KR0168509B1 - Extraction device for fluid flowing in axial direction - Google Patents

Abstract

An axial flow fluid extraction device capable of shortening the processing time, increasing the processing capacity by reducing dead space, equalizing the extraction rate by securing the uniformity of the fluid flow, and reducing the cost by rationalizing the processing and maintenance. to provide.

To fit the cylindrical body 2 having the upper opening portion 10A and the lower opening portion 10B and the upper and lower openings 10A and 10B to allow the object 9 to enter and exit, respectively. The pressure container 1 is formed by the upper lid 3A and the lower lid 3B, and the fluid introduction openings 5A and 5B are provided near the upper and lower ends of the main body 2, respectively. In the main body 2, the upper filter 4A and the lower filter 4B are interposed between the workpiece 9 to be filled and the respective fluid inlet and exit ports 5A and 5B, respectively, and the upper filter ( 4A is integrally fixed to the upper lid 3A and the lower filter 4B to the lower lid 3B, respectively.

The fluid extraction fluid introduced from one fluid outlet 5A flows in the axial direction of the body 2 with respect to the workpiece 9 directly filled in the body 2 and the other fluid outlet 5B. It consists of an axial flow direct filling fluid extraction device which is derivable.

Description

Axial Flow Fluid Extractor

The present invention relates to a fluid extraction device for extracting certain substances from solid materials such as natural materials and ceramics, and a fluid extraction apparatus adapted to direct filling of axial flow, which is suitably used for a supercritical fluid extraction apparatus.

In recent years, a fluid extraction device using a supercritical fluid for extracting a desired component (hereinafter referred to as a solvent) from a to-be-processed object has been in the spotlight, and is disclosed in Japanese Patent Laid-Open No. 6-63307 as this typical prior art. There is a device.

The outline of the structure of the prior art is as follows. As shown in FIGS. 1 and 5 of the publication, the outer container 10, which is a pressure container, and the inner container 22 inserted into the outer container 10, comprises an upper filter 24, In the inner container 22 provided with the lower filter 26, the periphery of a filter is fixed to the annular filter attachment member 34 attached to the container edge part, and the caught part 42 is attached to the filter attachment member 34. On the other hand, the inner container 22 is provided with a catching portion 40, and by the hooking or peeling operation of the caught portion 42 and the catching portion 40, the filter for the inner container 22 It is designed to be easy to attach and detach (24, 26).

By the way, the fluid extracting device consisting of such a double container: ① when removing the inner container from the outer container, when the container is inserted in reverse, the lid opening and closing of the outer container and the lid opening and closing for the entry and exit of the object from the inner container. Therefore, in the preparation step of the extraction process, a lot of effort and effort are wasted, and the time for the preparation process is long, and the pretreatment time is delayed, which leads to a decrease in processing capacity. (2) Since the inner container is moved in and out of the outer container each time, the guide member is required at the lower part of the inner container so that the inner surface of the outer container is not damaged by the inner container. As a result, the filling amount of the processed material decreases, and as a result, the processing capacity decreases. ③ When extraction is performed using a supercritical fluid, the viscosity loss of the filter and the filling part of the processing object is small because the viscosity is smaller than that of general liquid extraction. For example, since it is easy to be affected by the shape of the upper fluid inlet part, the flow becomes uneven, and an extraction distribution occurs in the treated object, and ④ each time, the inner container is moved in and out of the outer container. The wear of the sealing material between the inner container and the outer container is severe, the frequency of seal replacement is increased, and the maintenance and repair can not be avoided. There is a problem to be solved in this regard.

The present invention has been made to solve such a problem, and an object of the present invention is to shorten the processing time, increase the processing capacity by reducing dead space, equalize the extraction rate by securing the uniformity of the fluid flow, It is an object of the present invention to provide an axial flow fluid extraction device capable of reducing costs due to rationalization of processing and maintenance, in particular a fluid extraction device adapted to direct filling of axial flow, which is suitably used for a supercritical fluid extraction device.

1 is a schematic structural diagram showing a supercritical fluid extraction apparatus according to a first embodiment of the present invention.

2 is a structural diagram of an essential part schematically showing a supercritical fluid extraction device according to a second embodiment of the present invention.

3 is a structural diagram of an essential part schematically showing a supercritical fluid extraction device according to a third embodiment of the present invention.

4 (a) is a structural diagram of a principal part schematically showing a supercritical fluid extraction device according to a fourth embodiment of the present invention. (b) is sectional drawing seen from the A-A line | wire in FIG.4 (a).

5 is a structural diagram of a main part schematically showing a supercritical fluid extraction device according to a fifth embodiment of the present invention.

6 (a) is a structural diagram of a principal part schematically showing a supercritical fluid extraction device according to a sixth embodiment of the present invention. (b) is sectional drawing seen from the B-B line | wire in FIG.

