Extraction and recovery device for specific substances based on liquid-liquid extraction

Abstract

To provide a device 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: A device includes an agitation vane having a vane part located in the vicinity of an interface between a heavy liquid phase and a light liquid phase in a container, introduces a phase-separated liquid phase formed simultaneously with an emulsion mixed state in the same container, into a back-extraction liquid of another container, and extracts and recovers a specific substance in the other container.SELECTED DRAWING: Figure 1(p)

Description

[Technical field]

[0001] The present invention relates to an apparatus for extracting and recovering a specific substance based on liquid-liquid extraction, and more specifically, to an apparatus for extracting and recovering a specific substance that grows an emulsion phase (two-liquid emulsion mixture phase) by countercurrently contacting a heavy liquid phase (often an aqueous phase) and a light liquid phase (often an oil phase) in a vessel for phase mixing, while simultaneously separating the two phases (phase separation), thereby obtaining a specific substance that is separated and purified in the heavy liquid phase, the light liquid phase, or both phases. In particular, the present invention relates to an apparatus for extracting and recovering a specific substance based on liquid-liquid extraction that can efficiently phase mix the heavy liquid phase and the light liquid phase to easily obtain an emulsion phase that is stable over a wide range. [Background technology]

[0002] Liquid-liquid extraction (also called solvent extraction) can be used to separate and concentrate target components in an aqueous solution, or to separate and remove impurities from the target components, to obtain high-quality metal products, chemical products (organic compounds, etc.), etc. Liquid-liquid extraction is a method for separating, purifying, and concentrating metal ions, organic compounds, biopolymers, etc., by utilizing the difference in the distribution of substances between two immiscible liquid phases (for example, an aqueous phase and an oil phase), and is widely used industrially.

[0003] Separation based on liquid-liquid extraction can involve many chemical reactions, such as complexation reactions, dehydration reactions, solvation reactions, ion-exchange reactions, acid-base reactions, redox reactions, catalytic reactions, and self-organization reactions, depending on the target compound.

[0004] In fact, when liquid-liquid extraction is carried out industrially, the mixer-settler method is often used, in which two liquid phases are mixed by rotating agitator blades, and then the two liquid phases are transported to a separate chamber and separated by gravity. The mechanism of liquid-liquid extraction based on the mixer-settler method is the most widespread device representing industrial liquid-liquid extraction because it has a relatively simple structure and stable performance.

[0005] In the mechanism of the conventional mixer-settler apparatus (hereinafter simply referred to as the conventional apparatus), the position of the interface between the two liquid phases is easily changed, and it requires skill to handle it, such as adjusting the interface position. In addition, the ratio of the liquid delivery speeds of the two liquid phases is the volume ratio of both phases involved in the phase mixing (so-called O / A ratio). For example, if you want to increase the liquid delivery speed of the aqueous phase containing the target component in order to increase its processing speed, you must also increase the liquid delivery speed of the oil phase at the same time, otherwise the volume ratio of both phases will change.

[0006] In the mechanism of the conventional device, both the aqueous phase and the oil phase are supplied from the bottom of the mixer chamber through inlets adjacent to each other, and the two phases are immediately mixed and stirred by the mixing blade part (the blade part located at the tip of the rotating shaft) installed below the mixer chamber. In addition, a front chamber into which the aqueous phase and the oil phase are introduced is provided at the bottom of the mixer chamber, and a mechanism is also known as a general mixer settler device in which the two phases are introduced from the front chamber into the mixer chamber through a passage provided in a partition plate between the front chamber and the mixer chamber, by using the negative pressure generated by the rotation of the mixing blade to suck up the two phases (Patent Document 1, Figure 3 of Patent Document 2). [Prior art documents] [Patent documents]

[0007] [Patent Document 1] Special Publication No. 61-19281 [Patent Document 2] Patent No. 6119029 Summary of the Invention [Problem to be solved by the invention]

[0008] When the aqueous phase is a heavy liquid phase and the oil phase is a light liquid phase, both the aqueous phase and the oil phase are supplied into the aqueous phase, and the impeller portion of the impeller is located in the aqueous phase directly above the inlets of both phases. In this way, both phases are introduced into the aqueous phase (heavy liquid phase) and are immediately stirred in the aqueous phase, so that the stirring and mixing inevitably involves the surrounding aqueous phase. Therefore, the emulsion mixing state may be insufficient or a stable state may not be maintained over a wide area. In addition, in the type with a front chamber, the oil phase remains at the top of the front chamber, which helps to increase the ratio of the oil phase by suction, but the volume ratio of the two phases actually mixed is not stable.

