JPH04281802A - Extraction chamber for supercritical fluid - Google Patents

Abstract

PURPOSE:To obtain uniform qualities of extracted components by increasing the amt. of an extracting medium fluid in contact with objects to be treated and decreasing variation in extraction. CONSTITUTION:A case 7 having cylindrical two dispersion filters 13, 14 concentrically provided and housing the object 6 to be treated is installed in a cylindrical extraction chamber 2. The extracting medium fluid in a supercritical state is introduced so that the fluid is introduced from the outer surface of the filter 14 to the inside of the case to dissolve and extract specified components from the object 6. Then the fluid in which the specified components are dissolved is drained through the filter 13 and discharged to the outside of the chamber 2.

Description

[Detailed description of the invention]

0001

[Industrial Application Fields] The present invention is applicable to the iron industry (recovery of mill scale, degreasing of ceramics and powder metallurgy, etc.), the coal industry (extraction of coal liquefied oil), the food industry (decaf of coffee and tea, hop extraction), pharmaceutical industry (extraction of vitamins and medicinal herb extracts), chemical industry (aroma, separation of paraffinnaphthenes), petroleum industry (deastrophication of petroleum residue oil), fragrance industry (
The present invention relates to a supercritical fluid extraction vessel that is widely applied to industries such as natural flavor extraction) and other industries (adsorbent regeneration).

0002

[Prior Art] Supercritical fluid extraction technology is a type of separation technology, along with membrane and organic solvent extraction, distillation, adsorption, and chromatography. It takes advantage of the characteristics of a state approximately intermediate between gases and fluids, which have a density close to that of a liquid and a diffusion coefficient and viscosity 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 separation rate, and an oxygen-free process that does not cause 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. Separates solvent fluid and soluble components in a tank,
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 Patent Application Laid-open No. 63-285176)
. This extraction container 31 includes a cylindrical container main body 32, a constant temperature jacket 33 fitted around the outer periphery of the container main body 32,
An upper lid 34, a lower lid 35, and a cylindrical processed product case 3 disposed inside the main body 32 and containing a processed product 36 therein.
7, filters 38 and 39 are provided at the upper and lower ends of the processed product case 37, and are held within the press frame 40. Then, the supercritical extraction medium fluid is introduced into the container body 32 from the port 41 of the lower lid 35, enters the processed product case 37 through the lower filter 39, passes through the processed product 36, and dissolves the extracted substance. The extract material passes through the upper filter 38, is led out from the port 42 of the upper lid 34, and is led to a separately provided separation tank (not shown), where the extracted substance is separated from the extraction medium fluid.

[0005]

[Problems to be Solved by the Invention] In the above-mentioned prior art, when the product to be processed is powder or granular material (for example, coffee, chopped tobacco, etc.), uneven extraction may occur between the upper and lower parts of the product case 37, and There is a problem in that complete extraction is not possible in areas where it is difficult for the supercritical extraction fluid to pass, making it difficult to maintain uniform quality.

The present invention has been made in view of the above-mentioned circumstances, and its purpose is to increase the amount of supercritical extractant fluid that comes into contact with the product to be processed and to reduce uneven extraction. An object of the present invention is to provide a supercritical fluid extraction vessel capable of achieving a uniform extraction degree.

[0007]

[Means for Solving the Problems] In order to achieve the above object, the present invention takes the following technical measures. That is, in the present invention, a processed product case containing a processed product is placed inside a cylindrical extraction container body, and a fluid in a supercritical state is introduced, and the fluid dissolves and dissolves specific components from the processed product. In a supercritical fluid extraction container for extracting and leading out a fluid in a supercritical state in which the specific component is dissolved to the outside of the extraction container, the processed product case has a double internal and external fluid-permeable cylindrical body of substantially similar shape,
It is characterized in that fluid in a supercritical state is introduced from one of the dual inner and outer cylinders, and fluid in a supercritical state is led out from the other.

[0008] It is preferable that the double inner and outer cylindrical body is constituted by a sintered metal dispersion filter.

[0009]

[Operation] According to the present invention, the extractant fluid in the supercritical state is
It is introduced into the extraction container 1 , flows into the processed product case 7 through one entire circumferential surface of the double internal and external fluid permeable cylinders 13 and 14 , efficiently contacts the processed product 6 , and extracts the extractant components. The extractant fluid in which the extractant components have been dissolved flows out from the entire circumferential surface of the other fluid-permeable cylinder 13, 14, exits the processed product case 7, and is led out of the extraction container 1, Sent to a separation tank. And a double internal and external fluid permeable cylinder 1
The intervals between 3 and 14 (shortest fluid transmission distance) are all equal, and the amount of extraction medium fluid that comes into contact with the workpiece 6 increases,
Uneven extraction is reduced, the degree of extraction becomes uniform, and extraction work can be done more efficiently. Furthermore, when the processed material is used after the components have been extracted, the quality is particularly uniform and the quality is improved.

0010

Embodiments Hereinafter, embodiments of the present invention will be explained based on the drawings. 1 to 3 show a first embodiment of the present invention, in which an 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 a container body 2. It consists of an upper lid 4 and a lower lid 5, and a cylindrical processing product case 7 in which a processed product 6 is housed, and is held within a press frame 8.

[0011] The upper lid 4 is provided with a discharge port 9 for extracting medium fluid in which extractant components in a supercritical state are dissolved.
It is removably fitted into the upper end opening of the container body 2 via a packing 10 in a sealed manner. In addition, the lower lid 5
is provided with an introduction port 11 for the extraction medium fluid in a supercritical state, and is removably fitted in a sealed manner to the lower end opening of the container body 2 via a packing 12.