7 (a) is a structural diagram of a principal part schematically showing a supercritical fluid extraction device according to a seventh embodiment of the present invention. (b) is sectional drawing seen from the C-C line | wire in FIG.7 (a).

Figure 8 (a) is a structural diagram of a principal part schematically showing a supercritical fluid extraction device which is a comparative example to the embodiment of the present invention. (b) is sectional drawing seen from the D-D line | wire in FIG.8 (a).

9 is an overall structural diagram schematically showing a supercritical fluid extraction device according to an eighth embodiment of the present invention.

10 is a structural diagram of a main part schematically showing a supercritical fluid extraction device according to a ninth embodiment of the present invention.

FIG. 11 is a structural diagram of an essential part schematically showing a supercritical fluid extraction device according to a tenth embodiment of the present invention. FIG.

12 is a conceptual diagram of a supercritical fluid extractor.

FIG. 13 is a pressure loss ratio-nonuniform ratio relationship diagram in the extractor shown in FIG.

* Explanation of symbols for main parts of the drawings

1: Pressure vessel 2: Body

3A: Upper lid 3B: Lower lid

4A: upper filter 4B: lower filter

5A: Upper fluid outlet 5B: Lower fluid outlet

6A: Upper seal member 6B: Lower seal member

7A: Upper seal member 7B: Lower seal member

8: fixing member 9: workpiece

10A: upper opening 10B: lower opening

11: obstruction plate 12: cover

13: receiving hopper 14: receiving hopper

15: filter cover

This invention is set as the structure demonstrated below in order to achieve the said objective. That is, according to the invention of claim 1, the pressure is provided by a cylindrical main body having upper and lower ends opened to stand up the workpiece, and an upper lid and a lower lid fitted to the two openings so that liquid does not penetrate the respective openings. The fluid inlet is formed in the container, and the fluid inlet is provided in one of the upper and lower lids near the upper and lower ends of the body, respectively, while the upper filter is interposed between the object to be filled and the respective fluid inlet. And an axial flow direct filling type in which a lower filter is formed, respectively, and fluid introduced from one fluid inlet port flows in the axial direction of the body with respect to an object to be directly filled in the body and is drawn out of the other fluid inlet port. In the fluid extraction device, the upper filter is characterized in that the lower filter is integrally fixed to the lower lid, respectively do.

In addition, according to the second aspect of the present invention, a lid and a filter corresponding to one of the fluid inlet and outlet of the fluid inlet are gradually narrowed toward the far side from the side close to the fluid inlet in the positions of the upper and lower sides of the fluid inlet. In a row facing each other, according to the invention of claim 3, a lid and a filter corresponding to one fluid inlet and outlet on the fluid inlet side are arranged so as to have a substantially constant spacing at the upper and lower sides of the fluid inlet and outlet. It is provided face to face, and according to the invention of claim 4, the filter is formed so as to gradually increase the filter resistance from the side closer to the fluid inlet and toward the far side.

According to the invention of claim 5, one fluid inlet and outlet on the fluid introduction side is formed in the shape of a trumpet having a maximum diameter of an opening facing the inside of the main body, and according to the invention of claim 6, one fluid inlet and outlet on the fluid introduction side is In the circumferential direction of the main body, a plurality of them are provided, and according to the invention of claim 7, the fluid inlet and outlet is located at a position facing one fluid inlet and the fluid inlet side between the cap and the filter, which face each other in a parallel shape. A baffle is provided to disperse the fluid introduced therefrom. In addition, according to the invention of claim 8, the filter has a filter pressure loss in the range of 300 to 3000 Pa, and in the invention of claim 9, the seal is provided around the lid and the filter which are integrally provided in a face to face. A protective cover is installed.

According to the invention of claim 10, the pressure vessel includes a cylindrical main body having upper and lower ends opened to enter and exit the object, and an upper lid and a lower lid fitted to each of the openings so as not to infiltrate the liquid. And a fluid inlet opening is formed in each of the upper lid and the lower lid near the upper and lower ends of the main body, respectively, while the upper filter and the upper filter are interposed between the object to be filled and the respective fluid inlet openings. The lower filter is formed in each of the axial flow fluid extraction devices which can be drawn from the other fluid inlet and flow out in the axial direction of the main body with respect to the object to be directly filled in the body. The end fitting cylinder in which the main body inside makes at least one inner diameter of the said opening part larger than the inner diameter of the to-be-processed object filling part. The lid is formed in the shape of a large diameter portion in which the fluid inlet and outlet is provided, while one filter corresponding to the fluid inlet is formed in a ring shape, and is fitted to the end wall portion of the opening and the opening. In this case, the axial flow fluid extraction device according to any one of the above-mentioned claims is provided at the time of discharging the object to be treated. In extracting the lower lid which is fitted to the main body, the receiving hopper is inserted between the lower part of the main body and the lower lid and stops the object to be processed.