[0009] There is also a structure in which both phases are introduced from the top of the mixer chamber and the stirring blade portion is located at the bottom of the mixer chamber (Fig. 1 of Patent Document 2), but since the blade portion of the stirring blade is located at the bottom of the mixer chamber where the heavy liquid phase is rich, there is a similar tendency for the proportion of the heavy liquid phase to be large at the beginning of mixing of the two liquid phases.

[0010] As described above, the mechanism of the conventional device is a system in which 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 devices that introduce the heavy liquid phase from the top and the light liquid phase from the bottom. In a system in which the heavy liquid phase and the light liquid phase flow in opposite directions, more efficient extraction is possible due to countercurrent contact of the two phases. Conventional column-type liquid-liquid extraction devices (e.g., spray column type, pulse column type, etc.) have a lower two-liquid phase mixing capacity than mixer settlers that use stirring blades, but can be expected to improve the number of theoretical plates based on countercurrent contact of the two phases.

[0011] In addition, the mechanism of the conventional device has the advantage that the liquid can be delivered without relying on a pump because the suction force generated by the rotation of the impeller is used to deliver the liquid. In other words, the load on the pump can be significantly reduced by the rotation of the impeller, but on the other hand, there is a problem that the delivery speed changes depending on the difference in the mixing strength of the two liquid phases (difference in the rotation speed of the impeller, etc.).

[0012] While the mechanism of conventional equipment has a relatively simple structure and provides stable performance, it has problems such as difficulty in handling due to the tendency for the interface position to change (requiring skilled handling), non-independence of the volume ratio of the two liquid phases involved in phase mixing (dependent on the ratio of the liquid flow rates of the two phases), inefficient two-liquid phase mixing that is prone to resulting in an abundance of the heavy liquid phase (lack of the light liquid phase), and the effect of the rotation of the agitator blades on the liquid flow rate.

[0013] The object of the present invention is to provide an apparatus for extracting and recovering a specific substance based on liquid-liquid extraction, which solves the above-mentioned problems and enables a specific substance to be separated and purified in a heavy liquid phase, a light liquid phase, or both phases, to exhibit innovative features that cannot be obtained by the mechanisms of conventional apparatuses. [Means for solving the problem]

[0014] According to one aspect of the present invention, there is provided an apparatus for extracting and recovering a specific substance based on liquid-liquid extraction, the apparatus comprising: a first vessel in which a heavy liquid phase and a light liquid phase are placed; a first liquid introducing means for introducing a heavy liquid phase from above the first vessel; a second liquid introducing means for introducing a light liquid phase from below the first vessel; a stirring means equipped with a stirring blade having a blade portion for stirring the heavy liquid phase and the light liquid phase in the first vessel; a second vessel in which a stripping liquid for recovering a specific substance is placed; a first pipe connected to an upper part of the first vessel and a lower part of the second vessel in order to transfer the light liquid phase present in the upper part of the first vessel into the stripping liquid in the second vessel; and a second pipe for returning the light liquid phase from the upper part of the second vessel to the lower part of the first vessel, The heavy liquid phase and the light liquid phase in the first vessel are arranged to have the same volume, and the blade portion of the stirring blade located at the tip of the rotating shaft is arranged at a distance of up to three times the thickness of the blade portion in either the up or down direction from the interface between the heavy liquid phase and the light liquid phase in the first vessel, While rotating the stirring blade, the heavy liquid phase is introduced from above the first vessel and the light liquid phase is introduced from below, thereby allowing both phases to coexist in the first vessel in an emulsion state and a phase-separated state, and the light liquid phase containing a specific substance that is present in the upper part of the first vessel in a phase-separated state is introduced from below into the second vessel containing the heavy liquid phase that is a stripping liquid, and the reset light liquid phase obtained from above the second vessel is returned to the first vessel, and the specific substance is recovered in the stripping liquid.

