JPH05184806A - Extraction vessel of supercritical fluid extracting and separating device - Google Patents

Abstract

PURPOSE:To extremely easily switch the supercritical fluid-introducing direction by providing a guide to fix the inner cylinder at two different positions at the bottom of a vessel and appropriately changing the positions of the inner cylinder in the vessel main body. CONSTITUTION:A guide 10 is provided at the bottom of a vessel main body 6 to fix an inner cylinder 1 at two different positions 8 and 9. When the inner cylinder 1 is fixed at the position 8, a supercritical fluid is introduced from an inlet passage 13, sent downward into the inner cylinder 1, passed through a material 2 to be extracted, sent into a surplus space 7 from an aeration space 3, passed through the outlet passage 14 of a lid 11 and discharged to the outside. Besides, when the supercritical fluid is passed upward through the material 2 because of the property of the material 2, the inner cylinder 1 is fixed at the other position 9, and hence the supercritical fluid introduced from the inlet passage 13 is sent downward through the space 7, introduced into the aeration space 3 of the inner cylinder 1, sent upward in the inner cylinder 1, passed through the material 2 and discharged to the outside from the outlet passage 14 of the lid 11.

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention uses a supercritical fluid as a solvent to extract animal and vegetable fats and caffeine from foods,
The present invention relates to an extraction container of a supercritical fluid extraction / separation device for extracting medicinal components from plant matter and nicotine from tobacco.

[0002]

2. Description of the Related Art Generally, a fluid having one phase that is neither a gas nor a liquid under a condition of exceeding a critical temperature and a critical pressure is called a supercritical fluid.
Its density is close to that of liquid, it has a dissolving power similar to that of liquid, and its diffusion coefficient is remarkably larger than that of liquid. It has a property intermediate between gas and liquid, and has excellent properties as a solvent.

Therefore, in recent years, research on a supercritical fluid extraction separation technique using the above-mentioned supercritical fluid as a solvent has been actively conducted.

FIG. 4 shows an example of a conventional supercritical fluid extraction / separation apparatus. In the figure, a is a CO ₂ cylinder, b is a compression pump, c and c ′ are heat exchangers, d is an extraction vessel, and e is e. Separation vessels, f and g are throttle valves, and the CO ₂ cylinders a to C
After supplying O ₂ to replace the air in the system with CO ₂ , CO ₂ is pressurized and heated by the compression pump b and the heat exchanger c to a supercritical state, and this is introduced into the extraction vessel d. Then, the soluble matter (extract) in the substance to be extracted previously stored in the extraction container d is dissolved in CO ₂ in the supercritical state for extraction, and then the soluble matter is dissolved. The supercritical state of CO ₂ is released by leaking CO ₂ to the separation container e side while maintaining the critical pressure on the extraction container d side by the throttle valve f and reducing the pressure to below the critical pressure in the separation container e. CO ₂
And the soluble component are separated, and the separated soluble component is stored as an extract in the separation container e, and CO ₂ is stored in the heat exchanger c ′.
It is recirculated through the valve, or the throttle valve g is opened to discharge it out of the system.

The details of the extraction container d are as shown in FIGS. 5 and 6, and a container body i having an upper opening provided with a flow path h vertically penetrating the bottom portion at the center of the bottom and the container body at the center of the lower surface. The upper part of the container body i is closed by a fitting convex portion j that fits on the inner peripheral portion of i and is provided with two flow paths k and m penetrating between the lower surface and the upper surface of the fitting convex portion j. An extract to be stored in the container body i, which has a lid n and a bottom p that is raised to ensure an appropriate ventilation space o at the bottom and a communication part q with a filter provided at the center of the bottom p. and an inner cylinder s for storing r, and each of the flow passages h, k, and m has an extraction container d
4 is connected outside as shown in FIG. 4, and by operating the switching valves u, v, w, x, y of the piping system t, for example, switching valves v, y, and switching valve u opened x, is introduced from the flow path k of the lid n as shown in FIG. 5 by closing the w of CO ₂ in the supercritical state for the extraction vessel d, the CO ₂ that the introduction, the After passing the extract r, the extract r is led to the communication part q with a filter and the flow path h so that it can be discharged to the outside of the extraction container d.

Here, the introduction of CO ₂ into the extraction container d is carried out by opening the switching valves u, y, w and closing the switching valves v, x as shown in FIG. It is also possible to introduce CO ₂ from the flow path h at the bottom of the main body i and discharge it from the flow path m of the lid n.

[0007] Thus, the reason you have to be switched to the direction of introduction of the CO ₂ is because it is necessary to switch the direction of introduction of the CO ₂ by the nature of the substance to be extracted r,
For example, when the substance r to be extracted is a powder and CO ₂ is introduced from the lower side to the upper side of the extraction container d, the substance r to be extracted is entrained in the flow of the CO ₂ and the flow path m of the lid n. This is because of a problem such as a problem of blocking.