According to the apparatus of claim 1, the apparatus is a method of directly filling an object to be treated with a pressure vessel, which is compared with an internal container filling method in which a conventional inner container is filled into an outer container of an extraction apparatus. Handling is significantly simplified.

According to this apparatus, since the upper filter and the lower filter corresponding to the upper lid and the lower lid in the conventional inner container are integrated in the upper lid and the lower lid as the outer container, respectively, the filling and discharging of the object to be treated are It can be done simply and quickly by just putting together the lid and the lower lid, and at the same time, the space in the pressure vessel can be effectively used with a minimum of dead space.

According to the apparatus of claim 2, the lid and the filter corresponding to one fluid inlet and outlet on the fluid inlet side are spaced apart from the side close to the fluid inlet in the up and down positions at which the fluid inlet and outlet are fitted. By confronting in the form of a gradually narrowing uneven shape, the flow rate of the fluid introduced from the fluid inlet and reaching the filter can be made substantially constant over the front of the filter to eliminate the pressure distribution. Uniform flow is obtained.

In addition, according to the apparatus of claim 3, the cap and the filter corresponding to one fluid inlet and outlet on the fluid inlet side face each other in a parallel shape with a substantially constant spacing at positions on the upper and lower sides of the fluid inlet and outlet. Since the device can be constructed in a symmetrical step around the axis, the device is not directional, easy to assemble, and simple in structure for the assembly of the lid and the filter to the main body.

According to the apparatus of claim 4, the filter is formed so as to gradually increase the filter resistance toward the far side from the side close to the fluid inlet port, thereby adjusting the pressure loss of the packing part of the object to be processed including the filter, so that the fluid inlet port (fluid inlet) The pressure distribution of the part can be relaxed, and as a result, a uniform flow is obtained with respect to the workpiece.

Further, according to the apparatus of claim 5, one of the fluid introduction openings on the fluid introduction side is formed in a trumpet shape with the maximum opening of the opening facing the inside of the main body, and according to the device of claim 6, one of the fluid introduction openings A plurality of fluid inlets and outlets are arranged in a circumferential direction of the main body, and according to the apparatus of claim 7, between the cap and the filter, which are installed to face each other in a parallel shape, at a position facing one of the fluid inlets on the fluid inlet side. And a baffle plate for dispersing the fluid introduced from the fluid inlet and outlet is provided. According to the apparatus having each of these structures, the flow rate of the fluid introduced from the fluid inlet and reaching the filter can be substantially constant over the entire surface of the filter, thereby eliminating pressure distribution, and providing a uniform flow to the workpiece. Is obtained.

In addition, according to the apparatus of claim 8, by using a filter having a filter pressure loss in the range of 300 to 3000 Pa, it is possible to eliminate the variation in extraction rate with respect to the workpiece.

According to the apparatus of claim 9, a cover for protecting the seal portion is provided around the lid and the filter which are integrally provided in a face to face, and thus the protection of the seal portion of the lid and the filter is ensured, and the opening and the fluid inlet and outlet of the pressure vessel body are completed. Accumulation of the object to be treated is prevented.

Further, according to the axial flow fluid extraction device of claim 10, the main body portion is formed in an end-fitting cylindrical shape having an inner diameter of at least one of the openings larger than that of the filling part of the workpiece, and the fluid inlet and outlet portion is formed in the large diameter portion. While the filter is formed in a ring shape, the filter is fitted into the lid and the end wall of the opening, and the filter is installed and fixed inside the fluid inlet. In the state, filling of the object to be processed is performed without any trouble, and workability is good, and wear of the sealing material corresponding to the filter can be reduced.

In addition, when the surface of the apparatus of claim 11 is discharged from the surface, the front and rear lids of the main body are pulled back and forth between the lower part of the main body and the lower lid to stop the object. By setting up the receiving hopper, the work efficiency can be improved without scattering the processing object around the lower lid during discharge.

EXAMPLE

EMBODIMENT OF THE INVENTION Hereinafter, each Example of this invention is described, referring an accompanying drawing.

1, the overall structure of the supercritical fluid extraction device according to the first embodiment of the present invention is schematically shown. Reference numeral 1 denotes a vertical pressure vessel, which includes a metal main body 2 serving as a shell of an extraction device, a metal upper lid 3A, and a metal lower lid 3B. In the pressure vessel 1, the solid workpiece 9 is filled in a predetermined amount. The main body 2 is formed of a cylindrical body, for example, a cylindrical body, whose upper and lower ends are opened, and allows the object to be processed to enter and exit from these upper and lower openings 10A and 10B.

On the other hand, the upper lid 3A and the lower lid 3B are formed on a half body of an end-fitting structure having a large diameter portion and a small diameter portion in the same shaft, for example, an end-shaped disk having the same shape, and each small diameter portion is formed. The upper and lower lids 3A and 3B are inserted into the upper and lower portions of the main body 2 by being inserted into the upper opening portion 10A and the lower opening portion 10B so as not to penetrate through the sealing member 6A and 6B for the lid. By fitting so that liquid does not penetrate with respect to both ends, in this way, the main body 2 and the upper and lower lids 3A and 3B are integrally combined, and a pressure vessel is formed.

