JP2024009325A - Method of extracting and recovering specific substance based on liquid-liquid extraction - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method of efficiently extracting and recovering a specific substance included in a heavy liquid phase, a light liquid phase, or both phases, in a simple manner.

SOLUTION: In a liquid-liquid extraction utilizing mechanical agitation, while an agitation vane is rotated a vane part of which is located in the vicinity of an interface between a heavy liquid phase and a light liquid phase, a heavy liquid phase is sent and introduced from above a container and a light liquid phase is sent and introduced from below the container, forming areas of an emulsion mixed state and a phase separation state. The phase-separated liquid phase is introduced into a back-extraction liquid of another container, and the specific substance is extracted and recovered.

SELECTED DRAWING: Figure 1(p)

COPYRIGHT: (C)2024,JPO&INPIT

Description

The present invention relates to a method for extracting and recovering specific substances based on liquid-liquid extraction, and in particular, a heavy liquid phase (in many cases, an aqueous phase) and a light liquid phase (in many cases, an oil phase) are separated by phase mixing. By growing an emulsion phase (two-liquid emulsion mixed phase) while bringing them into countercurrent contact with each other in a container for storage, simultaneous separation of both phases (phase separation) allows It is an extraction and recovery method for specific substances to obtain specific substances that are separated and purified within a phase or within both phases.In particular, it is an emulsion phase that is stable over a wide range by efficiently mixing the heavy liquid phase and the light liquid phase. The present invention relates to a method for extracting and recovering a specific substance based on liquid-liquid extraction, by which the substance can be easily obtained.

By using liquid-liquid extraction (also called solvent extraction) to separate and concentrate target components in aqueous solutions and to separate and remove impurities from target components, high-grade metal and chemical products can be produced. (organic compounds, etc.). Liquid-liquid extraction is the separation, purification, and concentration of metal ions, organic compounds, biopolymers, etc. based on the difference in the distribution of substances between two immiscible liquid phases (e.g., water phase and oil phase). This method is widely used industrially.

Separation based on liquid-liquid extraction involves many chemical reactions, such as complexation reactions, dehydration reactions, solvation reactions, ion exchange reactions, acid-base reactions, redox reactions, catalytic reactions, and self-assembly reactions, depending on the target. reactions may be involved.

In fact, when liquid-liquid extraction is carried out industrially, a mixer-settler method is often used in which two liquid phases are mixed by rotation of a stirring blade and then transported to a separate chamber and separated by gravity. The liquid-liquid extraction mechanism based on the mixer-settler method has a relatively simple structure but provides stable performance, making it the most popular device representing industrial liquid-liquid extraction.

On the other hand, in the mechanism of the conventional mixer-settler method (hereinafter simply referred to as the conventional method), the position of the interface between the two liquid phases is likely to change, and the adjustment of the interface position requires skill. In addition, since the ratio of the liquid feeding speeds of the two liquid phases directly becomes the volume ratio of both phases participating in phase mixing (so-called O/A ratio), for example, the processing speed of the aqueous phase containing the target component (processing speed ) If it is desired to increase the liquid feeding rate of the aqueous phase in order to increase the liquid phase, the liquid feeding rate of the oil phase must also be increased at the same time, otherwise the volume ratio of both phases will change.

In the conventional method, both the aqueous phase and the oil phase are supplied from the bottom of the mixer chamber through adjacent inlets, and are supplied by a stirring blade section (blade section located at the tip of the rotating shaft) installed below the mixer chamber. The basic mechanism is that both phases are stirred and mixed immediately. In addition, a front chamber is provided at the bottom of the mixer chamber into which the aqueous phase and oil phase are introduced, and the negative pressure generated by the rotation of the stirring blades is A mechanism for mixing both phases while guiding them from the front chamber to the mixer chamber using suction is also known as a general mixer-settler device (see FIG. 3 of Patent Document 1 and Patent Document 2).

Special Publication No. 61-19281 Patent No. 6119029

When the water phase is a heavy liquid phase and the oil phase is a light liquid phase, both the water phase and the oil phase are supplied into the water phase, and the blade part of the stirring blade is inside the water phase directly above the inlet of both phases. It is located in In this way, since both phases are introduced into the aqueous phase (inside the heavy liquid phase) and immediately stirred within the aqueous phase, it is inevitable that the agitation and mixing will involve the surrounding aqueous phase. I have no choice but to. Therefore, the emulsion mixing state may be insufficient or a stable state may not be maintained over a wide range. In addition, in the type with a front chamber, the oil phase stays in the upper part of the front chamber, and sucking it up helps to increase the ratio of the oil phase, but the volume ratio of both phases actually mixed is stable. do not.

There is also a structure in which both phases are introduced from the upper part of the mixer chamber and the blade part of the stirring blade is installed in the lower part of the mixer room (see Figure 1 of Patent Document 2). Since the heavy liquid phase is placed at the bottom of the heavy liquid phase mixer chamber, the proportion of the heavy liquid phase tends to increase at the initial stage of mixing the two liquid phases.

As described above, the conventional method is such that both the heavy liquid phase and the light liquid phase are introduced from the bottom of the mixer chamber, or both phases are introduced from the top of the same chamber. In this respect, it differs from many column-type liquid-liquid extraction methods in which a heavy liquid phase is introduced from the top and a light liquid phase is introduced from the bottom. In a system in which a heavy liquid phase and a light liquid phase flow oppositely, more efficient extraction is possible due to countercurrent contact between the two phases. Conventional column-type liquid-liquid extraction methods (e.g., spray column method, pulse column method, etc.) have a lower two-liquid phase mixing capacity than mixer-settlers that use stirring blades, but on the other hand, they have a lower number of theoretical plates based on countercurrent contact of both phases. is expected to improve.

In addition, the conventional system utilizes the suction force generated by the rotation of the stirring blades for liquid feeding, so it has the advantage of being able to feed liquid without relying on a pump. In other words, the load on the pump can be significantly reduced by rotating the stirring blade, but on the other hand, the liquid feeding speed changes due to the difference in the strength of stirring of the two liquid phases (such as the difference in the rotational speed of the stirring blade). There is a problem.

Although the conventional method has a relatively simple structure and provides stable performance, it is difficult to handle due to the fact that the interface position changes easily (requiring skill to handle it), and the volume ratio of the two liquid phases that participate in phase mixing is difficult. (dependent on the ratio of the liquid feeding speeds of both phases), inefficient two-liquid phase mixing that tends to result in heavy liquid phase richness (light liquid phase deficiency), and the influence of stirring blade rotation on liquid feeding speed. There is a problem.

The purpose of the present invention is to solve the above-mentioned problems and to develop innovative characteristics that cannot be obtained by conventional methods, by allowing specific substances to be separated and purified within the heavy liquid phase, the light liquid phase, or both phases. An object of the present invention is to provide a method for producing a specific substance that enables the production of specific substances.

In the present invention, a stirring blade and both phases, a heavy liquid phase and a light liquid phase, are installed inside a container so that they have the same volume, and the blade portion of the stirring blade is separated from the interface between the two phases. a first container disposed above and below in a range within three times the thickness of the blade section; and a first container for back-extracting a specific substance from the light liquid phase sent from the first container. At least two of the second containers are prepared, and while the stirring blade is rotated and both phases are stirred by the blade portion of the stirring blade, the heavy liquid phase is lightened from above the first container from below. By feeding and introducing the liquid phase, a state where both phases are emulsified and mixed and a state where they are phase separated coexist in the first container, and the upper part of the first container is in the phase separated state. The light liquid phase present in the liquid is fed into the heavy liquid phase from below the second container containing the heavy liquid phase which is the reverse extraction liquid, and the reset light liquid obtained from the upper part of the second container is The method is characterized in that the phase is returned to the first container again, and the specific substance is recovered in the back-extraction liquid in the second container.

The following seven features can be obtained in the optimal form of the method for extracting and recovering a specific substance according to the present invention. 1) The position of the interface between the two liquid phases in the container or room is always stable without fluctuation, 2) The volume ratio of both phases participating in phase mixing can be set independently (independently) regardless of the liquid feeding rate, and 3) By efficiently mixing both phases, a stable emulsion phase (two-liquid emulsion mixed phase) can be grown over a wide range, and 4) the rotation of the stirring blade (strength of phase mixing) does not affect the liquid feeding speed. , 5) The number of theoretical plates is improved by countercurrent contact of both phases based on counter-feeding of the heavy liquid phase and the light liquid phase, and 6) Phase separation proceeds simultaneously in a container or room for mechanical stirring (mixer room). This improves phase separation, and 7) switching from liquid feeding by overflow to liquid feeding by pressure action facilitates circulating liquid feeding.

In conventional arrangements, both a heavy liquid phase (often a water phase) and a light liquid phase (often an oil phase) are introduced from the bottom of the mixer chamber. The lower part of the mixer chamber tends to become rich in the heavy liquid phase, and the two liquid phases introduced there form an emulsified mixed phase (emulsion phase) while remaining rich in the heavy liquid phase. That is, in the early stage of mixing the heavy liquid phase and the light liquid phase, the two liquid phases are emulsified and mixed with a large proportion of the heavy liquid phase. Therefore, in order to reduce this influence, the blade portion of the stirring blade is often installed directly above the inlets for both phases in the lower part of the mixer chamber. In addition, if a front chamber is provided directly below the inlet for both phases, the upper part of the front chamber will have a large proportion of light liquid phase, so by sucking it up with the suction action of the stirring blade, it will be possible to enrich the heavy liquid phase as described above. Although emulsion mixing in this state can be offset or alleviated, the ratio of the two phases sucked up is not constant, so there is a drawback that the volume ratio of the two phases being mixed is not stable.

In contrast, in the present invention, the blade part of the stirring blade for phase mixing the heavy liquid phase and the light liquid phase is moved near the interface between the two liquid phases (the rotation of the stirring blade causes the mixing of the heavy liquid phase and the light liquid phase to occur). A liquid-liquid extraction method in which a heavy liquid phase is introduced from above and a light liquid phase is introduced from below in a container or room (mixer room) in which the stirring blades are stored. By utilizing this mechanism, the phases can be mixed while the volume ratio of the heavy liquid phase and the light liquid phase present in the emulsion phase (two-liquid emulsion mixed phase) remains unchanged throughout.

The present invention solves the problems of the conventional mixer-settler method (referred to as the "conventional method") in liquid-liquid extraction using mechanical stirring, and also brings out innovative features not found in conventional methods. be.

Specifically, in the best embodiment of the present invention, problems with the mechanism of the conventional method, such as difficulty in handling such as the interface position easily changing, and the volume ratio of the two liquid phases participating in phase mixing (so-called O/ This is caused by the operational limitation that the A ratio) depends on the ratio of the liquid feeding speed of both phases, inefficient two-liquid phase mixing that involves the surrounding heavy liquid phase, and the interlocking of stirring blade rotation and liquid feeding speed. It can solve operational complications. That is, according to the method of the present invention, the interface position does not fluctuate and is always stable, the volume ratio of both phases can be set independently (independently), and the volume ratio of both phases within the emulsion phase can be set independently. Efficient two-liquid phase mixing can be achieved while maintaining the ratio consistently from beginning to end, and the rotation of the stirring blade can be prevented from affecting the liquid feeding speed.

Furthermore, in the present invention, as an innovative feature not found in conventional methods, the number of theoretical plates is improved by countercurrent contact based on opposing flows of a heavy liquid phase and a light liquid phase. The number of theoretical plates mentioned here is an index that expresses the separation performance in liquid-liquid extraction based on the distribution equilibrium value in a batch system, and as the number of theoretical plates increases, the degree of separation between two substances increases. The value of the separation coefficient (ratio of distribution ratios of two substances), which indicates , increases. In addition, phase separation properties are improved by simultaneous progress of phase separation in a container or room for mechanical stirring (mixer room). Furthermore, by switching from overflow to pressure liquid feeding, circulating liquid feeding can be facilitated. In addition, the circulating liquid feeding adaptive mechanism can be used for the multi-stage effect produced by integrating forward extraction, washing, and reverse extraction and synchronously circulating the liquid, and is more effective than the conventional mechanism. , the equipment system can be significantly downsized.