[0015] In the optimal form of the specific substance extraction and recovery device according to the present invention, the following seven features can be obtained: 1) the position of the two-liquid phase interface in the vessel or chamber is always stable without fluctuation, 2) the volume ratio of both phases involved in the phase mixing can be set independently of the liquid transfer speed, 3) a stable emulsion phase (two-liquid emulsion mixed phase) is developed over a wide range by efficiently mixing both phases, 4) the rotation of the stirring blades (strength of phase mixing) does not affect the liquid transfer speed, 5) the number of theoretical plates is increased by countercurrent contact of both phases based on the opposing liquid transfer of the heavy liquid phase and the light liquid phase, 6) phase separation is improved by simultaneously progressing phase separation in the vessel or chamber (mixer chamber) for mechanical mixing, and 7) circulation liquid transfer can be facilitated by switching from liquid transfer by overflow (overflow) to liquid transfer by pressure action.

[0016] In the mechanism of the conventional device, both the heavy liquid phase (in most cases, the water phase) and the light liquid phase (in most cases, the oil phase) are introduced from the bottom of the mixer chamber. The bottom of the mixer chamber is prone to becoming rich in the heavy liquid phase, and the two liquid phases introduced there form a phase in an emulsion state (emulsion phase) while remaining rich in the heavy liquid phase. That is, in the initial stage of mixing the heavy liquid phase and the light liquid phase, the two liquid phases are mixed in an emulsion state with a large proportion of the heavy liquid phase. Therefore, in order to reduce the influence, the blade part of the mixing impeller is often installed directly above the inlet of both phases at the bottom of the mixer chamber. Also, if a front chamber is provided directly below the inlet of both phases, the proportion of the light liquid phase becomes large in the upper part of the front chamber, and by sucking it up with the suction action of the mixing impeller, the emulsion mixing in the above-mentioned heavy liquid phase-rich state can be offset or alleviated, but since the proportion of both phases sucked up is not constant, there is a disadvantage that the volume ratio of both phases mixed is not stable.

[0017] In contrast, in the present invention, the blade portion of the impeller for phase mixing the heavy liquid phase and the light liquid phase is positioned near the interface between the two liquid phases (at a position near the interface where the rotation of the impeller promotes emulsion mixing of the heavy liquid phase and the light liquid phase), and a liquid-liquid extraction mechanism is utilized in which the heavy liquid phase is introduced from above and the light liquid phase is introduced from below into a container or room (mixer chamber) that houses the impeller, thereby enabling phase mixing without changing the volume ratio of the heavy liquid phase and the light liquid phase present in the emulsion phase (two-liquid emulsion mixture phase) throughout. Effect of the Invention

[0018] The present invention solves the problems inherent in the structure of conventional mixer-settler apparatus (referred to as the conventional apparatus) in liquid-liquid extraction using mechanical stirring, and also realizes innovative features not found in the conventional apparatus.

[0019] Specifically, the best embodiment of the present invention can solve the problems of the mechanism of the conventional device, such as the difficulty of handling due to the interface position being easily changed, the operational limitation that the volume ratio of the two liquid phases involved in the phase mixing (so-called O / A ratio) depends on the ratio of the liquid feed rates of both phases, inefficient two-liquid phase mixing involving the surrounding heavy liquid phase, and the operational complication caused by the interlocking of the stirring blade rotation and the liquid feed rate. That is, according to the device of the present invention, the interface position does not fluctuate and is always stable, the volume ratio of both phases can be set independently of the liquid feed rate (independently), and efficient two-liquid phase mixing can be realized while consistently maintaining the volume ratio of both phases in the emulsion phase, and the stirring blade rotation can be prevented from affecting the liquid feed rate.

[0020] In addition, in the present invention, as an innovative feature not found in conventional devices, the theoretical plate number is improved by countercurrent contact based on the opposing flows of the heavy liquid phase and the light liquid phase. The theoretical plate number referred to here is an index that expresses the performance of separation in liquid-liquid extraction based on the distribution equilibrium value in a batch system, and when the theoretical plate number is improved, the value of the separation coefficient (ratio of the distribution ratio of two substances) that indicates the degree of separation between two substances increases. In addition, by simultaneously carrying out phase separation in a vessel or room (mixer room) for mechanical stirring, the phase separation property is improved. Furthermore, by switching from overflow to pressure liquid delivery, circulating liquid delivery can be made easier. In addition, the mechanism of circulating liquid delivery adaptation can be utilized for the multi-stage effect generated by integrating forward extraction, washing, and back extraction and synchronously circulating liquid delivery, and compared with the mechanism of conventional devices, the device system can be significantly downsized. [Brief description of the drawings]