In the figure, z indicates a sealing material.

[0009]

However, in the above-mentioned conventional supercritical fluid extraction / separation device, since it is necessary to switch the CO ₂ introduction direction as described above, the flow path is switched to the outside of the extraction container d. The piping system t is required, and the flow passages h, k, and m have to be bored in both the container body i and the lid n that form the extraction container d, and the manufacturing cost of the supercritical fluid extraction / separation device is high. There was a problem of causing a sharp rise in the price.

The present invention has been made in view of the above situation, and an object thereof is to reduce the manufacturing cost of a supercritical fluid extraction / separation device.

[0011]

According to the present invention, a communicating portion with a filter is provided at a bottom portion raised to secure a ventilation space at a lower portion, and an opening portion for opening the ventilation space to an outer periphery of the lower end is formed at a lower end. Any one of an inner cylinder for containing the substance to be extracted, a container body with an upper opening having a guide portion capable of fixing the inner cylinder at two different fixed positions, and the two fixed positions. An inlet passage and a discharge which can be simultaneously opened and closed with the upper part of the container body fixed to and accommodated in the container body and communicate with the inside of the container body above each of the two fixed positions when closed. The present invention relates to an extraction container of a supercritical fluid extraction / separation device, which is provided with a lid body having a channel formed therein.

[0012]

Therefore, in the present invention, when the inner cylinder containing the substance to be extracted is fixed at one fixing position on the inner bottom of the container body and the lid is attached to the upper part of the container body, the upper part of the container body and the upper part of the inner cylinder are separated from each other. At the same time, they are closed, and at this time, one flow path of the lid body communicates with the inner cylinder and the other flow path communicates with an extra space in the container body other than the inner cylinder.

Here, if the one flow path is the introduction flow path and the other flow path is the discharge flow path, the supercritical fluid introduced from the introduction flow path descends in the inner cylinder. After passing through the extract, the soluble matter (extract) in the substance to be extracted is extracted, passes through the communication part with the filter, and flows out from the ventilation space to the excess space in the container body through the opening, It is discharged from the excess space to the outside of the extraction container through the discharge passage of the lid.

When it is desired to pass the supercritical fluid from the lower side to the upper side of the substance to be extracted depending on the property of the substance to be extracted,
The inner cylinder is positionally fixed to the other fixing position on the inner bottom of the container main body, and the lid is mounted on the upper part of the container main body. The discharge passage of the lid communicates with the inner cylinder and the introduction passage is inside the container main body. When communicating with an excess space other than the cylinder, the supercritical fluid introduced from the introduction flow path descends through the excess space and flows into the ventilation space from the opening at the lower end of the inner cylinder, and the inflowing supercritical fluid The fluid rises in the inner cylinder from the ventilation space through the communication part with the filter, passes through the substance to be extracted, and is discharged from the upper part of the inner cylinder to the outside of the extraction container through the discharge passage of the lid.

[0015]

Embodiments of the present invention will be described below with reference to the drawings.

1 to 3 show an embodiment of an extraction container of a supercritical fluid extraction / separation apparatus of the present invention, in which 1 denotes an inner cylinder for accommodating a substance to be extracted 2, and said inner cylinder Bottom of 1 '
Has a raised bottom so as to ensure an appropriate ventilation space 3 at its lower part, and a communication part 4 with a filter is provided at the center thereof. Furthermore, an opening 5 is formed at the lower end of the inner cylinder 1 to open the ventilation space 3 to the outer periphery of the lower end.

Reference numeral 6 denotes a relatively large surplus space 7 for the inner cylinder 1.
2 shows a container body having an upper opening capable of being housed, and the inner cylinder 1 can be selectively fixed to two different fixing positions 8 and 9 on the bottom surface of the container body 6 as shown in FIG. A guide portion 10 having a shape is formed.

Reference numeral 11 denotes a lid body capable of simultaneously opening and closing the upper portion of the container body 6 and the upper portion of the inner cylinder 1 which is fixedly held at one fixing position 8 on the inner bottom portion of the container body 6.
At the center of the lower surface of the container, a fitting convex portion 12 that fits into the inner peripheral portion of the container body 6 is provided in a protruding manner, and the lower surface of the fitting convex portion 12 can close the upper portion of the inner cylinder 1. There is. Further, the lid 11, CO ₂ from the interior of the extraction vessel at the introduction channel 13 and the other fixed position 9 above leads to CO ₂ from the outside to the inside of the extraction vessel at one fixed position 8 above the outside A discharge flow path 14 for discharging is discharged.

Reference numeral 15 is a sealing material, and 16 is the lid 11.
A bolt for attaching and detaching the container to and from the container body 6 is shown.