A single-chamber system that circulates the heavy liquid phase and light liquid phase (Part 1). A single-chamber system that circulates the heavy liquid phase and light liquid phase (Part 2). A single-chamber mechanism that circulates the heavy liquid phase and light liquid phase (part 3). A single-chamber system that circulates the heavy liquid phase and light liquid phase (part 4). A single-chamber mechanism that circulates the heavy liquid phase and light liquid phase (Part 5). A single-chamber system that circulates only the light liquid phase (Part 1). A single-chamber system that circulates only the light liquid phase (Part 2). A single-chamber system that circulates only the light liquid phase (Part 3). A single-chamber mechanism that circulates only the light liquid phase (part 4). A single-chamber system that circulates only the light liquid phase (Part 5). A single-chamber system that circulates only the heavy liquid phase (Part 1). A single-chamber system that circulates only the heavy liquid phase (Part 2). A single-chamber system that circulates only the heavy liquid phase (part 3). A single-chamber system that circulates only the heavy liquid phase (part 4). A single-chamber system that circulates only the heavy liquid phase (Part 5). A single-chamber system that transports heavy liquid phase and light liquid phase once (Part 1). A single-chamber system that transports the heavy liquid phase and light liquid phase once (Part 2). A single-chamber mechanism that transports the heavy liquid phase and light liquid phase once (part 3). A single-chamber system that transports the heavy liquid phase and light liquid phase once (part 4). A single-chamber system that transports heavy liquid phase and light liquid phase once (part 5). A single-chamber system with an upper and lower overhang that circulates the heavy liquid phase and light liquid phase (Part 1). A single-chamber system with an upper and lower overhang that circulates the heavy liquid phase and light liquid phase (Part 2). A single-chamber system with an upper and lower overhang that circulates the heavy liquid phase and light liquid phase (part 3). A single-chamber system with an upper and lower overhang that circulates the heavy liquid phase and light liquid phase (part 4). A single-chamber mechanism with an upper and lower overhang that circulates the heavy liquid phase and light liquid phase (Part 5). A single-chamber system with an upper and lower overhang that circulates and pumps only the light liquid phase (Part 1). A single-chamber system with an upper and lower overhang that circulates and pumps only the light liquid phase (Part 2). A single-chamber mechanism with an upper and lower overhang that circulates and pumps only the light liquid phase (part 3). A single-chamber system with an upper and lower overhang that circulates and pumps only the light liquid phase (Part 4). A single-chamber system with an upper and lower overhang that circulates and pumps only the light liquid phase (Part 5). A single-chamber system with an upper and lower overhang that circulates and pumps only the heavy liquid phase (Part 1). A single-chamber system with an upper and lower overhang that circulates and pumps only the heavy liquid phase (Part 2). A single-chamber system with an upper and lower overhang that circulates only the heavy liquid phase (part 3). A single-chamber system with an upper and lower overhang that circulates and pumps only the heavy liquid phase (Part 4). A single-chamber system with an upper and lower overhang that circulates and pumps only the heavy liquid phase (Part 5). A single-chamber system with an upper and lower overhang that transports the heavy liquid phase and light liquid phase once (part 1). A single-chamber mechanism with an upper and lower overhang that transports the heavy liquid phase and light liquid phase once (part 2). A single-chamber system with an upper and lower overhang that transports the heavy liquid phase and light liquid phase once (part 3). A single-chamber system with an upper and lower overhang that transports the heavy liquid phase and light liquid phase once (part 4). A single-chamber system with an upper and lower overhang that transports the heavy liquid phase and light liquid phase once (Part 5). Vertically long, single-chamber system that uses a shaft holder or bearing (part 1). A vertically elongated single-chamber type with vertically extending upper and lower sides that uses a shaft holder or bearing (part 1). Vertically long, single-chamber system that uses a shaft holder or bearing (Part 2). A mechanism using a shaft holder or bearing in a vertically elongated single-chamber type with upper and lower overhangs (Part 2). A vertically elongated, single-chamber system that uses two axes orthogonal gears. A vertically elongated single-chamber type with vertically extending top and bottom, and a mechanism that uses two axes orthogonal gears. A multi-chamber system that circulates the heavy liquid phase and light liquid phase (Part 1). A multi-chamber system that circulates the heavy liquid phase and light liquid phase (Part 2). A multi-chamber system that circulates the heavy liquid phase and light liquid phase (Part 3). A multi-chamber system that circulates the heavy liquid phase and light liquid phase (part 4). A multi-chamber system that circulates only the light liquid phase (Part 1). A multi-chamber system that circulates only the light liquid phase (Part 2). A multi-chamber system that circulates only the light liquid phase (part 3). A multi-chamber system that circulates only the light liquid phase (part 4). A multi-chamber system that circulates only the heavy liquid phase (Part 1). A multi-chamber system that circulates only the heavy liquid phase (Part 2). A multi-chamber system that circulates only the heavy liquid phase (part 3). A multi-chamber system that circulates only the heavy liquid phase (part 4). A multi-chamber system that transports heavy liquid phase and light liquid phase once (part 1). A multi-chamber mechanism (part 2) that transports the heavy liquid phase and light liquid phase once. A multi-chamber system that transports heavy liquid phase and light liquid phase once (part 3). A multi-chamber system that transports heavy liquid phase and light liquid phase once (part 4). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 1). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 1). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 2). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 2). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 3). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 3). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 4). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 4). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 5). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 5). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 6). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 6). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 7). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 7). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 8). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 8). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 9). Relationship between the structure of the partition plate and the upper and lower communication parts when installing two liquid phases (Part 9). A multi-chamber mechanism that circulates the heavy liquid phase and light liquid phase (Part 5). A multi-chamber mechanism that circulates the heavy liquid phase and light liquid phase (Part 6). A multi-chamber mechanism that circulates the heavy liquid phase and light liquid phase (Part 7). A multi-chamber mechanism that circulates the heavy liquid phase and light liquid phase (Part 8). A multi-chamber system that circulates only the light liquid phase (Part 5). A multi-chamber system that circulates only the light liquid phase (Part 6). A multi-chamber system that circulates only the light liquid phase (Part 7). A multi-chamber system that circulates only the light liquid phase (Part 8). A multi-chamber system that circulates only the heavy liquid phase (Part 5). A multi-chamber system that circulates only the heavy liquid phase (Part 6). A multi-chamber system that circulates only the heavy liquid phase (Part 7). A multi-chamber system that circulates only the heavy liquid phase (Part 8). A multi-chamber system that transports the heavy liquid phase and light liquid phase once (part 5). A multi-chamber system that transports heavy liquid phase and light liquid phase once (part 6). A multi-chamber system that transports the heavy liquid phase and light liquid phase once (part 7). A multi-chamber system that transports heavy liquid phase and light liquid phase once (part 8). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 1). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 1). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 2). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 2). Relationship between the structure of the upper partition plate and lower partition plate and the upper and lower communication parts (part 3). Relationship between the structure of the upper partition plate and lower partition plate and the upper and lower communication parts (part 3). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 4). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 4). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 5). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 5). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 6). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 6). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 7). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 7). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 8). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 8). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 9). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 9). A multi-chamber system that circulates the heavy liquid phase and light liquid phase (part 9). A multi-chamber system that circulates the heavy liquid phase and light liquid phase (Part 10). A multi-chamber system that circulates the heavy liquid phase and light liquid phase (Part 11). A multi-chamber system that circulates the heavy liquid phase and light liquid phase (Part 12). A multi-chamber system that circulates only the light liquid phase (part 9). A multi-chamber system that circulates only the light liquid phase (Part 10). A multi-chamber system that circulates only the light liquid phase (Part 11). A multi-chamber system that circulates only the light liquid phase (Part 12). A multi-chamber system that circulates only the heavy liquid phase (part 9). A multi-chamber system that circulates only the heavy liquid phase (Part 10). A multi-chamber system that circulates only the heavy liquid phase (Part 11). A multi-chamber system that circulates only the heavy liquid phase (Part 12). A multi-chamber system that transports the heavy liquid phase and light liquid phase once (part 9). A multi-chamber mechanism that transports heavy liquid phase and light liquid phase once (part 10). A multi-chamber mechanism that transports heavy liquid phase and light liquid phase once (Part 11). A multi-chamber system that transports heavy liquid phase and light liquid phase once (part 12). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 10). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 10). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 11). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 11). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 12). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 12). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 13). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 13). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 14). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 14). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 15). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 15). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 16). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 16). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 17). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 17). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 18). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 18). A multi-chamber mechanism that circulates the heavy liquid phase and light liquid phase (Part 13). A multi-chamber mechanism that circulates the heavy liquid phase and light liquid phase (Part 14). A multi-chamber mechanism that circulates the heavy liquid phase and light liquid phase (Part 15). A multi-chamber system that circulates the heavy liquid phase and light liquid phase (Part 16). A multi-chamber system that circulates only the light liquid phase (Part 13). A multi-chamber system that circulates only the light liquid phase (Part 14). A multi-chamber system that circulates only the light liquid phase (Part 15). A multi-chamber system that circulates only the light liquid phase (Part 16). A multi-chamber system that circulates only the heavy liquid phase (Part 13). A multi-chamber system that circulates only the heavy liquid phase (Part 14). A multi-chamber system that circulates only the heavy liquid phase (Part 15). A multi-chamber system that circulates only the heavy liquid phase (Part 16). A multi-chamber mechanism that transports heavy liquid phase and light liquid phase once (part 13). A multi-chamber system that transports heavy liquid phase and light liquid phase once (Part 14). A multi-chamber system that transports heavy liquid phase and light liquid phase once (Part 15). A multi-chamber system that transports heavy liquid phase and light liquid phase once (Part 16). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 19). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 19). Relationship between the structure of the upper partition plate and lower partition plate and the upper and lower communication parts (Part 20) Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 20). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 21). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 21). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 22). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 22). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 23). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 23). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 24). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 24). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 25). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 25). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 26). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 26). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 27). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 27). A multi-chamber system that circulates the heavy liquid phase and light liquid phase (Part 17). A multi-chamber system that circulates the heavy liquid phase and light liquid phase (Part 18). A multi-chamber system that circulates the heavy liquid phase and light liquid phase (Part 19). A multi-chamber mechanism that circulates the heavy liquid phase and light liquid phase (Part 20). A multi-chamber system that circulates only the light liquid phase (Part 17). A multi-chamber system that circulates only the light liquid phase (Part 18). A multi-chamber system that circulates only the light liquid phase (Part 19). A multi-chamber system that circulates only the light liquid phase (Part 20). A multi-chamber system that circulates only the heavy liquid phase (Part 17). A multi-chamber system that circulates only the heavy liquid phase (Part 18). A multi-chamber system that circulates only the heavy liquid phase (Part 19). A multi-chamber system that circulates only the heavy liquid phase (Part 20). A multi-chamber system that transports heavy liquid phase and light liquid phase once (Part 17). A multi-chamber system that transports heavy liquid phase and light liquid phase once (part 18). A multi-chamber system that transports the heavy liquid phase and light liquid phase once (part 19). A multi-chamber system that transports heavy liquid phase and light liquid phase once (part 20). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 28). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 28). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 29). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (Part 29). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 30). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 30). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 31). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 31). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 32). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 32). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 33). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 33). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 34). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 34). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 35). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 35). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 36). Relationship between the structure of the upper partition plate and the lower partition plate and the upper and lower communication parts (part 36). The region of the emulsion mixed state when the mechanism shown in FIG. 1(f) is operated. The region of the emulsion mixed state when the mechanism shown in FIG. 2(f) is operated. The region of the emulsion mixed state when the mechanism of FIG. 4(e) is operated. The region of the emulsion mixed state when the mechanism of FIG. 6(e) is operated. The region of the emulsion mixed state when the mechanism of FIG. 8(e) is operated. The region of the emulsion mixed state when the mechanism of FIG. 10(e) is operated. The region of the emulsion mixed state when the mechanism shown in FIG. 12(e) is operated. In the partition plate shown in FIG. 4(e), horizontal passage ports are installed in addition to the communication areas between the upper and lower chambers. The region of the emulsion mixed state when the mechanism of FIG. 21 is operated. The conventional mixer settler mechanism corresponds to Figure 8(m).

In liquid-liquid extraction based on mechanical stirring performed by installing a heavy liquid phase and a light liquid phase in a container 1 equipped with stirring blades 2, the present invention can always maintain the interface between the two liquid phases at the same position, and The volume ratio of both phases in a container or room can be set independently of the liquid feeding rate, and the heavy liquid phase and light liquid phase can be efficiently mixed to create a stable emulsion phase (two-liquid emulsion mixed phase) over a wide range. ), the rotation of the stirring blade (strength of phase mixing) can be prevented from affecting the liquid feeding speed, and the number of theoretical plates can be increased due to countercurrent contact between the heavy liquid phase and the light liquid phase, and the phase mixing can be improved. The liquid is characterized in that the phase separation property is improved by simultaneously proceeding phase separation in the container 1, and the circulating liquid can be easily transferred by switching from liquid feeding by overflow to liquid feeding by pressure action. This invention relates to a method for extracting and recovering specific substances based on liquid extraction.

