, 35, 36, 37
Flow path (fluid lead-out path) 38 Flow path (fluid lead-out space)

Claims (4)

[Claims] Claim 1: A processing product case containing a processed product is placed in a cylindrical extraction container main body, and a fluid in a supercritical state is introduced, and a specific component is dissolved and extracted from the processed product using the fluid. In a supercritical fluid extraction vessel that leads out the supercritical fluid in which the specific component is dissolved, to the outside of the extraction vessel,
A supercritical fluid extraction container characterized in that it has a plurality of the processed product cases and the plurality of processed product cases are stacked in the vertical direction of the container. [Claim 2] Each of the plurality of processed product cases includes:
2. The supercritical fluid extraction vessel according to claim 1, wherein a pipe for introducing fluid in a supercritical state and a pipe for leading out the fluid are independently connected. 3. Each of the processing product cases includes a bottomed cylinder and upper and lower filters disposed at an upper opening and a lower part of the cylinder, and the fluid in a supercritical state is disposed in either of the upper or lower filters. The supercritical fluid extraction vessel according to claim 1 or 2, wherein the supercritical fluid extraction vessel is introduced from one side and drawn out from the other side. 4. A cylindrical body of each of the processed product cases is provided with a tube extending vertically through the cylindrical body and independently connected to each of other processed product cases disposed below or above the processed product case. a channel for introducing the fluid; a channel for vertically penetrating the cylindrical body and leading out the fluid independently from each of other processing product cases disposed above or below the processing product case; 4. The supercritical fluid extraction vessel according to claim 3, further comprising: a.