[0021] [Figure 1(a)] A single-chamber system that circulates heavy and light liquid phases (part 1). [Figure 1(b)] A single-chamber system for circulating heavy and light liquid phases (part 2). [Figure 1(c)] A single-chamber system that circulates heavy and light liquid phases (part 3). [Figure 1(d)] A single-chamber system that circulates heavy and light liquid phases (part 4). [Figure 1(e)] A single-chamber system that circulates heavy and light liquid phases (part 5). [Figure 1(f)] A single-chamber system that circulates only the light liquid phase (part 1). [Figure 1(g)] A single-chamber system that circulates only the light liquid phase (part 2). [Figure 1(h)] A single-chamber system that circulates only the light liquid phase (part 3). [Figure 1(i)] A single-chamber system that circulates only the light liquid phase (part 4). [Figure 1(j)] A single-chamber system that circulates only the light liquid phase (part 5). [Figure 1(k)] A single-chamber system that circulates only the heavy liquid phase (part 1). [Figure 1(l)] A single-chamber system that circulates only the heavy liquid phase (part 2). [Figure 1(m)] A single-chamber system that circulates only the heavy liquid phase (part 3). [Figure 1(n)] A single-chamber system that circulates only the heavy liquid phase (part 4). [Figure 1(o)] A single-chamber system that circulates only the heavy liquid phase (part 5). [Figure 1(p)] A single-chamber system in which the heavy liquid phase and the light liquid phase are passed through in a single pass (part 1). [Figure 1(q)] A single-chamber system in which the heavy liquid phase and the light liquid phase are passed through in a single pass (part 2). [Figure 1(r)] A single-chamber system in which the heavy liquid phase and the light liquid phase are passed through in a single pass (part 3). [Figure 1(s)] A single-chamber system in which the heavy liquid phase and the light liquid phase are passed through in a single pass (part 4). [Figure 1(t)] A single-chamber system in which the heavy liquid phase and the light liquid phase are passed through in a single pass (part 5). [Figure 2(a)] A single-chamber system with upper and lower overhangs that circulates and pumps heavy and light liquid phases (part 1). [Figure 2(b)] A single-chamber mechanism with upper and lower overhangs that circulates and pumps heavy and light liquid phases (part 2). [Figure 2(c)] A single-chamber mechanism with upper and lower overhangs that circulates and pumps heavy and light liquid phases (part 3). [Figure 2(d)] A single-chamber mechanism with upper and lower protruding sections that circulates and pumps heavy and light liquid phases (part 4). [Figure 2(e)] A single-chamber mechanism with upper and lower protruding sections that circulates and pumps heavy and light liquid phases (part 5). [Figure 2(f)] A single-chamber system with upper and lower overhangs that circulates only the light liquid phase (part 1). [Figure 2(g)] A single-chamber system with upper and lower overhangs that circulates only the light liquid phase (part 2). [Figure 2(h)] A single-chamber system with upper and lower overhangs that circulates only the light liquid phase (part 3). [Figure 2(i)]A single-chamber system with upper and lower overhangs that circulates only the light liquid phase (part 4). [Figure 2(j)] A single-chamber system with upper and lower overhangs that circulates only the light liquid phase (part 5). [Figure 2(k)] A single-chamber system with upper and lower overhangs that circulates only the heavy liquid phase (part 1). [Figure 2(l)] A single-chamber system with upper and lower overhangs that circulates only the heavy liquid phase (part 2). [Figure 2(m)] A single-chamber system with upper and lower overhangs that circulates only the heavy liquid phase (part 3). [Figure 2(n)] A single-chamber system with upper and lower overhangs that circulates only the heavy liquid phase (part 4). [Figure 2(o)] A single-chamber system with upper and lower protruding sections that circulates and pumps only the heavy liquid phase (part 5). [Figure 2(p)] A single-chamber system with upper and lower overhangs that transports the heavy liquid phase and the light liquid phase in a single pass (part 1). [Figure 2(q)] A single-chamber mechanism with upper and lower overhangs that transports the heavy liquid phase and the light liquid phase in a single pass (part 2). [Figure 2(r)] A single-chamber mechanism with upper and lower overhangs that transports the heavy liquid phase and the light liquid phase in a single pass (part 3). [Figure 2(s)] A single-chamber mechanism with upper and lower overhangs that transports the heavy liquid phase