In conventional liquid-liquid extraction mechanisms using mechanical stirring, such as the mixer-settler method, the interface position tends to fluctuate, and the volume ratio of the two liquid phases participating in phase mixing depends on the ratio of the liquid feeding speeds of both phases. There are problems such as, the surrounding heavy liquid phase is dragged in when two liquid phases are mixed, and the rotational speed of the stirring blade 2 affects the liquid feeding speed. The present invention solves the problems inherent in the mechanisms of these conventional methods and, in addition, brings out innovative features that cannot be obtained with the mechanisms of the conventional methods. A method using this mechanism makes it possible to produce specific substances more efficiently and effectively than conventional methods.

The blade part of the stirring blade 2 is arranged near the interface 100 between the heavy liquid phase 4 and the light liquid phase 5 and rotated, and the heavy liquid phase 4 is drawn from above and the light liquid from below of the container 1 in which the stirring blade is stored. By using a mechanism for feeding and introducing phase 5, the problems associated with the mechanism of the conventional method described above can be solved. Furthermore, in the mechanism of the present invention, the heavy liquid phase 4 and the light liquid phase 5 flow in opposite directions, so that the two phases come into countercurrent contact, and the number of theoretical plates increases. Further, phase separation properties are improved by allowing phase separation to proceed simultaneously in the container 1 for phase mixing. Furthermore, by switching from overflow to pressure liquid feeding, circulating liquid feeding can be facilitated. In other words, it not only solves the problems of conventional methods, but also brings out innovative features that cannot be obtained with conventional methods, making it possible to extract and recover specific substances based on liquid-liquid extraction more efficiently and effectively than conventional methods. You will be able to do this.

First, as the most basic and simple mechanism of the present invention, reference will be made to FIGS. 1(a) to 1(t), but the invention is not limited thereto. A structure in which a heavy liquid phase 4 and a light liquid phase 5 are placed in one container 1 equipped with a stirring blade 2, and a blade portion of the stirring blade 2 is placed near an interface 100 between both phases in the container, While rotating the stirring blade, the heavy liquid phase 4 is introduced from the top of the container, and the light liquid phase 5 is introduced from the bottom, so that a state where both phases are emulsified and mixed and a state where they are phase separated coexist. Perform liquid-liquid extraction. According to such a mechanism, countercurrent contact of two liquid phases, which could not be realized in conventional liquid-liquid extraction using mechanical stirring, such as the mixer-settler method, becomes possible. In addition, in these figures, as an example, the heavy liquid phase and the light liquid phase are shown to have the same volume, but this is not a limitation. Figure 1(a), Figure 1(b), Figure 1(c), Figure 1(d), Figure 1(e), Figure 1(f), Figure 1(g), Figure 1(h), Figure 1 (i), FIG. 1(j), FIG. 1(k), FIG. 1(l), FIG. 1(m), FIG. 1(n), and FIG. 1(o) show the heavy liquid phase or light liquid phase or This is an example of a mechanism for circulating liquid in both of them. This is an example of a mechanism for sending both liquid phases in one pass.

In FIGS. 1(a), 1(b), 1(c), 1(d), and 1(e), both the heavy liquid phase and the light liquid phase are circulated. Figure 1(f), Figure 1(g), Figure 1(h), Figure 1(i), and Figure 1(j) show that the light liquid phase is circulated while the heavy liquid phase is fed in one pass. Send liquid. In addition, as for the method of discharging the heavy liquid phase, Fig. 1(f) and Fig. 1(g) show a piping method, and Fig. 1(h), Fig. 1(i), and Fig. 1(j) show an in-container passage method. . The heavy liquid phase can be discharged either by piping method (Fig. 1(f) and Fig. 1(g)) or by internal passage method (Fig. 1(h), Fig. 1(i), and Fig. 1(j)). , the discharge position is placed upward. Figure 1(k), Figure 1(l), Figure 1(m), Figure 1(n), and Figure 1(o) show that the heavy liquid phase is circulated and the light liquid phase is passed once. Send liquid. In addition, as for the method of discharging the light liquid phase, Fig. 1(k) and Fig. 1(l) show the piping method using the liquid feed line 7, and Fig. 1(m), Fig. 1(n), and Fig. 1(o) show the method of discharging the light liquid phase. This is an in-container passage system using a liquid phase passage 12. The light liquid phase can be discharged by placing the discharge position upward in the piping method (Figs. 1(k) and 1(l)), and in the container passage method (Fig. 1(m), Fig. 1(n), In FIG. 1(o)), the discharge position is placed downward. Regarding Figures 1(k) and 1(l), if you want to manage the supply and discharge of the light liquid phase at the same height, it is also possible to extend the discharge piping from the top to the bottom. . In addition, specific substances to be separated and purified in the oil phase (light liquid phase 5 in most cases) are placed in a back extraction container (Fig. (not shown), it can be collected in the back extraction liquid (in most cases, heavy liquid phase) placed in the back extraction vessel. That is, similar to FIG. 1 of Japanese Patent Application No. 2019-113657 previously filed by the same applicant, for example, the light liquid phase taken out from the inlet of the liquid feeding line 7 is transferred to a reverse extraction container having the same structure as the container 1. The specific substance is recovered in the reverse extraction solution by feeding the liquid into the reverse extraction solution (heavy liquid phase) from below and returning the reset light liquid phase obtained from above to the liquid supply line 7. .

Figure 1(p), Figure 1(q), Figure 1(r), Figure 1(s), and Figure 1(t) are examples of a mechanism in which both the heavy liquid phase and the light liquid phase are transferred in one pass. It is. In FIG. 1(p), both the heavy liquid phase 4 and the light liquid phase 5 are discharged by a piping method, and the liquids are sent in one pass. In FIG. 1(q), the heavy liquid phase is discharged by an in-container passage method, and the light liquid phase is discharged by a piping method, and the liquid is sent in one pass. In FIG. 1(r), the heavy liquid phase is discharged by a piping method, and the light liquid phase is discharged by a passage method in a container, and the liquid is sent in one pass. In FIGS. 1(s) and 1(t), the discharge method for both the heavy liquid phase and the light liquid phase is a container passage method, and the liquid is sent in one pass. Further, FIG. 1(s) shows a shape in which the passages in the container for the heavy liquid phase and the light liquid phase are brought to one side of the container 1, and FIG. 1(t) shows a shape in which the passages in the container for both phases are distributed to the left and right. The heavy liquid phase 4 can be discharged either by piping method (Fig. 1 (p) and Fig. 1 (r)) or by internal passage method (Fig. 1 (q), Fig. 1 (s), and Fig. 1 (t)). However, it is done by placing the ejection position upward. In addition, the light liquid phase 5 is discharged by placing the discharge position upward in the piping method (Fig. 1 (p) and Fig. 1 (q)), and by placing the discharge position upward in the pipe method (Fig. 1 (r), Fig. 1 (s)). , and FIG. 1(t)), the discharge position is placed downward. Regarding Figures 1(p) and 1(q), if you want to manage the supply and discharge of the light liquid phase at the same height, it is also possible to extend the discharge piping from the top to the bottom. .

Further, the positions of the blade portions of the stirring blades 2 shown in FIGS. 1(a) to 1(t) can have a certain width, for example, the blades are located above and below the interface 100 between the two liquid phases. The method of the present invention is effective within a range of about 2 to 3 times the thickness (height) of the part.

The mechanism shown in FIGS. 1(a) to 1(t) is characterized by the coexistence of a state where the heavy liquid phase 4 and the light liquid phase 5 are emulsified and mixed, and a state where both phases are separated. It functions by discharging or circulating the two separated phases. That is, phase separation is the key to the present invention, and it is important to perform phase separation reliably. Therefore, for example, by providing the upper part, the lower part, or both of the container 1 with a shape (overhanging shape) having a larger cross-sectional area than the middle part of the container, the heavy liquid phase 4 and the light liquid phase 5 can be phase separation is promoted. Note that even when the cross-sectional area of the central portion of the container is increased for reasons such as increasing the size of the wing portion, the same effect can be obtained by narrowing the space between the projecting shape and the central portion.

FIGS. 2(a) to 2(t) show examples in which both the upper and lower parts of the container 1 are provided with a shape (overhanging shape) that has a larger cross-sectional area than the middle part of the container. That's not the limit. Even in a container having such a shape, a flow path mechanism similar to the structure shown in FIGS. 1(a) to 1(t) is possible.

In the mechanisms shown in FIGS. 1(a) to 1(t), etc., and FIGS. 2(a) to 2(t), etc., if the area where the heavy liquid phase 4 and the light liquid phase 5 are emulsified and mixed is enlarged, If the processing speed of liquid-liquid extraction can be increased, and the region where both phases are separated can be increased, a margin can be given to phase separation. For example, if the container 1 is made to have a more vertically elongated shape (a shape expanded in the vertical direction) and its volume is increased (hereinafter referred to as the elongated shape becoming more pronounced), the emulsified mixed state of the heavy liquid phase 4 and the light liquid phase 5 will change. By expanding the area in the vertical direction, the processing speed increases, a margin is created for phase separation, and phase separation of both phases is promoted. In addition, the vertically elongated shape is advantageous in that the installation floor area can be reduced.

Furthermore, since the mechanism is such that a high number of theoretical plates can be expected by bringing the heavy liquid phase 4 and the light liquid phase 5 into countercurrent contact, if the vertically elongated shape is made more pronounced, the selective separation power will improve from the viewpoint of the number of theoretical plates. Therefore, more advanced separation becomes possible.

On the other hand, if the vertically elongated shape of the container 1 is made more pronounced, the rotational axis of the stirring blade 2 must necessarily be made longer. However, if the rotating shaft becomes longer, shaft vibration and shaft runout will increase, and normal mechanical stirring may become impossible. Therefore, by installing a shaft holder, a bearing, or a biaxial orthogonal gear, shaft vibration and shaft wobbling can be eliminated. Note that two or all of the shaft holder, bearing, and biaxial orthogonal gear may be used in combination. Although FIGS. 3(a) to 3(f) show examples in which shaft holders, bearings, or two-axis orthogonal gears are installed, the present invention is not limited thereto.

Fig. 3(a) shows the structure of Fig. 1(a) in which the vertically elongated shape of the container 1 is made more conspicuous.In order to eliminate shaft vibration and shaft runout, a shaft is installed above the blade part of the stirring blade 2. A holder or bearing is installed. Note that the shaft holder referred to here is something that limits the wobbling of the rotating shaft (especially movement in the left and right direction), and is intended to have a structure in which the rotating shaft and shaft holder do not touch at any point or surface. . On the other hand, a bearing is intended to be a structure in which a rotating shaft and a bearing are in contact with each other at a point or a plane, that is, a rolling bearing or a sliding bearing. In addition, FIG. 3(b) shows the structure of FIG. 2(a) in which the vertically elongated shape of the container 1 is emphasized, and like FIG. 3(a), there is a shaft above the blade part of the stirring blade 2. A holder or bearing is installed. Note that a plurality of shaft holders or bearings may be installed above the blade portion of the stirring blade 2.

The shaft holder or bearing can also be installed below the blade section by extending the rotating shaft of the stirring blade 2 to below the blade section. For example, as shown in FIG. 3(c) or FIG. 3(d), a shaft holder or a bearing can be installed near the bottom of the container 1, but this is not a limitation. Note that shaft holders or bearings may be installed both above and below the blade portion of the stirring blade 2, or a plurality of shaft holders or bearings may be installed above or below the blade portion of the stirring blade 2, or both. It's okay.

A biaxial orthogonal gear can also be used instead of a shaft holder or bearing. In FIG. 3(e), the vertically elongated shape of the container 1 shown in FIG. A biaxial orthogonal gear is installed above the wing section. Further, in FIG. 3(f), a biaxial orthogonal gear is similarly installed for the container 1 shown in FIG. 2(a), which has a more pronounced vertically elongated shape. In these cases, the horizontal rotation axis perpendicular to the vertical rotation axis is fixed by a bearing installed on the vessel wall, but this is not the case. Note that even when using biaxial orthogonal gears, a plurality of biaxial orthogonal gears may be installed above the blade portion of the stirring blade 2, as in the case of using a shaft holder or a bearing. Furthermore, it is also possible to extend the rotating shaft of the stirring blade 2 below the blade part and then install a biaxial orthogonal gear below the blade part. In that case, biaxial orthogonal gears can be installed both above and below the blade part of the stirring blade 2, or a plurality of biaxial orthogonal gears can be installed above or below the blade part of the stirring blade 2, or both. You may do so.

In addition, when using two-axis orthogonal gears, it is not necessarily necessary to use the vertical rotation axis as the power axis.If the horizontal rotation axis is used as the power axis and the vertical rotation axis is fixed with a bearing, the container 1 A motor can be installed on the side to rotate the stirring blade twice. In terms of maintenance and management of the stirring blade rotation motor, it may be more convenient to install it on the side of the vertically long container 1 rather than on the top.