The processed product case 7 includes an inner and outer dual fluid permeable cylinder (dispersion filter) 13, 14, and an upper lid 15.
and a lower lid 16, the cylinders 13 and 14 are formed into concentric cylindrical shapes by sintered metal filters, and the upper lid 15
has an annular shape with an extraction medium fluid outlet 17 in the center,
The upper ends of the inner and outer cylinders 13 are fixed to the outlet 17,
It is removably fitted into the upper end opening of the outer cylindrical body 14 via a seal packing 18 . Further, the lower lid 16 is disc-shaped, and has a fitting recess 19 for the inner cylinder 13 in the center of its upper surface, and is removably fitted into the lower end opening of the outer cylinder 14, so that the lower surface of the lower lid 16 and the container A flow path 20 for the extraction medium fluid is formed between the main body 2 and the lower lid 5 . The outer diameter of the outer cylindrical body 14 is smaller than the inner diameter of the container body 2 except for the upper end, and an annular flow path 21 for the extraction medium fluid is formed between the container body 2 and the outer cylindrical body 14 over the entire circumference. A seal packing 22 is provided on the outer periphery of the upper end of the outer cylindrical body 14 to close the upper end of the annular flow passage 21 and prevent the extraction medium fluid from flowing from the entire outer periphery of the outer cylindrical body 14 toward the inner cylindrical body 13. flows into the inner cylindrical body 13, passes through the outlet 17 of the upper lid 15, reaches the space above the upper lid 15, and enters the discharge port 9.
It is designed to be guided out from the extraction container 1.

In the first embodiment, the extraction medium fluid (for example, carbon dioxide gas) brought to a supercritical state flows from the introduction port 11 of the lower lid 5 to the lower flow path 20 of the processed product case 7.
It flows into the annular flow path 21 outside the outer cylinder 14, permeates from the entire outer circumference of the outer cylinder 14 toward the center, uniformly contacts the product 6, and absorbs extractive components. is dissolved and extracted. Then, the extractant fluid in which the extractant components are dissolved passes through the entire circumferential surface of the inner cylinder 13 and passes through the inner cylinder 13.
from the outlet 17, passes through the upper side of the processed product case 7, is taken out of the extraction container 1 through the discharge port 9, and is sent to a separation tank where the extractant components are separated from the extractant fluid. The fluid is again fed to the extraction vessel 1 and used for circulation. Note that the shortest distance through which the extraction medium fluid permeates from the outer cylinder 14 to the inner cylinder 13 is the distance between the two cylinders 13 and 14.
They are all spaced at the same distance, and the amount of extraction medium fluid that comes into contact with the workpiece 6 increases, and the amount is the same over the entire area, which greatly reduces uneven extraction of components.

In the first embodiment, the extraction medium fluid is transferred from the inner cylinder 13 to the outer cylinder 14 by using the discharge port 9 of the upper lid 4 as an extraction medium fluid inlet and the introduction port 11 of the lower lid 5 as a discharge port. It can be passed through. FIG. 4 is a cross-sectional view of the main part of the second embodiment of the present invention, that is, the processed product case 7, and shows sintered metal cylinders 13A, 13B, 14A, 14B.
The product case has a four-layer structure, and the product to be processed 6 is accommodated between the cylinders 13A and 14A and between the cylinders 13B and 14B, respectively, and the extraction medium fluid is introduced from the space between the cylinders 14A and 13B. (or derived) and cylinder 1
The extraction medium fluid is drawn out (or introduced) from the inside of the cylindrical body 3A and the outside of the cylindrical body 14B, and the same effects as those of the first embodiment can be expected.

[0015] The present invention is not limited to the above-mentioned embodiments; for example, the cylindrical body 13 constituting the processed product case 7,
14 can have a square or triangular cross-sectional shape.

[0016]

Effects of the Invention As described above, the present invention provides that the processed product case in the extraction container main body has two fluid-permeable cylinders, the inner and the outer sides of which are substantially similar, and the supercritical state is obtained from one of the cylinders. Since the extraction medium fluid is configured to be introduced from one side and taken out from the other, the permeation distance of the extraction medium fluid is short and the same, and the entire area is effectively used, there is no dead space, and it comes into contact with the product to be processed. The amount of extraction medium fluid is increased, extraction unevenness is very small, and extraction efficiency can be improved and quality can be made uniform.

[Brief explanation of the drawing]

FIG. 1 is a central vertical sectional view showing a first embodiment of the present invention.

FIG. 2 is a sectional view taken along the line AA in FIG. 1;

FIG. 3 is a central vertical sectional view of the processed product case.

FIG. 4 is a cross-sectional view of the main part of the second embodiment of the present invention, particularly the processed product case.

FIG. 5 is a central vertical cross-sectional view of a conventional example.

[Explanation of symbols]

1 Extraction container 2　Container body 6 Items to be processed 7 Processed product case 13 Inner fluid permeable cylinder 14 Outer fluid permeable cylinder

Claims (2)

[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,
The processed product case has an inner and outer double fluid-permeable cylinder of substantially similar shape, and a fluid in a supercritical state is introduced from one of the double cylinders, and a fluid in a supercritical state is introduced from the other. A supercritical fluid extraction vessel characterized in that it derives. 2. The supercritical fluid extraction vessel according to claim 1, wherein the double inner and outer cylinders are made of a sintered metal dispersion filter.