The main body 2 is provided with fluid inlets 5A and 5B at positions near the upper and lower ends thereof, respectively. The fluid introduction openings 5A and 5B are provided in the shape of a long hole through the cylinder body at a position close to the inside of the main body, avoiding the fittings of the upper and lower lids 3A and 3B. Meanwhile, the upper filter 4A and the lower filter 4B are integrally fixed to the upper lid 3A and the lower lid 3B, respectively. The upper filter 4A and the lower filter 4B are formed on a flat body, for example, a disk of the same shape, and the annular sealing material 7A and the sealing material 7B are attached to the periphery at the same time. The upper lid 3A and the lower lid 3B are fixed to the inner end portions of the upper lid 3A and the lower lid 3B by a plurality of fixing members 8 serving as spacers, so that in the example shown in FIG. It is fixed integrally by the arrangement | positioning which faced in parallel shape which kept constant space | interval with respect to the inner end surface part of 3B).

The upper lid 3A and the upper filter 4A, and the lower lid 3B and the lower filter 4B, which are integrally formed as described above, have the upper lid 3A and the lower lid 3B as the main body 2. The upper lid 3A and the lower lid 3B are arranged in parallel to each other in the up-down direction with the fluid inlet openings 5A and 5B interposed therebetween. The upper filter 4A and the lower filter 4B serve as the upper portion of the main body 2 while the upper openings 10A and 10B of the main body 2 are closed to function as an outer lid for maintaining the inner portion of the main body so that no liquid penetrates. It is erected horizontally in the lower part and the lower part, and is held close to the inner wall of the main body 2 with the sealing member 7A and the sealing member 7B interposed therebetween, thereby accommodating the object 9 in the main body 2. It functions as a partition member for forming a space. Further, in the first embodiment, the filter cover 15 is covered with at least one end of the fluid inlet 5A, 5B, for example, in the inlet of the inner side of the main body at the fluid inlet 5A which becomes the fluid inlet side. ), And the filter cover 15 is provided to prevent the deposition of blood to be deposited at the fluid inlet 5A so that clogging occurs.

1 shows an embodiment of the extraction operation in the apparatus shown in the drawing, the lower lid 3 is set on the main body 2, and the solid workpiece (with the upper opening 10A open) ( 9) is fed directly into the body 2. In this case, the workpiece 9 is deposited on the lower filter 4B. Subsequently, the upper lid 3A and the upper filter 4A, which are integrated, are lowered by a lifting device such as a crane and set at the upper opening 10 of the main body 2. In this state, the supercritical fluid is introduced into the main body 2 from the upper fluid inlet 5A, so that the supercritical fluid passes through the upper filter 4A to the layer of the workpiece 9 immediately below. It transfers and the desired substance contained in the to-be-processed object 9 fuse | melts with the supercritical fluid. The supercritical fluid flows down the inside of the object 9 to pass through the lower filter 4B, passes the gap between the lower filter 4B and the lower lid 3B, and passes the lower fluid inlet and outlet ( 5B) is drawn outside of the main body 2.

As described above, in this apparatus, it is only necessary to perform the operation of putting the upper lid 3A and the upper filter 4A integrated into the main body 2 only once in each extraction operation. In addition, since the filling and direct discharging method is used instead of the inner container method, and the lid and the filter have a compact integrated structure, the dead space is extremely narrowed for the filling of the object 9 and the main body 2 Effective use of is planned.

2 is a structural diagram of an essential part schematically showing a supercritical fluid extraction device according to a second embodiment of the present invention. The second embodiment is similar to the first embodiment described above, and corresponding members are assigned the same reference numerals. The same reference numerals are given to the corresponding members in the same manner for the respective examples after the third embodiment to be described later.

In the embodiment shown in FIG. 2, the upper lid 3A and the upper filter 4A, which are provided in correspondence with the upper fluid outlet portion 5A on the fluid introduction side, are provided with the fluid inlet 5A. It is a characteristic that it is the structure arrange | positioned so that it may face in an unbalanced shape which gradually narrows the space | interval toward the far side from the side near this fluid introduction opening 5A in the up-and-down both sides to fit. Specifically, as shown in the drawing, the lower surface of the upper lid 3A is formed in a tapered plane that slopes toward the far side from the side close to the fluid inlet 5A, while the upper filter 4A is It is arranged to be arranged in a horizontal shape.