The same mechanism as described above is applied to a container structure that is separated into a mixer chamber 30 for stirring and mixing the heavy liquid phase 4 and light liquid phase 5 and a settler chamber 40 for phase-separating both phases, as in the conventional method. Can be applied. Specifically, communication parts are provided at two locations, between the ceiling surface and the partition plate of the container 1 that houses the mixer chamber 30 and the settler chamber 40, and between the bottom surface and the partition plate, so that the heavy liquid phase and the light liquid phase can be exchanged between the two chambers. If they are allowed to freely come and go, it can be handled in the same way as the above-mentioned container structure in which there is no distinction between the mixer chamber 30 and the settler chamber 40. Basically, the operation is performed so that the mixed phase in the emulsion mixture state does not pass through the upper and lower two communicating portions of the partition plate between the mixer chamber 30 and the settler chamber 40. By providing the settler chamber 40, it is expected that phase separation properties and stability during operation will be improved. That is, unexpected growth (expansion of range) of the emulsion phase (two-liquid emulsion mixed phase) reduces the risk of contamination of the emulsion phase with the heavy and light liquid phases being discharged or recycled.

4(a) to 4(p) show the mechanism of a container structure that is separated into a mixer chamber 30 and a settler chamber 40 by one partition plate (M chamber/S chamber partition plate). Even in such a container structure, a flow path mechanism similar to the structures shown in FIGS. 1(a) to 1(t) and the structures shown in FIGS. 2(a) to 2(t) is possible. be. In addition to Figs. 4(a) to 4(p), there are also structures in which the internal passages of both phases are allocated to the left and right (Fig. 1(e), Fig. 1(j), Fig. 1(o), Fig. 1 (t), FIG. 2(e), FIG. 2(j), FIG. 2(o), and FIG. 2(t)) are also possible. However, in that the settler chamber 40 is installed to improve phase separation, it is not possible to provide a passage (passage for discharge or circulation) in the container for the heavy liquid phase 4 or the light liquid phase 5 on the mixer chamber 30 side. I can't say it's desirable.

5(a1), 5(b1) and 5(b1) show the relationship between the communication parts installed between the ceiling surface and the partition plate of the container 1 that stores the mixer chamber 30 and the settler chamber 40, and between the bottom surface and the partition plate and the partition plate. ...shown in Figure 5 (i1). Further, the states in which the heavy liquid phase and the light liquid phase are installed are shown in FIGS. 5(a2), 5(b2), and 5(i2), respectively. Note that these figures are all views of the mixer chamber 30 side from the settler chamber 40 side. The light liquid phase communication part provided between the ceiling surface and the partition plate has a structure in which part or all of the upper end of the partition plate does not touch the ceiling surface, or a structure in which a passage port is provided at the upper end of the partition plate. obtained by. Similarly, the communication area for the heavy liquid phase provided between the bottom surface and the partition plate has a structure in which part or all of the bottom end of the partition plate is not in contact with the bottom surface, or a passage port is provided at the bottom end of the partition plate. Obtained by structure.

Note that the shapes of these communication parts are not limited to the shapes shown in FIGS. 5(a1) to 5(i2). That is, for a structure in which a part of the upper end or lower end of the partition plate is not in contact with the ceiling surface or the bottom surface, the shape is not limited to a square, but may be a semicircle, a triangle, or the like. Similarly, the shape of the passage opening provided at the upper end or lower end of the partition plate is not limited to a circle, but may be square, triangular, or the like.

Further, a structure in which part or all of the upper end or lower end of the partition plate does not touch the ceiling surface or the bottom surface and a structure in which a passage hole is provided at the upper end or lower end of the partition plate can be used in combination. FIG. 5(f1) to FIG. 5(i2) are examples of a combination of the two.

The mechanisms shown in FIGS. 4(a) to 4(p) are excellent as mechanisms for forming an emulsion-mixed region (emulsion phase) over a wide range in the mixer chamber 30, but on the other hand, It is not always easy to keep the height (width) of the emulsion phase constant in the mixer chamber 30 without causing it to flow into the settler chamber 40. That is, the height of the emulsion phase in the mixer chamber may easily fluctuate, and in that case, a structure that can afford such fluctuations or a structure that can control fluctuations is preferable.

First, there is a method in which the mixer chamber 30 is formed into a vertically elongated shape as a structure that allows a margin for variation in the height of the emulsion phase. The vertically elongated shape not only suppresses outflow of the emulsion phase into the settler chamber 40 and improves phase separation properties, but also has the advantage that contact between the two liquid phases is promoted by the emulsion phase growing higher. On the other hand, if the stirring blades 2 are made into a vertically elongated shape, as described above, the rotating shaft of the stirring blade 2 becomes longer, resulting in increased shaft vibration and shaft wobbling, which may make normal mechanical stirring impossible. Therefore, it is effective to eliminate shaft vibration and shaft runout by installing a shaft holder, a bearing, or a biaxial orthogonal gear, as shown in Figures 3(a) to 3(f), for example. It is. Note that two or all of the shaft holder, bearing, and biaxial orthogonal gear may be used in combination.

On the other hand, the upper and lower communication parts between the mixer chamber 30 and the settler chamber 40 are such that the upper communication part allows the light liquid phase to go back and forth between the two chambers, and the lower communication part allows the heavy liquid phase to go back and forth between the two chambers. Both of them do not originally have the role of causing the emulsion phase to flow out into the settler chamber 40. However, in a structure in which the emulsion phase does not move at all from the mixer chamber 30, there is no escape route for the overgrown emulsion phase other than the above-mentioned upper and lower communication parts, and in that respect, it is not necessarily preferable. Conversely, if the structure is such that a portion of the emulsion phase moves to the settler chamber 40, fluctuations in the height (width) of the emulsion phase in the mixer chamber 30 can be significantly suppressed.

Therefore, as a structure that can control the variation in the height (width) of the emulsion phase, in addition to the upper and lower communication parts, if a passage hole is provided in the partition plate at a height near the blade part of the stirring blade 2, it is possible to As the emulsion phase flows out into the settler chamber 40, fluctuations in the height of the emulsion phase in the mixer chamber 30 are suppressed. However, in such a structure, the emulsion phase generated in the mixer chamber 30 immediately moves to the settler chamber 40, so the development of the emulsion phase in the mixer chamber 30 is suppressed, and a large amount of the emulsion phase is transferred to the settler chamber 40. 40, making phase separation in the settler chamber 40 difficult.

On the other hand, if the emulsion phase generated in the mixer chamber 30 is moved through a passage formed in the vertical direction, guided to a vertical passage port, and then brought to the settler chamber 40, the phase will separate in the process. progresses, and the emulsion in the settler chamber 40 is largely eliminated. Some examples of such container structures are shown below.

Instead of the partition plates shown in FIGS. 4(a) to 4(p), an upper partition plate is provided at the upper part of the container 1 that stores the mixer chamber 30 and the settler chamber 40, forming a communication area for the light liquid phase of both chambers. , and by alternately installing lower partition plates at the bottom of the container that form a communication area for the heavy liquid phases in both chambers, a passageway and a vertical passage opening are created through which the two emulsion-mixed liquid phases can move in the vertical direction. can be formed.

An example in which the upper partition plate 20 is placed closer to the mixer chamber 30 and the lower partition plate 21 is installed closer to the settler chamber is shown in FIGS. 6(a) to 6(p), but this is not the case. Note that, under the condition that the upper partition plates 20 and the lower partition plates 21 are installed alternately, there may be a plurality of upper partition plates and a plurality of lower partition plates. In this way, regardless of the difference in the number of partition plates installed, a flow path mechanism similar to the structure shown in FIGS. 4(a) to 4(p) is possible.

In addition, the structure of the upper partition plate 20 (partition plate near the mixer room) at this time and the shape of the communicating part of the light liquid phase 5 formed thereby are shown in FIG. 7(a1), FIG. 7(b1)... It is shown in FIG. 7(i1). In addition, the structure of the lower partition plate 21 (partition plate near the settler chamber) and the shape of the communication area of the heavy liquid phase 4 formed thereby are shown in FIG. 7(a2), FIG. 7(b2)...FIG. Shown in i2). Here, FIG. 7(a1) and FIG. 7(a2), FIG. 7(b1) and FIG. 7(b2)...FIG. 7(i1) and FIG. 7(i2) are a pair of upper partition plate 20 and lower partition. A plate 21 is shown. The communication portion of the light liquid phase 5 provided between the ceiling surface and the upper partition plate 20 has a structure in which part or all of the upper end of the upper partition plate 20 is not in contact with the ceiling surface, or the upper end of the upper partition plate 20 This is achieved by a structure in which a passage hole is provided in the part. Similarly, the communication portion of the heavy liquid phase 4 provided between the bottom surface and the lower partition plate 21 is constructed such that part or all of the lower end of the lower partition plate 21 is not in contact with the bottom surface, or This is achieved by a structure in which a passage hole is provided at the lower end.

Note that the shapes of these communicating parts are not limited to the shapes shown in FIGS. 7(a1) to 7(i2). That is, for a structure in which a part of the upper end of the upper partition plate 20 does not touch the ceiling surface, or a structure in which a part of the lower end of the lower partition plate 21 does not touch the bottom surface, the shape is not limited to a square, but may be half-shaped. The shape may be a circle, a triangle, or the like. Similarly, the shape of the passage opening provided at the upper end of the upper partition plate 20 or the lower end of the lower partition plate 21 is not limited to a circle, but may be a square, a triangle, or the like.

In addition, there are two types of structures: a structure in which a part or all of the upper end of the upper partition plate 20 does not touch the ceiling surface, a structure in which a passage opening is provided at the lower end of the lower partition plate 21, and a passage opening in the upper end of the upper partition plate 20. A structure in which a part or all of the lower end of the lower partition plate 21 is not in contact with the bottom surface can be used in combination. FIG. 7(f1) to FIG. 7(i2) are examples of a combination of the two.

An example in which the lower partition plate 21 is placed closer to the mixer chamber 30 and the upper partition plate 20 is installed closer to the settler chamber 40 is shown in FIGS. 8(a) to 8(p), but this is not the case. Note that, under the condition that the lower partition plates 21 and the upper partition plates 20 are installed alternately, there may be a plurality of lower partition plates and a plurality of upper partition plates. In this case as well, regardless of the difference in the number of partition plates installed, a flow path mechanism similar to the structure shown in FIGS. 4(a) to 4(p) is possible.

In addition, the structure of the lower partition plate 21 (partition plate near the mixer room) at this time and the shape of the communication area of the heavy liquid phase 4 formed thereby are shown in FIGS. 9(a1), 9(b1)... 9(i1). In addition, the structure of the upper partition plate 20 (partition plate near the settler chamber) and the shape of the communication area of the light liquid phase 5 formed thereby are shown in FIGS. 9(a2), 9(b2), . . . Shown in i2). Here, FIG. 9(a1) and FIG. 9(a2), FIG. 9(b1) and FIG. 9(b2)...FIG. 9(i1) and FIG. 9(i2) are a pair of lower partition plate 21 and upper partition. A plate 20 is shown. The communication portion of the heavy liquid phase provided between the bottom surface and the lower partition plate 21 has a structure in which part or all of the lower end of the lower partition plate 21 is not in contact with the bottom surface, or it passes through the lower end of the lower partition plate 21. Obtained by a structure provided with a mouth. Similarly, the light liquid phase communication portion provided between the ceiling surface and the upper partition plate 20 has a structure where part or all of the upper end of the upper partition plate 20 is not in contact with the ceiling surface, or a structure where the upper partition plate 20 This is obtained by having a structure in which a passage hole is provided at the upper end of the .

Note that the shapes of these communication parts are not limited to the shapes shown in FIGS. 9(a1) to 9(i2). That is, for a structure in which a part of the upper end of the upper partition plate 20 does not touch the ceiling surface, or a structure in which a part of the lower end of the lower partition plate 21 does not touch the bottom surface, the shape is not limited to a square; The shape may be semicircular or triangular. Similarly, the shape of the passage opening provided at the upper end of the upper partition plate 20 or the lower end of the lower partition plate 21 is not limited to a circle, but may be a square, a triangle, or the like.

Furthermore, there are two types of structures: a structure in which a part or all of the lower end of the lower partition plate 21 does not touch the bottom surface, a structure in which a passage opening is provided at the upper end of the upper partition plate 20, and a structure in which a passage opening is provided in the lower end of the lower partition plate 21. A structure in which a part or all of the upper end of the upper partition plate 20 is not in contact with the ceiling surface can be used in combination. FIGS. 9(f1) to 9(i2) are examples of a combination of the two.

FIGS. 10(a) to 10(p) show an example in which a short lower partition plate 21 and an upper partition plate 20 bent at two points are combined to form a vertical passage and a vertical passage port. However, this is not limited to this. Note that, under the condition that the lower partition plates 21 and the upper partition plates 20 are installed alternately, there may be a plurality of lower partition plates and a plurality of upper partition plates. In this case as well, regardless of the number and shape of the partition plates installed, a flow path mechanism similar to the structures shown in FIGS. 4(a) to 4(p) is possible.