Thus, as shown in FIG. 1, the inner cylinder 1 accommodating the substance to be extracted 2 is fixed at one fixed position 8 on the inner bottom of the container body 6.
When the lid 11 is attached to the upper part of the container body 6 and is fixed to the upper part of the container body 6, the lower surface of the fitting convex portion 12 of the lid body 11 is pressed against the upper end of the inner cylinder 1 in the container body 6 and the upper part of the container body 6 and the inner cylinder 1 upper part And are closed at the same time.

At this time, the introduction flow path 13 of the lid 11 communicates with the inner cylinder 1 fixed at the one fixed position 8 and the discharge flow path 14 is a surplus portion other than the inner cylinder 1 in the container body 6. It communicates with the space 7.

From the introduction flow path 13 to the supercritical state C
When O ₂ is introduced, the CO ₂ descends in the inner cylinder 1 and passes through the substance to be extracted 2, and the soluble substance (extract) in the substance to be extracted 2 is extracted to cause the communication portion 4 with a filter. Passing through and flowing out of the ventilation space 3 into the surplus space 7 in the container body 6 through the opening 5,
The excess space 7 is discharged to the outside of the extraction container through the discharge passage 14 of the lid 11.

When it is desired to pass CO ₂ from the lower side to the upper side of the substance to be extracted 2 depending on the properties of the substance to be extracted 2,
As shown in FIG. 3, the inner cylinder 1 is fixed to the other fixing position 9 on the inner bottom portion of the container body 6 and the lid body 11 is attached to the upper part of the container body 6 so that the discharge flow passage 14 of the lid body 11 is 1 and the introduction channel 13 communicates with the excess space 7 other than the inner cylinder 1 in the container body 6, CO ₂ introduced from the introduction channel 13 descends through the excess space 7 and CO ₂ flows into the ventilation space 3 through the opening 5 at the lower end of the cylinder 1 and flows into the ventilation space 3.
Goes up from the ventilation space 3 through the communication part 4 with the filter to the inside of the inner cylinder 1 to pass the substance to be extracted 2, and from the upper part of the inner cylinder 1 to the outside of the extraction container through the discharge flow path 14 of the lid 11. Is discharged.

Therefore, according to the above embodiment, the CO ₂ introduction direction can be switched very easily by appropriately changing the fixing position of the inner cylinder 1 in the container body 6, so that the flow path is switched to the outside of the extraction container. Since it is not necessary to provide a piping system for the use, and a passage is not required to be formed on the container body 6 side that constitutes the extraction container, the manufacturing cost of the supercritical fluid extraction / separation device can be significantly reduced. ..

The extraction container of the supercritical fluid extraction / separation apparatus of the present invention is not limited to the above-mentioned embodiment, and the solvent used as the supercritical fluid may be other than CO ₂ .
Of course, various changes can be made without departing from the scope of the present invention.

[0026]

According to the extraction container of the above-described supercritical fluid extraction / separation device of the present invention, the introduction direction of the supercritical fluid can be switched very easily by appropriately changing the fixing position of the inner cylinder in the container body. Therefore, it is not necessary to provide a piping system for switching the flow path outside the extraction container, and since the flow path is not required to be formed on the container body side that constitutes the extraction container, the supercritical fluid extraction / separation device It is possible to achieve an excellent effect that the manufacturing cost can be significantly reduced.

[Brief description of drawings]

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

FIG. 2 is a view taken along line II-II in FIG.

FIG. 3 is a cross-sectional view showing a state in which the CO ₂ introduction direction in FIG. 1 is switched.

FIG. 4 is a schematic view showing an example of a conventional supercritical fluid extraction / separation device.

5 is a cross-sectional view of the extraction container of FIG.

6 is a cross-sectional view showing a state in which the CO ₂ introduction direction in FIG. 5 is switched.

[Explanation of symbols]

 1 Inner cylinder 1'Bottom part 2 Extracted substance 3 Ventilation space 4 Communication part with filter 5 Opening part 6 Container body 7 Excess space 8 Fixed position 9 Fixed position 10 Guide part 11 Lid body 13 Introduction flow path 14 Discharge flow path

Claims (1)

[Claims] 1. An inner cylinder for storing a substance to be extracted, which has a communication part with a filter at a bottom part raised to secure a ventilation space at a lower part and an opening part for opening the ventilation space to the outer periphery of the lower end at a lower end. And a container body with an upper opening having guide portions formed on the bottom surface that can fix the inner cylinder at two different positions,
It is possible to simultaneously open and close the inner cylinder upper part and the container main body upper part fixed in either one of the two fixed positions and accommodated in the container main body, and above each of the two fixed positions when closed. An extraction container of a supercritical fluid extraction / separation device, comprising: a lid body having an introduction passage and a discharge passage that communicate with the inside of the container body.