In the second embodiment of this structure, the space portion as the supercritical fluid chamber formed between the upper lid 3A and the upper filter 4A is directed toward the far side from the side close to the fluid inlet 5A. Since the passage cross-sectional area is gradually reduced, the flow rate of the supercritical fluid reaching the front surface of the upper filter 4A from the fluid inlet 5A is made substantially constant, and as a result, the pressure-reduced object 9 A uniform flow of fluid flowing through the layer can be obtained. An example that achieves the same effect as the second embodiment is schematically shown in FIG. 3 as the third embodiment. In the third embodiment, the upper lid 3A provided corresponding to the upper fluid introduction opening 5A to be the fluid introduction side maintains the lower surface in a flat horizontal state while being fitted to the main body 2. On the other hand, the upper filter 4A is unevenly attached to the upper lid 3A so that the upper filter 4A becomes a tapered plane that slopes from the side close to the fluid introduction opening 5A toward the far side. In this configuration, a uniform flow of the fluid flowing through the layer of the object 9 can be obtained.

Fig. 4 (a) is a schematic structural view of the supercritical fluid extraction device according to the fourth embodiment of the present invention, and in Fig. 4 (b), a cross section taken along the line AA in Fig. 4 (a) is shown, respectively. Is shown.

This fourth embodiment is characterized by the structure of the upper filter 4A provided in correspondence with the fluid inlet 5A on the upper side to be the fluid inlet side, and the filter toward the far side from the side close to the fluid inlet 5A. It is formed to gradually increase resistance. Specifically, the disk-shaped filter is composed of a combination of three parts of the side 4A1, the center side 4A2, and the far side 4A3 close to the fluid inlet 5A, and the mesh of the filter medium is coarse on the side 4A1. The thin ones, the center side 4A2 are the middle rough ones, and the far side 4A3 are the dense ones. By configuring in this way and changing the pressure loss in a filter part three steps, it is possible to make uniform the flow of the supercritical fluid which reaches the front surface of the upper filter 4A from the fluid introduction opening 5A. That is, since it is difficult for the fluid to flow smoothly near the fluid inlet 5A, it is preferable to reduce the filter resistance at the inlet.

Moreover, it is preferable to employ | adopt that a filter resistance is large as a whole as a filter provided corresponding to 5 A of upper fluid introduction openings which become a fluid introduction side. By doing so, it is possible to obtain a uniform flow of the fluid flowing through the layer of the object 9 by largely reducing the pressure loss of the filling portion of the object 9 including the filter.

5 schematically shows the structure of the main part of the supercritical fluid extraction apparatus according to the fifth embodiment of the present invention. The fifth embodiment is characterized in that the upper fluid introduction port 5A on the fluid introduction side is formed in a trumpet shape with the maximum opening opening facing the inside of the main body. That is, as illustrated in FIG. 5, the fluid inlet 5A curves the inner wall on the R surface toward the inlet edge at the opening side facing the inside of the main body, so that the lower surface and the upper filter 3A of the upper lid 3A ( It has almost expanded to the upper surface of 4A). Since the fluid inlet 5A is widened in the shape of a trumpet, the fluid inlet 5A smoothly diffuses into the supercritical fluid flowing from the fluid inlet 5A to the front surface of the upper filter 4A, thereby achieving a uniform flow. It is possible.

6 (a) is a structural diagram of a principal part of a schematic diagram of a supercritical fluid extraction device according to a sixth embodiment of the present invention, and FIG. 6 (b) is seen from the line BB in FIG. 6 (a). The cross section of the time is shown respectively. This sixth embodiment is characterized in that the upper fluid introduction port 5A on the fluid introduction side is provided with a plurality of distributing in the circumferential direction of the main body 2. Specifically, as shown in FIG. 6 (b), four fluid introduction ports 5A of the same structure are provided in an arrangement which is divided into four in the circumferential direction of the main body 2. By providing a plurality of the fluid inlet and outlet 5A in this way, it is possible to balance the flow of the supercritical fluid reaching the front surface of the upper filter 4A and achieve a uniform flow.

Fig. 7 (a) is a structural diagram of a principal part of a schematic illustration of the supercritical fluid extraction device according to the seventh embodiment of the present invention, as shown in Fig. 7 (b) when viewed from the line CC in Fig. 7 (a). Each of the cross sections of is shown. This seventh embodiment is interposed between the upper lid 3A and the upper filter 4A located on both upper and lower sides of the upper fluid inlet 5A on the fluid inlet side and facing the fluid inlet 5A. It is characterized by the fact that the plate 11 is provided with a structure. The obstruction plate 11 receives the supercritical fluid introduced from the fluid inlet and outlet 5A at the front end, and serves to disperse the flow in both the left and right sides thereof. Specifically, as shown in the figure, the obstruction plate 11 formed in the shape of a bullet cone is disposed so that the tip of the horn faces close to the opening of the fluid introduction opening 5A. The second impingement plate 11 reaches the front surface of the upper filter 4A while the fluid diffuses between the upper lid 3A and the upper filter 4A as in the streamline of FIGS. 7A and 7B. It is possible to balance the flow of the critical fluid to achieve a uniform flow. Compared with the extraction apparatus listed as a comparative example for this seventh example producing a streamline as shown in Figs. 8A and 8B, a larger bacteriostatic effect is achieved, and the initial purpose is sufficiently achieved. Not to mention that.