In addition, the structure of the lower partition plate 21 (short-shaped partition plate) at this time and the shape of the communication area of the heavy liquid phase formed thereby are shown in FIGS. 11(a1), 11(b1)... Shown in (i1). In addition, the structure of the upper partition plate 20 (a partition plate bent at two points) and the shape of the light liquid phase communication area formed thereby are shown in FIGS. 11(a2), 11(b2)... It is shown in FIG. 11(i2). Here, FIG. 11(a1) and FIG. 11(a2), FIG. 11(b1) and FIG. 11(b2)...FIG. 11(i1) and FIG. 11(i2) are a pair of lower partition plate 21 and upper partition. A plate 20 is shown. Shown on the right. The communication portion of the light liquid phase 5 provided between the ceiling surface and the upper partition plate has a structure in which part or all of the upper end of the upper partition plate 20 is not in contact with the ceiling surface, or a structure in which the light liquid phase 5 passes through the upper end part of the upper partition plate 20. Obtained by a structure provided with a mouth. Similarly, the communication portion of the heavy liquid phase 4 provided between the bottom surface and the lower partition plate is constructed such that part or all of the lower end of the lower partition plate 21 is not in contact with the bottom surface, or the lower end portion of the lower partition plate 21 is This is obtained by a structure provided with a passage hole.

Note that the shapes of these communicating parts are not limited to the shapes shown in FIGS. 11(a1) to 11(i2). That is, for a structure in which a part of the upper end of the upper partition plate 20 does not touch the ceiling surface, or a structure in which a part of the lower end of the lower partition plate 21 does not touch the bottom surface, the shape is not limited to a square; The shape may be semicircular or triangular. Similarly, the shape of the passage opening provided at the upper end of the upper partition plate 20 or the lower end of the lower partition plate 21 is not limited to a circle, but may be a square, a triangle, or the like.

Furthermore, there are two types of structures: a structure in which a part or all of the lower end of the lower partition plate 21 does not touch the bottom surface, a structure in which a passage opening is provided at the upper end of the upper partition plate 20, and a structure in which a passage opening is provided in the lower end of the lower partition plate 21. A structure in which a part or all of the upper end of the upper partition plate 20 is not in contact with the ceiling surface can be used in combination. FIGS. 11(f1) to 11(i2) are examples of a combination of the two.

An example in which a short upper partition plate 20 and a lower partition plate 21 bent at two points are combined to form a vertical passage and a vertical passage opening is shown in FIGS. 12(a) to 12(p). However, this is not limited to this. Note that, under the condition that the upper partition plates 20 and the lower partition plates 21 are installed alternately, there may be a plurality of upper partition plates and a plurality of lower partition plates. In this case as well, regardless of the number and shape of the partition plates installed, a flow path mechanism similar to the structures shown in FIGS. 4(a) to 4(p) is possible.

In addition, the structure of the upper partition plate 20 (short-shaped partition plate) at this time and the shape of the heavy liquid phase communication region formed thereby are shown in FIGS. 13(a1), 13(b1)... Shown in (i1). In addition, the structure of the lower partition plate 21 (a partition plate bent at two points) and the shape of the light liquid phase communication area formed thereby are shown in FIG. 13(a2), FIG. 13(b2)... It is shown in FIG. 13(i2). Here, FIG. 13(a1) and FIG. 13(a2), FIG. 13(b1) and FIG. 13(b2)...FIG. 13(i1) and FIG. 13(i2) are a pair of upper partition plate 20 and lower partition plate. A plate 21 is shown. Shown on the right. The light liquid phase communication portion provided between the ceiling surface and the upper partition plate 20 has a structure in which part or all of the upper end of the upper partition plate 20 is not in contact with the ceiling surface, or the upper end portion of the upper partition plate 20 This is achieved by a structure in which a passage hole is provided in the. Similarly, the communication portion of the heavy liquid phase provided between the bottom surface and the lower partition plate 21 has a structure in which part or all of the lower end of the lower partition plate 21 is not in contact with the bottom surface, or the lower end of the lower partition plate 21 This is achieved by a structure in which a passage hole is provided in the part.

Note that the shapes of these communicating parts are not limited to the shapes shown in FIGS. 13(a1) to 13(i2). That is, for a structure in which a part of the upper end of the upper partition plate 20 does not touch the ceiling surface, or a structure in which a part of the lower end of the lower partition plate 21 does not touch the bottom surface, the shape is not limited to a square; The shape may be semicircular or triangular. Similarly, the shape of the passage opening provided at the upper end of the upper partition plate 20 or the lower end of the lower partition plate 21 is not limited to a circle, but may be a square, a triangle, or the like.

In addition, there are two types of structures: a structure in which a part or all of the upper end of the upper partition plate 20 does not touch the ceiling surface, a structure in which a passage opening is provided at the lower end of the lower partition plate 21, and a passage opening in the upper end of the upper partition plate 20. A structure in which a part or all of the lower end of the lower partition plate 21 is not in contact with the bottom surface can be used in combination. FIGS. 13(f1) to 13(i2) are examples of a combination of the two.

In addition, from FIG. 6(a) to FIG. 6(p), from FIG. 8(a) to FIG. 8(p), from FIG. 10(a) to FIG. 10(p), and from FIG. 12(a) to FIG. Although the example up to (p) is an example in which two partition plates (upper partition plate 20 and lower partition plate 21) are installed between mixer chamber 30 and settler chamber 40, the number of partition plates can be further increased. That is, it is possible to enhance the phase separation effect by alternately arranging the upper partition plates 20 and the lower partition plates 21, such as 3, 4, 5, or more, but the container structure It becomes more complicated.

The details of the container structure, flow channel structure, etc. to which the method of the present invention can be applied have been described above, and from FIG. 1(a) to FIG. 1(t) and from FIG. 2(a) to FIG. 2(t) For convenience, the system using one container for stirring and mixing the heavy liquid phase 4 and the light liquid phase 5, such as the system described in Figure 4(a) to Figure 4(p), is referred to as a single-chamber system. , from Fig. 6(a) to Fig. 6(p), from Fig. 8(a) to Fig. 8(p), from Fig. 10(a) to Fig. 10(p), and from Fig. 12(a) to Fig. 12( As in the mechanism described up to p), a room (mixer chamber 30) for stirring and mixing heavy liquid phase 4 and light liquid phase 5 and a chamber (settler chamber 40) for phase separation of both phases are separated by a partition plate. For convenience, the system using the container structure described above is referred to as the multi-chamber system.

The single-chamber type has a simple mechanism and functions stably under conditions where the liquid feeding speed of the two liquid phases and the rotational speed of the stirring blade 2 are kept constant. On the other hand, the height (width) of the emulsion phase can change rapidly due to unpredictable phenomena, such as large changes in the composition of the aqueous phase (often heavy liquid phase) to be treated or the introduction of solid components. In some cases. In preparation for such cases, the container 1 can be made into a vertically elongated shape, or a shape with a large cross-sectional area (overhanging shape) can be provided at the top and bottom of the container 1 to provide some margin for fluctuations in the height (width) of the emulsion phase. can be set. However, if the upper limit is exceeded and the emulsion phase develops further, normal operation will immediately become impossible.

On the other hand, in the multi-chamber type, the development of the emulsion phase beyond expectations can be suppressed by installing the settler chamber 40. That is, the multi-chamber type is a mechanism that attempts to maintain normal operation by guiding a part of the emulsion phase that has developed beyond the upper limit to the settler chamber 40. For example, in the mechanism shown in FIGS. 4(a) to 4(p), the emulsion phase that has developed excessively in the mixer chamber 30 is transferred to the container through which the phase-separated heavy liquid phase 4 and light liquid phase 5 should originally pass. Although it flows out from the upper and lower communication parts toward the settler chamber 40, it can be operated for a short time without causing significant turbidity in both phases. In addition, FIGS. 6(a) to 6(p), FIGS. 8(a) to 8(p), FIGS. 10(a) to 10(p), and FIGS. 12(a) to 12(p) In a structure having a vertical passage port as shown, phase separation progresses while the emulsion phase moves through the vertical passage port, so that by the time it reaches the settler chamber 40, the emulsion has already been largely eliminated. .

Further, in both the single-chamber type and the multi-chamber type, it may be difficult to form an emulsion phase only by mechanical stirring based on the rotation of the stirring blades 2. In that case, the formation of the emulsion phase may be promoted by feeding the heavy liquid phase 4 or the light liquid phase 5, or both, through a nozzle (not shown) having pores or capillaries.

Hereinafter, examples will show the region of the emulsion mixture state generated by the mechanism shown in the present invention, and the specific substances that are separated and purified by performing liquid-liquid extraction using the generation of such an emulsion mixture state. Although a specific example of the extraction and recovery method will be shown, the present invention is not limited to the following example.

Area of mixed emulsion state.

As an example of the single-chamber mechanism of the present invention shown in FIGS. 1(a) to 1(t), the area of the emulsion mixed state (emulsion) generated by operating the mechanism of FIG. 1(f) is It is shown in FIG. Experiments were conducted using ion-exchanged water (pure water) or 0.1M (mol dm-3) nitric acid aqueous solution as the heavy liquid phase, and a solvent containing an alkane as the main component (product name: ShellSol D70) as the light liquid phase. As a result, above and below the emulsion mixed state region, a region where the two liquid phases are phase separated (the upper part is the light liquid phase and the lower part is the heavy liquid phase region) is created, and the emulsion mixed region and the phase separation state are created. The extent (height) of the area remained stable. Note that the range (height) of the region of the emulsion mixed state is affected by the rotational speed of the stirring blade 2 and the feeding speed of the two liquid phases, but if these speeds do not change, it will be stably maintained. Ta. On the other hand, if the region of the emulsion mixture state becomes too large and the region of the phase separation state cannot be maintained sufficiently (if such a stirring blade rotation speed and liquid feeding speed are set), the inside of the container 1 will become cloudy throughout. However, it became virtually impossible to perform liquid-liquid extraction.

Note that similar emulsion mixing can be applied to mechanisms other than those shown in Figure 1(f) (the mechanisms shown in Figures 1(a) to 1(e) and 1(g) to 1(t)). The state domain is obtained. That is, it was confirmed that the difference in the channel structure for feeding the light liquid phase 5 and the heavy liquid phase 4 did not affect the region of the emulsion mixed state.

In comparison with the mechanism of the conventional mixer-settler method (referred to as the conventional method), the area of emulsion mixing state in the mechanism (single chamber type mechanism) shown in FIGS. 1(a) to 1(t) of the present invention corresponds to the mixer chamber, and the region in the phase-separated state corresponds to the settler chamber, so by increasing the region in the emulsion mixed state, the processing speed of liquid-liquid extraction was increased. For example, by making the container 1 into a vertically elongated shape while maintaining the bottom area, the processing speed could be increased without changing the installation floor area. In addition, the vertically elongated shape is effective in providing a margin for the region in the phase-separated state, and it has been found that not only can the region in the emulsion mixed state be enlarged, but also a sufficient region in the phase-separated state can be secured. Ta.

Furthermore, in order to suppress the region of the emulsion mixture state and secure the region of the phase separation state, the upper and lower sides of the container 1, or both, have a shape that has a larger cross-sectional area than the middle part of the container. It was found that phase separation of the heavy liquid phase 4 and the light liquid phase 5 was promoted when the liquid phase 4 was provided with a shape of 3 mm. FIG. 15 shows an area in which an emulsion mixture state occurs by operating a mechanism in which a shape with a large cross-sectional area is provided at the top and bottom of the container 1, as shown in FIG. 2(f). In this way, phase separation is promoted when the region in the emulsion-mixed state reaches a portion having a large cross-sectional area, so that the region in the emulsion-mixed state does not become too large and its growth can be suppressed. Note that the same emulsion mixing method can be used for mechanisms other than those shown in Figure 2(f) (the mechanisms shown in Figures 2(a) to 2(e) and 2(g) to 2(t)). The state domain is obtained. In other words, similar to the mechanisms shown in FIGS. 1(a) to 1(f), the difference in channel structure for feeding the light liquid phase and the heavy liquid phase does not affect the region of the emulsion mixed state. This was confirmed.

On the other hand, as the vertically elongated shape becomes more pronounced, the rotating shaft of the stirring blade 2 becomes longer, and shaft vibration and shaft runout become larger. By using , bearings, biaxial orthogonal gears, or a combination thereof, shaft vibration and shaft runout were significantly suppressed.

Similar to the mechanism of the conventional method, the container structure (multi-chamber mechanism) is separated into a mixer chamber 30 for stirring and mixing the heavy liquid phase 4 and light liquid phase 5 and a settler chamber 40 for phase separation of the two liquid phases. Also, a region of mixed emulsion was confirmed. FIG. 16 shows an area in an emulsified state that is generated by operating the mechanism shown in FIG. 4(e). In addition, in order to clarify the range of the mixer chamber 30 and the settler chamber 40, the range of the mixer chamber is clearly indicated by surrounding it with a broken line.

Similar to the emulsion mixed state region shown in FIG. 14, the region of the emulsion mixing state shown in FIG. Ta. On the other hand, in the container structure of FIG. 4(e) having a settler chamber, the emulsion mixed state (emulsion) moves from the mixer chamber 30 to the settler chamber 40 through the communication parts installed above and below the partition plate, Gravitational separation was possible at 40°C. In that case, although some turbidity occurred in the wastewater, it was possible to continue liquid-liquid extraction. In this respect, it can be said that the multi-chamber type has an advantage over the single-chamber type. Note that even if the emulsion flows into the settler chamber 40, the position of the interface between the two liquid phases remains almost unchanged before and after operation, and the heavy liquid phase 4 and light liquid phase 5 that participate in phase mixing remain the same. The volume ratio (so-called O/A ratio) was maintained.

The same emulsion mixing state can be applied not only to the mechanism shown in FIG. 4(e) but also to the mechanisms shown in FIGS. 4(a) to 4(d) and 4(f) to 4(p). area was obtained. That is, the light liquid phase 5 and the heavy liquid phase 4 are fed in the same way as the mechanism shown in FIGS. 1(a) to 1(t) and the mechanism shown in FIGS. 2(a) to 2(t). It was confirmed that the difference in channel structure does not affect the area of emulsion mixing state.

In addition, as a result of using the structures shown in Figures 5 (a1) to 5 (i2) for the communication parts installed above and below the partition plate, in each case, they functioned sufficiently as upper and lower communication parts, and large No difference was observed. As shown on the right side of each figure, the multi-chamber mechanism must be operated in a state where the liquid level of the light liquid phase 5 reaches the communication part (upper communication part) of the light liquid phase 5. If the light liquid phase 5 is operated in a state where the liquid level has not reached the communication area, only the heavy liquid phase 4 will move to the settler chamber 40 without the light liquid phase 5 being able to move to the settler chamber 40. It is no longer possible to maintain the position of the interface between the two liquid phases in the chamber. Note that if the liquid level of the light liquid phase 5 is set to be located below the communication area and an emulsion mixed state (emulsion) is developed to the bottom of the mixer chamber 30, the mechanism of the conventional method is different from that of the conventional method. Similarly, the ratio of the liquid feeding speeds of the two liquid phases corresponded to the volume ratio of both phases.

In addition, in the mechanism shown in FIGS. 4(a) to 4(p), the range (height) of the region of the emulsion mixed state is determined by the rotational speed of the stirring blade 2 and the amount of both phases, as in the single-chamber type. It depended on the liquid delivery rate. On the other hand, from FIG. 6(a) to FIG. 6(p), from FIG. 8(a) to FIG. 8(p), from FIG. 10(a) to FIG. 10(p), and from FIG. 12(a) As shown in FIG. 12(p), a vertical passage opening for the emulsion to move is formed by two partition plates (an upper partition plate and a lower partition plate). It has been found that by using this mechanism, the range (height) of the emulsion-mixed state region can be maintained almost constant regardless of changes in the rotational speed of the stirring blade 2 and the liquid feeding speed of both phases. That is, fluctuations in the range (height) of the emulsion mixed state (emulsion) in the mixer chamber 30 were suppressed. However, since the mechanism having the vertical passage port is based on moving the emulsion mixed state (emulsion) to the settler chamber 40, It was found that the phase separation ability was slightly reduced compared to the mechanism shown. In this regard, from FIG. 6(a) to FIG. 6(p), from FIG. 8(a) to FIG. 8(p), from FIG. 10(a) to FIG. 10(p), and from FIG. 12(a) ) to Figure 12(p), no major differences were observed.

Regarding the mechanisms shown in FIGS. 6(a) to 6(p), the range (height) of the area in the emulsion mixing state is shown in FIG. 17, with the channel structure in FIG. 6(e) as a representative. In addition, in order to clarify the range of the mixer chamber 30 and the settler chamber 40, the range of the mixer chamber 30 is clearly surrounded by a broken line. In this way, the range of the mixer chamber 30 was defined as the area in which the emulsion was mixed up to the outlet of the vertical passage port. 16 in that there is a communication area for the light liquid phase 5 near the ceiling surface of the container 1 and a communication area for the heavy liquid phase 4 near the bottom surface of the container 1.

Note that the same emulsion mixing method can be used for mechanisms other than those shown in FIG. 6(e) (the mechanisms shown in FIGS. 6(a) to 6(d) and 6(f) to 6(p)). The state domain is obtained. That is, the mechanisms shown in Figures 1(a) to 1(t), the mechanisms shown in Figures 2(a) to 2(t), and the mechanisms shown in Figures 4(a) to 4(p). Similarly, it was confirmed that the difference in the channel structure for feeding the light liquid phase 5 and the heavy liquid phase 4 did not affect the region of the emulsion mixed state.

Furthermore, regarding the communication area of the light liquid phase 5 formed by the upper partition plate located near the mixer chamber 30 and the communication area of the heavy liquid phase 4 formed by the lower partition plate 21 located near the settler chamber 40, FIG. 7 (a1) As a result of using the structures shown in FIG. 7(i2) through FIG. 7(i2), they functioned sufficiently as upper and lower communicating parts in all cases, and no major differences were observed.

FIG. 18 shows the range (height) of the region in the emulsion mixing state for the mechanisms shown in FIGS. 8(a) to 8(p), with the channel structure in FIG. 8(e) as a representative. Similar to FIGS. 16 and 17, the range of the mixer chamber 30 is clearly indicated by surrounding it with a broken line. 18 is similar to FIGS. 16 and 17 in that there is a communication area for the light liquid phase near the ceiling surface of the container 1 and a communication area for the heavy liquid phase 4 near the bottom surface of the container 1.

Note that the same emulsion mixing method can be used for mechanisms other than those shown in FIG. 8(e) (the mechanisms shown in FIGS. 8(a) to 8(d) and 8(f) to 8(p)). The state domain is obtained. That is, the mechanism shown in FIG. 1(a) to FIG. 1(t), the mechanism shown in FIG. 2(a) to FIG. 2(t), the mechanism shown in FIG. 4(a) to FIG. 4(p), Similarly to the mechanisms shown in FIGS. 6(a) to 6(p), the difference in the channel structure for feeding the light liquid phase 5 and the heavy liquid phase 4 affects the region of the emulsion mixed state. It was confirmed that it does not.

Furthermore, regarding the communication area of the heavy liquid phase 4 formed by the lower partition plate 21 located near the mixer chamber 30 and the communication area of the light liquid phase 5 formed by the upper partition plate 20 located near the settler chamber 40, FIG. As a result of using the structures shown in ) to FIG. 9(i), they functioned sufficiently as upper and lower communication parts in all cases, and no major differences were observed.

Regarding the mechanisms shown in FIGS. 10(a) to 10(p), FIG. 19 shows the range (height) of the area in the emulsion mixing state, with the channel structure in FIG. 10(e) being representative. Similar to FIGS. 16, 17, and 18, the range of the mixer chamber 30 is clearly indicated by surrounding it with a broken line. 19 is similar to FIGS. 16, 17, and 18 in that there is a communication area for the light liquid phase 5 near the ceiling surface of the container 1 and a communication area for the heavy liquid phase 4 near the bottom surface of the container 1. It is.

Note that the same emulsion mixing method can be used for mechanisms other than those shown in FIG. The state domain is obtained. That is, the mechanism shown in FIG. 1(a) to FIG. 1(t), the mechanism shown in FIG. 2(a) to FIG. 2(t), the mechanism shown in FIG. 4(a) to FIG. 4(p), Similar to the mechanisms shown in FIGS. 6(a) to 6(p) and the mechanisms shown in FIGS. 8(a) to 8(p), for feeding the light liquid phase 5 and the heavy liquid phase 4. It was confirmed that the difference in channel structure does not affect the area of emulsion mixing state.

In addition, the structure and arrangement of the lower partition plate 21 (left side of each figure) and the structure and arrangement of the upper partition plate 20 (right side of each figure), such as the structures shown in FIGS. 11(a1) to 11(i2). In each case, the communication site between the light liquid phase 5 and the heavy liquid phase 4 formed by the above sufficiently functioned as an upper and lower communication site, and no major differences were observed.

Regarding the mechanisms shown in FIGS. 12(a) to 12(p), FIG. 20 shows the range (height) of the region in the emulsion mixing state, with the channel structure in FIG. 12(e) as a representative. Similar to FIGS. 16, 17, 18, and 19, the range of the mixer chamber 30 is clearly indicated by surrounding it with a broken line. 16, 17, 18, and 20 in that there is a communication area for the light liquid phase 5 near the ceiling surface of the container 1 and a communication area for the heavy liquid phase 4 near the bottom surface of the container 1 in FIG. It is the same as 19.

Note that the same emulsion mixing method can be used for mechanisms other than those shown in FIG. The state domain is obtained. That is, the mechanism shown in FIG. 1(a) to FIG. 1(t), the mechanism shown in FIG. 2(a) to FIG. 2(t), the mechanism shown in FIG. 4(a) to FIG. 4(p), Similar to the mechanism shown in Figures 6(a) to 6(p), the mechanism shown in Figures 8(a) to 8(p), and the mechanism shown in Figures 10(a) to 10(p). Furthermore, it was confirmed that the difference in the channel structure for feeding the light liquid phase 5 and the heavy liquid phase 4 did not affect the region of the emulsion mixed state.

In addition, the structure and arrangement of the lower partition plate (on the left of each figure) and the structure and arrangement of the upper partition plate (on the right of each figure), such as the structures shown in FIGS. 13(a1) to 13(i2), In both cases, the communication site between the light liquid phase 5 and the heavy liquid phase 4 functioned sufficiently as an upper and lower communication site, and no major differences were observed.

Comparative example 1

A multi-chamber system in which one of the communication parts for the heavy liquid phase or the light liquid phase is missing.

A feature of the present invention is that in the container 1 or the room (mixer chamber 30) where two liquid phases are mixed, a region in an emulsion mixture state and a region in a phase separation state coexist, and the mixer chamber 30 and the settler chamber 40, both the phase-separated heavy liquid phase 4 and light liquid phase 5 communicate between both chambers. As a comparison, a case where only either the heavy liquid phase 4 or the light liquid phase 5 communicated with both chambers was investigated.

First, if there is a communicating area only for the phase-separated heavy liquid phase 4, use the mechanism shown in FIG. We considered operating the system in a state where the target level was not reached. As shown in Example 1, only the heavy liquid phase 4 moves to the settler chamber 40 while the light liquid phase 5 cannot move to the settler chamber 40, so the position of the interface between the two liquid phases cannot be maintained in both chambers. lost.

Next, we modified the mechanism shown in FIG. 4(e) to consider a case where a communicating portion was provided only to the phase-separated light liquid phase 5. That is, the mechanism shown in FIG. 4E, which has a communicating portion between the bottom of the container 1 and the partition plate, was modified to a mechanism in which the entire lower end of the partition plate is joined to the bottom of the container. Using this modified mechanism, it was operated with the liquid level of the light liquid phase 5 reaching the communication area between the container ceiling surface and the partition plate. As a result, only the light liquid phase 5 moved to the settler chamber without the heavy liquid phase 4 being able to move to the settler chamber, making it impossible to maintain the position of the interface between the two liquid phases in both chambers.

Comparative example 2

In a multi-chamber system, there is a horizontal passageway in addition to the communication area between the upper and lower chambers.

In the multi-chamber system shown in FIGS. 4(a) to 4(p), as in the single-chamber system, the range (height) of the region of the emulsion mixed state (emulsion) is determined by the rotational speed of the stirring blade 2. and the liquid feeding speed of both phases, but in order to suppress these effects, it is effective to provide a passage port between the mixer chamber 30 and the settler chamber 40 for moving the emulsion mixed state. . Therefore, with respect to the partition plate shown in FIG. 4(e), a perforated partition plate 24 having passage ports (horizontal passage ports) in addition to the upper and lower chamber communication portions was installed. The mechanism is shown in FIG. 21.

With the mechanism shown in FIG. 21, it was possible to suppress the influence of the rotational speed of the stirring blade 2 and the liquid feeding speed of both phases on the range (height) of the region of the emulsion mixed state (emulsion). However, on the other hand, the emulsion mixed phase (emulsion phase) generated near the blade part of the stirring blade 2 in the mixer chamber 30 immediately moves to the settler chamber 40 through the horizontal passage port. 30, the emulsion phase could not be sufficiently developed, and a large amount of emulsion flowed into the settler chamber 40, which adversely affected phase separation. FIG. 22 shows the emulsion mixed state (emulsion) when the mechanism shown in FIG. 21 is operated.