By the way, the filter 4 provided on the fluid inflow side needs to be sufficiently considered so as not to cause an obstacle in terms of making the material extraction rate with respect to the layer of the to-be-processed object 9 uniform. For this purpose, the pressure loss of the fluid inlet side filter is preferably 300 Pa or more and 3000 Pa or less. This will be described with reference to the drawings below. In general, when a fluid slows down due to expansion of a flow path, the velocity energy is converted into pressure energy. This pressure energy is proportional to the square of the rate of conversion and the density of the fluid.

Although a conceptual diagram of a supercritical fluid extractor is shown in FIG. 12, the possibility of pressure distribution by deceleration at the top of the extractor into which fluid is introduced is considered. In addition, the pressure loss and filter pressure loss of the packed bed are proportional to the roughness of the filter, the flow rate, and the viscosity of the fluid. Since the fluid flow rate distribution in the packed bed is determined by the pressure distribution, if a large pressure distribution is attached at the top of the extractor, the flow rate to the packed bed varies depending on the location, but if the pressure loss of the filter or the like is increased with respect to the pressure distribution, The pressure difference is negated so that the flow rate becomes approximately constant.

In general, supercritical fluid extraction is compared and examined for liquid solvent extraction performed as extraction. Supercritical fluids are characterized by a similar density and very low viscosity compared to liquids. For this reason, in the supercritical fluid extraction, since the density is about the same as that of the solvent extraction, the pressure distribution in the upper part of the extractor is considered the same, but the pressure loss of the packed bed and the pressure loss of the filter are small because of the small viscosity. Therefore, it is thought that in supercritical fluid extraction, pressure distribution is more likely to occur than solvent extraction, and nonuniformity due to the place of extraction rate is likely to occur due to the occurrence of flow rate distribution. Where the flow rate is large, the extraction rate becomes large quickly, and when it is small, the extraction rate becomes small. Non-uniformity of this extraction rate is undesirable in terms of product quality. For these reasons, it is necessary to carefully consider the generation of pressure distribution in the supercritical fluid extraction rather than liquid solvent extraction.

The pressure distribution in the supercritical fluid extraction device is summarized below. For the extractor, the ratio of the pressure difference in the upper part and the pressure loss in the packed bed and the volume ratio in which the extraction ratio is non-uniform in the packed bed are summarized as shown in FIG. As is apparent from this figure, it can be seen that the extraction ratio distribution hardly occurs when the pressure ratio is one or more.

In the supercritical fluid extraction device, the filter pressure loss on the packed bed, especially the inflow side, is 300 Pa or more so that the pressure ratio is 1 or more, and the suitable range is 300 to 3000 Pa.

9 is a schematic structural diagram of a supercritical fluid extraction apparatus according to an eighth embodiment of the present invention. In the eighth embodiment, the internal structure of the upper opening 10A of the main body 2 has an end-cylinder shape, and the upper filter 4A has a ring shape. Specifically, the upper fluid introduction port 5A is formed in an end-fitting cylindrical shape in which the inner diameter of the upper opening 10A is larger than the inner diameter of the object 9 to be filled, and becomes the fluid introduction side in this large diameter portion. ), While the upper filter 4A is formed in a ring shape like a cylinder cut into a circle. The upper filter 4A is fitted inside the upper fluid introduction opening 5A by being fitted with the short wall portion of the upper opening portion 10A and the upper lid 3A fitted to the opening, and the upper filter 4A is installed inside the upper lid 3A. It is fixed to). In this eighth embodiment, the upper filter 4A may be set at a place where the insertion of the object 9 is not impeded before the object 9 is filled. The wear of the ashes 6A and 7A is low.

10 is a structural diagram of a main part schematically showing a supercritical fluid extraction device according to a ninth embodiment of the present invention. This ninth embodiment is characterized by a structure in which a cover 12 for protecting the seal portion is provided around the lower lid 3B and the lower filter 4B, which are integrally provided to face each other. The cover 12 is formed of a cylindrical body with a jaw having a cylindrical portion 12A and a jaw portion 12B integrally, and the jaw portion 12B follows an upper circumferential edge of the lower lid 3B, A cylindrical portion 12A is installed to surround the lower filter 4B and the lower lid 3B. With respect to the ninth embodiment of such a structure, the sealing material 6B is protected and at the same time, the accumulation of the workpiece 9 at the upper surface and the lower fluid introduction opening 5B of the lower lid 3B can be prevented. Have

Further, in this embodiment, the receiving hopper 14 made of, for example, a metal plate is annularly arranged on the outer circumference of the large diameter portion of the lower lid 3B, and the lower lid 3B is also used as a workpiece receiver. If the lower lid 3B is peeled off from the lower opening 10B of the main body 2 at the time of discharge of the workpiece 9, the workpiece 9 does not scatter around the lower lid 3B. It is structured to be able to prevent it.