Confirmation of constancy of the interface position between two liquid phases in a multi-chamber system.

In the multi-chamber system, the interface between the two liquid phases was always at the same location in the mixer chamber 30 and the settler chamber 40. In addition, the position remained unchanged regardless of fluctuations in the liquid feeding speeds of both phases and no matter how long the system was operated. Specifically, FIGS. 4(a) to 4(p), FIGS. 6(a) to 6(p), FIGS. 8(a) to 8(p), and FIGS. 10(a) to 10( The invariance of the interface position between the two liquid phases was confirmed for the mechanisms shown in p) and FIGS. 12(a) to 12(p).

On the other hand, the mechanism of the conventional method is also a multi-chamber type consisting of a mixer chamber and a settler chamber, but the interface position between the two liquid phases does not necessarily match in both chambers. Furthermore, it is known that the position of the interface changes due to fluctuations in the liquid feeding speed of both phases, and that the position gradually changes due to long-term operation, requiring adjustment work on a daily basis. .

Confirmation of the independence of the ratio of liquid feeding speeds of the two liquid phases and the O/A ratio.

In the mechanism of the present invention, the liquid feeding speeds of the heavy liquid phase 4 and the light liquid phase 5 could be set independently of the volume ratio of both phases participating in phase mixing (so-called O/A ratio). Specifically, FIGS. 1(a) to 1(t), FIGS. 2(a) to 2(t), FIGS. 4(a) to 4(p), and FIGS. 6(a) to 6( p), FIGS. 8(a) to 8(p), FIGS. 10(a) to 10(p), and FIGS. 12(a) to 12(p), the heavy liquid phase 4 The ratio between the liquid feeding speed of the light liquid phase 5 and the liquid feeding speed of the light liquid phase 5 was varied from 1:1 to 1:10. It was found that the position of the interface did not change before and after operation. That is, the independence of the ratio of the liquid feeding speeds of the two liquid phases and the O/A ratio was confirmed.

Occurrence of emulsion mixed state and its stability.

For the mechanism shown in FIG. 8(m), ion exchange water (pure water) or 0.1M nitric acid aqueous solution was used as the heavy liquid phase 4, and the above-mentioned alkane solvent (ShellSol D70), toluene, Using methyl isobutyl ketone (MIBK) or n-octanol, experiments were conducted regarding the generation of an emulsified mixed state and its stability. As will be described later, in the conventional method, it took a considerable amount of time (usually several minutes to several hours) for the emulsion mixture of heavy liquid phase 4 and light liquid phase 5 to stabilize, but with this mechanism, It was possible to instantly (in a few seconds to about 1 minute) bring both phases into an emulsified state. That is, while feeding and introducing the heavy liquid phase 4 from above and the light liquid phase 5 from below into the container 1 or room (mixer chamber 30) for phase mixing, the stirring blades 2 installed near the interface between the two liquid phases are introduced. By rotating the wing portion, both phases could be immediately brought into an emulsion.

Furthermore, as will be described later, it was found that the rotational speed of the stirring blade 2 required to obtain a stable emulsion mixing state can be much slower than in the case of the conventional method (two-thirds of the rotation speed of the conventional method). (about half the rotation speed). Furthermore, droplet observation using a high-speed camera confirmed that the emulsion mixture obtained by this mechanism is denser and more homogeneous than that obtained by conventional methods. The difference in the emulsion mixing state was also obvious from visual observation, and no change was observed during operation even after a long period of time. On the other hand, the emulsion mixed state generated by the conventional method may change over a long period of time.

Note that depending on the type of extraction solvent phase (in many cases, a light liquid phase), it may be difficult to form an emulsion phase only by mechanical stirring based on the rotation of a stirring blade. This tendency was particularly observed when a polar organic solvent such as n-octanol was used. In that case, it has been found that the formation of an emulsion phase is facilitated by conveying the heavy liquid phase or the light liquid phase, or both, through a nozzle having pores or capillaries.

Comparative example 3

Comparison of generation of emulsion mixed state and its stability with conventional method.

A mechanism corresponding to the conventional method shown in FIG. 23 was created and compared with the mechanism shown in FIG. 8(m). The heavy liquid phase 4 and light liquid phase 5 used were the same as in Example 4. With the mechanism shown in Figure 8(m), it was possible to bring both phases into an emulsion-mixed state within a few seconds to a minute, whereas with the mechanism shown in Figure 23, the emulsion-mixed state of both phases was stabilized. It took several minutes to several hours. Furthermore, in the mechanism shown in Fig. 23, in order to obtain a stable emulsion mixing state, it is necessary to increase the rotational speed of the stirring blade 2 by 1.5 to 2 times compared to the mechanism shown in Fig. 8 (m). Ta. In the conventional method, it is necessary to reach a homogeneous emulsion mixed state throughout the mixer chamber, but if the rotation speed of the stirring blade 2 is insufficient, the emulsion mixed state becomes heterogeneous with dense areas and sparse areas. As a result of the generation of an emulsion phase, the interface position between the two liquid phases changed. Further, depending on the solvent, a stable emulsion mixed state may not be achieved in some cases. In particular, highly polar solvents such as alcohol tended to have difficulty developing an emulsion phase.

Confirmation of the independence of the rotational speed of the stirring blade and the liquid feeding speed of the two liquid phases.

In the conventional method (multi-chamber type), an increase in the rotational speed of the stirring blade 2 generates stronger shearing force, which tends to generate minute droplets that are difficult to coalesce, resulting in phase separation of the emulsion phase. Therefore, it is necessary to suppress the transfer of the emulsion phase to the settler chamber. The transition to the room is facilitated.

It has been found that in the mechanism of the present invention, the liquid feeding speeds of the heavy liquid phase and the light liquid phase can be set completely independently of the rotational speed of the stirring blade 2. Specifically, FIGS. 1(a) to 1(t), FIGS. 2(a) to 2(t), FIGS. 4(a) to 4(p), and FIGS. 6(a) to 6( p), FIGS. 8(a) to 8(p), FIGS. 10(a) to 10(p), and FIGS. 12(a) to 12(p), the stirring blade 2 As a result of examining the relationship between the rotational speed and the feeding speed of the two liquid phases, it was confirmed that the two are independent.

Confirmation of improvement in phase separation.

It has been found that in the mechanism of the present invention, the phase separation property is improved by simultaneous progress of phase separation in the container 1 or the room (mixer chamber 30) for mechanical stirring. Specifically, FIGS. 1(a) to 1(t), FIGS. 2(a) to 2(t), FIGS. 4(a) to 4(p), and FIGS. 6(a) to 6( p), FIG. 8(a) to FIG. 8(p), FIG. 10(a) to FIG. 10(p), and FIG. 12(a) to FIG. 12(p), the mechanism shown in FIG. When compared with the conventional method, it was confirmed that the phase separation property was significantly improved. In addition, high phase separation means that the processing speed can be increased, and if the same processing speed as when using the mechanism of the present invention is set for the mechanism of Fig. 23, the settler chamber 40 immediately became extremely cloudy and became difficult to drain.

Extraction and separation experiment of rare earth elements.

An experiment was conducted to extract and separate two rare earth elements, neodymium (Nd) and samarium (Sm) from an aqueous nitric acid solution using an alkyl diamide amine (ADAAM) using the mechanism shown in FIG. 4(e) of the present invention. Specifically, a ShellSol D70 solution containing 0.25 M (mol dm-3) ADAAM was used as a light liquid phase, and neodymium (Nd) dissolved in a 1.5 M nitric acid aqueous solution (heavy liquid phase) was used. Samarium (Sm) was extracted and separated into a light liquid phase. Note that ADAAM is a molecular extractant with excellent selective separation ability between rare earth elements, and is particularly suitable for separating medium rare earth elements such as the separation of Nd and Sm, which are adjacent to each other in the periodic table.

For comparison, a test tube batch experiment (batchwise experiment) was conducted using the same heavy liquid phase (aqueous phase) and light liquid phase (oil phase) as described above. Pour the same volume of heavy liquid phase 4 and light liquid phase 5 into a test tube with a stopper, shake thoroughly using a vertical shaker to reach extraction equilibrium, and then separate the two liquids using a centrifuge. The phases were separated. In addition, extraction equilibrium was considered to have been reached when the distribution ratio (the value obtained by dividing the concentration of rare earth elements in the oil phase by the concentration of rare earth elements in the water phase) did not change with respect to the shaking time. .

Regarding the extraction and separation of Sm from Nd using the molecular extractant ADAAM, the results of an experiment using the mechanism shown in FIG. 4(e) will be compared with the results of a test tube batch experiment. As a result of the experiment using the structure shown in FIG. 4(e), the distribution ratio of Nd was 8.5 and the distribution ratio of Sm was 0.38. On the other hand, as a result of the batch experiment, the distribution ratio of Nd was 5.9 and the distribution ratio of Sm was 0.42.

The value of the separation coefficient of Nd from Sm (the value obtained by dividing the distribution ratio of Nd by the distribution ratio of Sm) is 22.4 in the experiment using the mechanism shown in Figure 4(e), and 14.1 in the batch experiment. became. Since the results of the batch experiment are the results at extraction equilibrium, it was found that the mechanism shown in FIG. 4(e) provides a separation coefficient larger than that at extraction equilibrium. This result is considered to be due to the increase in the number of theoretical plates due to countercurrent contact between the heavy liquid phase (aqueous phase) and light liquid phase (oil phase) based on counter-feeding of the two phases.

In addition, even with the conventional method using the mechanism shown in Figure 23, as a result of conducting an experiment using the same heavy liquid phase (aqueous phase) and light liquid phase (oil phase) as described above, the distribution ratio of Nd was 3.2 and Sm The distribution ratio was 0.23. That is, the separation coefficient of Nd from Sm was 13.9, which was approximately the same value as the result of the batch experiment (result at extraction equilibrium).

Adaptability to circulating fluid delivery.

It was found that while the conventional liquid feeding mechanism using overflow is not suitable for circulating liquid feeding, the liquid feeding mechanism using pressure action of the present invention is highly adaptable to circulating liquid feeding. . Specifically, from FIG. 1(a) to FIG. 1(o), FIG. 2(a) to FIG. 2(o), FIG. 4(a) to FIG. 4(l), and FIG. 6(a) to By the mechanism shown in FIG. 6(l), FIG. 8(a) to FIG. 8(l), FIG. 10(a) to FIG. 10(l), and FIG. 12(a) to FIG. 12(l). It was confirmed that it was easy to circulate the heavy liquid phase 4, the light liquid phase 5, or both phases.

In addition, in addition to being able to easily circulate liquid by switching from liquid feeding by overflow to liquid feeding by pressure action, the mechanism of the present invention also allows for the separation of heavy liquid phase 4 and light liquid phase 5, which participate in phase mixing. The fact that the volume ratio (so-called O/A ratio) can be set independently of the liquid feeding rate is also one of the factors that facilitates circulating liquid feeding. In other words, the O/A ratio remains unchanged, and the ratio of the liquid delivery speeds of the two liquid phases can be freely set, so for example, when heavy liquid phase 4 (in most cases, the aqueous phase) is fed in a single pass method, Processing can proceed while permanently maintaining a stable emulsion phase under conditions where the liquid feeding rate for circulating the light liquid phase 5 (in most cases, the oil phase) is significantly increased compared to the liquid feeding rate of . I understand.

A mechanism adapted to circulating fluid delivery has various advantages. For example, the above-mentioned circulating liquid feeding mechanism in the present invention is effective when dealing with systems with slow extraction speeds or low extraction rates, and it integrates forward extraction, washing, and back extraction in a synchronous manner. It was confirmed that it can also be used for the multi-stage effect caused by circulating liquid feeding, and multi-stage synchronous circulating liquid feeding (Japanese Patent Application No. 2019-113657). In addition, in cases of difficult separation or precise separation that require multiple stages, by using multiple stages of synchronous circulation, the equipment system can be significantly downsized compared to the conventional mixer-settler method (multi-stage system). I also found out that it is possible.

Based on the results shown in the above-mentioned Examples and Comparative Examples, the following considerations can be made. First, with this mechanism, a stable emulsion phase can be grown more efficiently and over a wider range than with conventional methods. In other words, the heavy liquid phase introduced from above reaches the emulsion phase only after passing through the light liquid phase without contacting other heavy liquids, and the light liquid phase introduced from below reaches the emulsion phase only after passing through the light liquid phase without contacting other heavy liquids. It reaches the emulsion phase only after passing through the heavy liquid phase without contacting the liquid. Therefore, the volume ratio of the heavy liquid phase to the light liquid phase in the emulsion phase can always be stably maintained in a substantially constant state.

Furthermore, since the heavy liquid phase flows from the top to the bottom and the light liquid phase flows from the bottom to the top, both phases inevitably come into countercurrent contact. This increases the number of theoretical plates as well as many column type extraction devices (eg spray columns, pulse columns, emulsion flow).

Now, in the conventional method, the heavy liquid phase and light liquid phase that have been stirred and mixed are sent unilaterally from the mixer chamber to the settler chamber through one route due to overflow, so the heavy liquid phase The ratio of the liquid feeding speed of the light liquid phase and the light liquid phase directly becomes the volume ratio of the two liquid phases existing in the mixer chamber. In other words, it is not possible to change the volume ratio of both phases that participate in phase mixing while maintaining the ratio of the liquid feeding speeds of the heavy liquid phase and the light liquid phase. Also, the ratio of the liquid feeding speed cannot be changed. That is, the degree of freedom in operation is small in that it can only be operated within the constraint (restriction) that the volume ratio of the heavy liquid phase and the light liquid phase and the ratio of the liquid feeding speeds of both phases match. On the other hand, in a single-chamber system, a region in which the emulsion phase is generated and a region in which the emulsion phase has disappeared coexist within one container used for stirring and mixing two liquid phases, so that one container can It serves as both a mixer room and a settler room in the conventional method. In this case, the volume ratio of the two liquid phases present in the container becomes independent of the liquid feeding rate. In the case of a mixer room with a multi-chamber system, unlike the mixer room of the conventional method, the region where the emulsion phase is generated and the region where it disappears coexist in the mixer room, similar to the single-chamber system described above. However, since it communicates with the settler chamber, the volume ratio of the two liquid phases present in the mixer chamber is independent of the liquid feeding rate (details will be described later).

In other words, in the conventional method, if the ratio of the liquid feeding speeds of the heavy liquid phase and the light liquid phase is the same, the volume ratio of the heavy liquid phase and the light liquid phase existing in the mixer chamber does not change. If the liquid phase and the light liquid phase are contained in one container, and the introduction speed and discharge speed of the heavy liquid phase and the introduction speed and discharge speed of the light liquid phase are the same, the liquid phase exists in the container. The volume ratio of the two liquid phases does not change. In fact, the heavy liquid phase and the light liquid phase are introduced separately and mixed in the container, but again they are separated into the heavy liquid phase and the light liquid phase and discharged separately, so the introduction rate of both phases is and the discharge rate are always consistent. In other words, since the entrance and exit of both phases are controlled at the inlet (inlet) and outlet (outlet) (because the same volume of liquid phase is discharged as the volume introduced), The volume ratio of both phases installed in the container is maintained without being affected by the liquid feeding rate. In this case, the liquid feeding rate by a pump or the like is the introduction rate and also the discharge rate. That is, the liquid feeding rate of the heavy liquid phase (=introduction rate=discharge rate) and the liquid feeding rate of the light liquid phase (=introduction rate=discharge rate) can be freely set regardless of the volume ratio of both phases. This also means that the position of the interface between the heavy liquid phase and the light liquid phase within the container is independent of the liquid feeding speed of both phases.

In addition, when the liquid is sent unilaterally from the mixer chamber to the settler chamber by one route due to overflow, the heavy liquid phase and the light liquid phase are introduced into the mixer chamber separately, but on the other hand, the two phases are not separated and are transferred to the mixer chamber. At the exit from the mixer chamber (inlet to the settler chamber), individual control for each liquid phase does not work, as the heavy liquid phase (or light liquid phase) introduced into the mixer chamber The volume of the heavy liquid phase (or light liquid phase) transferred from the mixer chamber to the settler chamber does not necessarily match. For example, when starting operation after installing a heavy liquid phase and a light liquid phase in the mixer chamber, if the ratio of the liquid feeding speed of both phases and the volume ratio of both phases at the time of installation are different, the difference between the two phases in the mixer chamber. The volume ratio changes gradually. Therefore, in the conventional method (overflow method), operation is usually started with the mixer chamber empty.

In addition, the mechanism of the present invention, in which regions in which the emulsion phase is generated and regions in which it disappears coexist within one container used for stirring and mixing the heavy liquid phase and the light liquid phase, is superior to the conventional method in terms of phase separation. It's better than a system. In the conventional method, it is necessary to maintain the volume ratio of the heavy liquid phase to the light liquid phase at the time of introduction into the mixer room in the emulsion phase that moves from the mixer room to the settler room. It is preferable that both phases are stirred and mixed homogeneously throughout, but this is also the cause of poor phase separation. In contrast, in the system of the present invention, in which phase mixing and phase separation occur simultaneously within one container by mechanical stirring, it is not necessary that stirring and mixing occur homogeneously throughout the container, and phase separation occurs from the beginning. Therefore, the phase separation property is significantly improved compared to the conventional method.

Furthermore, in the case of the mechanism of the present invention, the heavy liquid phase and the light liquid phase do not necessarily need to be fed in a single pass mode, but may be fed in a circulation mode. The conventional liquid feeding mechanism using overflow is not suitable for circulating liquid feeding, but the mechanism of the present invention is rather suitable for circulating liquid feeding. Circulating liquid feeding is effective when dealing with systems where the extraction rate is slow or the extraction rate is small. In addition, such a mechanism adapted to circulating liquid feeding has a multi-stage effect produced by integrating forward extraction, washing, and back extraction and synchronously circulating liquid feeding, and a multi-stage synchronous circulating liquid feeding system (patent application 2019- 113657) can also be used. In cases of difficult or precise separation that require multiple stages, the use of multiple stages of synchronous circulation liquid feeding allows the equipment system to be significantly downsized compared to the conventional multi-stage method (multi-stage container number).

The mechanism, which has the many excellent features mentioned above, is similar to the mechanism of conventional methods, and has a container structure that is separated into a mixer chamber where the heavy liquid phase and light liquid phase are stirred and mixed, and a settler chamber where the two phases are separated. can also be applied. In other words, communication parts are provided in two places, between the ceiling surface and the partition plate of the container housing the mixer room and the settler room, and between the bottom surface and the partition plate, so that the heavy liquid phase and the light liquid phase can freely flow back and forth between the two chambers. By doing so, it can be handled in the same way as a container structure that is not divided into a mixer chamber and a settler chamber. At this point, the stirred and mixed heavy liquid phase and light liquid phase are unilaterally sent from the mixer chamber to the settler chamber by one route by the overflow (both phases come and go between the mixer chamber and the settler chamber). (not possible) is fundamentally different from the mechanism of conventional law.

In other words, the mechanism of the conventional method and the mechanism of the method of the present invention differ only in the arrangement of the blade parts of the stirring blades, the structure of the partition plate, and the positions of the inlets for the heavy liquid phase and light liquid phase. Therefore, it is easy to modify the mechanism of the conventional method based on the method of the present invention. In conventional method systems, the position of the liquid level (interface between the light liquid phase and gas phase) or the interface between the two liquid phases is often different between the mixer chamber and the settler chamber. In particular, the position of the interface between the two liquid phases is Since it tends to gradually fluctuate as the operation continues, its position must be adjusted periodically or from time to time. However, if the conventional device is modified according to the present invention, the phase-separated heavy liquid phase and light liquid phase can freely move back and forth between the mixer chamber and the settler chamber. (a) are the same, and since the interface between the two liquid phases in the settler chamber is always maintained at the same position without fluctuation, no adjustment work is required.

In addition, in the conventional method (overflow method), the volume ratio of the heavy liquid phase to the light liquid phase (so-called O/A ratio) in the mixer chamber corresponds to the ratio of liquid feeding speeds. Therefore, if you want to mix the two liquid phases more efficiently and effectively by placing the blade part of the stirring blade near the interface between the two phases, the length of the rotation axis of the stirring blade should be adjusted according to the liquid feeding speed condition. It is necessary to adjust the On the other hand, if the structure of the partition plate is improved so that the phase-separated heavy liquid phase and light liquid phase can freely move between the mixer chamber and the settler chamber, it is possible to adapt to such operating conditions. There is no need to adjust the length of the rotating shaft. For example, while maintaining the interface position in the mixer chamber at the position where the volume ratio of the heavy liquid phase to the light liquid phase is 1:1, the liquid feeding speeds of both phases can be freely set independently.

Furthermore, in the mechanism of the present invention, the strength of phase mixing and the liquid feeding rate are completely independent. In the conventional method, the rotational speed of the stirring blade affects the liquid feeding speed, which requires complicated and skillful adjustment work that takes into account the interlocking of the two.However, in the method of the present invention, the rotational speed of the stirring blade and the liquid feeding speed Since they are independent, the adjustment work is greatly reduced.

In the above explanation, the upper part, the lower part, or both of the container have a shape (overhanging shape) with a larger cross-sectional area than the middle part of the container, so that the heavy liquid phase and the light liquid phase can be separated. It has a structure that promotes phase separation. However, it is also possible to promote the phase separation by partially enlarging the cross-sectional area of the middle part of the container compared to the cross-sectional areas of the upper and lower parts and attaching stirring blades of large diameter there.

The present invention relates to a method for producing a substance to be separated and purified based on industrial liquid-liquid extraction using mechanical stirring. Liquid-liquid extraction is a method for separating substances such as metal ions, organic compounds, and biopolymers based on differences in the distribution of substances between two immiscible liquid phases, and is widely used industrially. There is. In particular, it is often used for so-called advanced separations, such as separation between substances that have similar chemical properties and are said to be difficult to separate, and high-precision separation that requires highly pure substances.

In industrial liquid-liquid extraction, mechanical agitation is generally used for phase mixing of a heavy liquid phase (often an aqueous phase) and a light liquid phase (often an oil phase), e.g. The settler method is a method that is said to be synonymous with liquid-liquid extraction, but its equipment has various settings that are difficult to handle, poor phase separation, and the volume ratio of the two liquid phases that participate in phase mixing (so-called O/A ratio). There were problems such as a low degree of separation and an increase in the size of the system due to the high-level separation requiring multiple stages. By using the method of the present invention, the above-mentioned problems faced by the current liquid-liquid extraction using mechanical stirring can be solved, so it is thought that the industrial applicability of liquid-liquid extraction will further expand.

1: Container 2: Stirring blade 3: Turbidity prevention partition 4: Heavy liquid phase 5: Light liquid phase 6: Heavy liquid phase liquid feeding line 7: Light liquid phase liquid feeding line 8: Pump for heavy liquid phase 9: Light liquid phase Liquid phase pump 10: Heavy liquid phase passage 11: Heavy liquid phase passage partition plate 12: Light liquid phase passage 13: Light liquid phase passage partition plate 14: Shaft holder, bearing, or two-axis orthogonal gear 15: M chamber/S Room partition plate 16: Ceiling surface/partition plate communication area 17: Bottom surface/partition plate communication area 18: Passage port at upper end of partition plate 19: Passage port at lower end of partition plate 20: Upper partition plate 21: Lower partition plate 22: Vertical passage port 23: Emulsion mixed state area 24: Perforated M chamber/S chamber partition plate 25: Horizontal passage port 26: Upper joint partition plate 27: Lower joint partition plate 30: Mixer chamber 40: Settler chamber 100: interface

Claims (4)

Inside the container, a stirring blade and both phases, a heavy liquid phase and a light liquid phase, are installed so that they have the same volume, and the blade portion of the stirring blade is located above and below the interface between the two phases. A first container disposed within a range of three times the thickness of the site, and a second container for back-extracting a specific substance from the light liquid phase sent from the first container. Prepare at least two containers,
While rotating the stirring blade and stirring both phases by the blade portion of the stirring blade, the heavy liquid phase is introduced from above the first container and the light liquid phase is introduced from the bottom of the first container. A state in which both phases are emulsified and mixed and a state in which they are phase separated coexist in a container.
A light liquid phase existing in the upper part of the first container in a phase-separated state is fed into the heavy liquid phase from below a second container containing a heavy liquid phase which is a reverse extraction liquid,
A liquid-liquid extraction characterized in that the reset light liquid phase obtained from above the second container is returned to the first container again, and the specific substance is recovered in the back extraction liquid in the second container. Extraction and recovery method of specific substances based on In claim 1, the cross-sectional area of the upper or lower part of the first container, or both, is made larger than the cross-sectional area of the intermediate portion of the container to promote phase separation between the heavy liquid phase and the light liquid phase. A method for extracting and recovering specific substances based on liquid-liquid extraction, characterized by: 3. The method for extracting and recovering a specific substance based on liquid-liquid extraction according to claim 1 or 2, characterized in that the heavy liquid phase and the light liquid phase are fed in one pass. The identification based on liquid-liquid extraction according to any one of claims 1 to 3, characterized in that the heavy liquid phase, the light liquid phase, or both are fed and introduced through a nozzle having pores or thin tubes. Method for extracting and recovering substances.