In FIG. 11, the structure of the principal part of the supercritical fluid extraction device concerning the tenth embodiment of the present invention is shown schematically. This tenth embodiment is characterized by a structure in which the receiving hopper 13 is attached to the lower lid 3B and the lower filter 4B. That is, as a specific structure, it is a receiving plate state formed, for example by cut | disconnecting and installing in the predetermined place the notch groove in which the fixing member 8 fits in the metal plate which is substantially equal to the outer diameter of the cylindrical main body 2. The receiving hoppers 13 move forward and backward with each other in pulling down the lower lid 3B fitted to the main body 2 at the time of discharge of the object 9, as shown in FIG. It is inserted into the gap between the lower part of the main body 2 and the lower lid 3B at an oblique angle, and sandwiched between the lower lid 3B and the lower filter 4B. By inserting in this way, the to-be-processed object 9 which falls from the lower opening part 10B can be guide | induced and guide | induced to the receiving hopper 13, and the to-be-processed object 9 is provided around the lower lid 3B. It can prevent scattering. 16 is a seal material cover for protecting the seal material 6B.

In each of the embodiments described above, the supercritical fluid is introduced from the upper fluid inlet and outlet 5A to the pressure vessel 1 including the main body 2 and the upper and lower lids 3A and 3B, and the lower fluid inlet and outlet is introduced. Although the structure is derived from (5B), the present invention is not limited to such a structure, and conversely, the supercritical fluid is introduced from the lower fluid inlet 5B and the structure is derived from the upper fluid inlet 5A. It goes without saying that the present invention is not limited to the supercritical fluid extraction device, but can be applied to the device for extracting the solvent from the solid by other liquids.

As described above, the present invention is a device for directly filling an object to be treated with a pressure vessel, which is compared with an inner container filling method for filling a container with an inner container filled with a conventional container. Handling is significantly simplified.

According to the apparatus of claim 1, in the conventional inner container, since the upper filter and the lower filter corresponding to the upper lid and the lower lid are integrated in the upper lid and the lower lid as the outer container, respectively, the filling and discharging of the object to be treated is It is possible to increase the processing capacity by shortening the processing time by simply and quickly removing the upper and lower lids, and the space in the pressure vessel can be effectively used with a minimum dead space. have. Further, according to the apparatus of claim 2, the gap corresponding to the fluid introduction port on one side of the fluid introduction port and the filter are gradually moved toward the far side from the side close to the fluid introduction port at the positions of the upper and lower sides of the fluid introduction port. By confronting in the form of narrowing unevenness, the flow rate of the fluid introduced from the fluid inlet and reaching the filter can be substantially constant over the entire surface of the filter, thereby eliminating the pressure distribution. One flow can be secured.

According to the apparatus of claim 3, the cap and the filter corresponding to one fluid inlet and outlet on the fluid inlet side face each other in a parallel shape with substantially constant spacing at the positions of the upper and lower sides of the fluid inlet and outlet. With this configuration, the device can be constructed in a symmetrical structure around the axis, whereby the assembly of the lid and the filter with respect to the main body is not directed, is easy to assemble, and the structure is simplified.

According to the apparatus of claim 4, the filter is formed such that the fluid gradually increases the filter resistance from the side close to the entrance to the far side, thereby adjusting the pressure loss of the packing part of the object to be processed including the filter, so that the fluid inlet (fluid The pressure distribution at the inlet) portion can be relaxed, and as a result, a uniform flow can be ensured with respect to the workpiece.

According to the apparatus of claim 5, one of the fluid inlet and outlet on the fluid introduction side is formed in a trumpet shape with the maximum diameter of the opening facing the inside of the main body. The fluid inlet and outlet are distributed in the circumferential direction of the main body, and are provided in plural, and according to the apparatus of claim 7, between the cap and the filter, which face each other in a parallel shape, face one fluid inlet and the fluid inlet side. In the position, a baffle plate for dispersing the fluid introduced from the fluid inlet and inlet is provided, and according to the apparatus having each of these structures, the flow velocity of the fluid introduced from the fluid inlet and reaching the filter is provided over the filter surface. It is possible to make the pressure distribution substantially constant, and to maintain a uniform flow with respect to the object to be processed.

In addition, according to the apparatus of claim 8, by using a filter having a filter pressure loss in the range of 300 to 3000 Pa, it is possible to eliminate nonuniformity in the extraction rate with respect to the workpiece. According to the apparatus of claim 9, a cover for protecting the seal portion is provided around the lid and the filter, which are integrally provided in a face to face, so that the protection of the seal portion of the lid and the filter is completed, and the opening of the pressure main body and Accumulation of the workpiece at the fluid inlet and outlet is prevented, and the improvement effect in terms of maintenance and device cost is great.

In addition, according to the axial flow fluid extraction device of claim 10, the filter is formed in a ring shape, and the filter is fitted into the opening and the end wall of the opening, which is installed and fixed inside the fluid inlet. By doing so, filling of the object to be processed in a state where the filter is attached in advance is satisfactory, and workability is good, and the wear life of the sealing material corresponding to the filter is reduced, and the service life can be extended.

In addition, according to the apparatus of claim 11, the lower lid which is fitted to the main body at the time of discharging the target object is moved back and forth to each other, and is inserted between the lower part of the main body and the lower lid to stop the object. By adopting the configuration in which the hopper is placed, the work efficiency can be improved without scattering the workpiece around the lower lid during discharge.

Claims (12)

It is formed in a pressure vessel with a cylindrical main body that opens both ends of the upper and lower ends in order to enter and exit the object, and an upper lid and a lower lid for fitting so that liquid does not penetrate the openings, respectively, the upper and lower ends of the main body The fluid inlet and outlet are respectively installed in one of the upper and lower lids adjacent to each other, while the upper filter and the lower filter are respectively interposed between the object to be filled and the respective fluid inlet and outlet. In the axial flow direct filling fluid extraction device, in which fluid introduced from one fluid inlet port flows in the axial direction of the main body with respect to a workpiece directly filled in the body, and is derived from the other fluid inlet port, the upper filter includes: Axial flow fluid extraction station, characterized in that the upper filter, the lower filter is fixed to each of the lower lid integrally . 2. The complaint of claim 1, wherein a lid and a filter corresponding to one fluid inlet on the fluid inlet side gradually narrow the gap toward the far side from the side close to the fluid inlet in the upper and lower positions of the fluid inlet. Axial flow fluid extraction device, characterized in that installed facing to the shape. A lid and a filter corresponding to one fluid inlet and outlet on the fluid inlet side face each other in a parallel shape with approximately constant spacing at positions on both the upper and lower sides of the fluid inlet and outlet. Axial flow fluid extraction device. 4. An axial flow fluid extraction device according to claim 2 or 3, wherein the filter is formed so as to gradually increase the filter resistance toward the far side from the side close to the fluid inlet. 4. An axial flow fluid extraction device according to claim 2 or 3, wherein one of the fluid introduction ports on the fluid introduction side is formed in a trumpet shape with a maximum diameter of an opening facing the inside of the main body. 4. An axial flow fluid extraction device according to claim 2 or 3, wherein a plurality of fluid inlet and outlets on one side of the fluid introduction side are disposed in a circumferential direction of the main body. The fluid introduced from the fluid inlet according to claim 2 or 3, wherein the fluid introduced from the fluid inlet is dispersed between the filter and the lid provided to face each other in a parallel shape and facing one fluid inlet on the fluid inlet side. Axial flow fluid extraction device, characterized in that the baffle plate is installed. 4. An axial flow fluid extraction device according to claim 2 or 3, wherein the filter has a filter pressure loss in the range of 300 to 3000 Pa. 4. An axial flow fluid extraction device according to claim 2 or 3, wherein a seal for protecting the seal is provided around the lid and the filter which are integrally provided in a face to face. It is formed in a pressure vessel with a cylindrical main body that opens both ends of the upper and lower ends in order to enter and exit the object, and an upper lid and a lower lid for fitting so that liquid does not penetrate the openings, respectively, the upper and lower ends of the main body One of the adjacent upper lid and the lower lid is respectively provided with the fluid inlet and outlet, while the upper filter and the lower filter are interposed between the to-be-processed object to be filled and the respective fluid inlet and outlet, respectively. An axial flow-filled fluid extraction device in which fluid introduced from one fluid inlet flows in an axial direction of the body with respect to a workpiece directly filled in the body, and is drawn out of the other fluid inlet. The inner diameter of at least one of the two openings is formed in a cylindrical shape with an end portion having a larger diameter than the inner diameter of the packing part to be processed. While the fluid inlet and outlet are provided in the neck portion, one filter corresponding to the fluid inlet and outlet is formed in a ring shape, and at the same time, the fluid is inserted into the end wall of the opening and the lid fitted to the opening. An axial flow fluid extraction device, characterized in that the interior of the doorway. The axial flow fluid extraction device according to any one of claims 1 to 3, wherein the lower lid which is fitted to the main body is pulled down from the front and rear of the main body at the time of discharge of the object to be treated. An axial flow fluid extraction device, characterized in that the receiving hopper is inserted between the lid to stop the object to be processed. 11. The axial flow fluid extraction device according to claim 10, which is inserted between the lower part of the main body and the lower lid before and after each other in pulling down the lower lid fitted to the main body when discharging the object. Axial flow fluid extraction device, characterized in that the receiving hopper is placed to stop.