and the light liquid phase in a single pass (part 4). [Figure 2(t)] A single-chamber mechanism with upper and lower overhangs that transports the heavy liquid phase and the light liquid phase in a single pass (part 5). [Figure 3(a)] A vertically long single-chamber type mechanism that utilizes a shaft holder or bearing (part 1). [Figure 3(b)] A vertically long single-chamber type with top and bottom protrusions that utilizes a shaft holder or bearing (part 1). [Figure 3(c)] A vertically long single-chamber type mechanism that utilizes a shaft holder or bearing (part 2). [Figure 3(d)] A vertically long single-chamber type with top and bottom protrusions that utilizes shaft holders or bearings (part 2). [Figure 3(e)] A vertically long, single-chamber type mechanism that uses two-axis orthogonal gears. [Figure 3(f)]A single-chamber type with vertical overhangs and a mechanism that uses two-axis orthogonal gears. [Figure 4(a)] A multi-chamber system that circulates heavy and light liquid phases (part 1). [Figure 4(b)] A multi-chamber system that circulates heavy and light liquid phases (part 2). [Figure 4(c)] A multi-chamber system that circulates heavy and light liquid phases (part 3). [Figure 4(d)] A multi-chamber system that circulates heavy and light liquid phases (part 4). [Figure 4(e)] A multi-chamber system that circulates only the light liquid phase (part 1). [Figure 4(f)] A multi-chamber system that circulates only the light liquid phase (part 2). [Figure 4(g)] A multi-chamber system that circulates only the light liquid phase (part 3). [Figure 4(h)] A multi-chamber system that circulates only the light liquid phase (part 4). [Figure 4(i)] A multi-chamber system that circulates only the heavy liquid phase (part 1). [Figure 4(j)] A multi-chamber system that circulates only the heavy liquid phase (part 2). [Figure 4(k)] A multi-chamber system that circulates only the heavy liquid phase (part 3). [Figure 4(l)] A multi-chamber system that circulates only the heavy liquid phase (part 4). [Figure 4(m)] A multi-chamber system in which the heavy liquid phase and the light liquid phase are passed through in a single pass (part 1). [Figure 4(n)] A multi-chamber system in which the heavy liquid phase and the light liquid phase are passed through in a single pass (part 2). [Figure 4(o)] A multi-chamber system in which the heavy liquid phase and the light liquid phase are passed through in a single pass (part 3). [Figure 4(p)] A multi-chamber system in which the heavy liquid phase and the light liquid phase are passed through in a single pass (part 4). [Figure 5(a1)] The relationship between the partition structure and the upper and lower communicating parts when installing two liquid phases (part 1). [Figure 5(a2)] The relationship between the partition structure and the upper and lower communicating parts when installing two liquid phases (part 1). [Figure 5(b1)] The relationship between the partition structure and the upper and lower communicating parts when installing two liquid phases (part 2). [Figure 5(b2)] The relationship between the partition structure and the upper and lower communicating parts when installing two liquid phases (part 2). [Figure 5(c1)] The relationship between the partition structure and the upper and lower communication points when installing two liquid phases (part 3). [Figure 5(c2)] The relationship between the partition structure and the upper and lower communication points when installing two liquid phases (part 3). [Figure 5(d1)] The relationship between the partition structure and the upper and lower communication points when installing two liquid phases (part 4). [Figure 5(d2)] The relationship between the partition structure and the upper and lower communication points when installing two liquid phases (part 4). [Figure 5(e1)] Relationship between the partition structure and the upper and lower communication points when installing two liquid phases (part 5). [Figure 5(e2)] Relationship between the partition structure and the upper and lower communication points when installing two liquid phases (part 5). [Figure 5(f1)] The relationship between the partition structure and the upper and lower communicating parts when installing two liquid phases (part 6). [Figure 5(f2)] The relationship between the partition structure and the upper and lower communicating parts when installing two liquid phases (part 6). [Figure 5(g1)] Relationship between the partition structure and the upper and lower communication points when installing two liquid phases (Part 7). [Figure 5(g2)] Relationship between the partition structure and the upper and lower communication points when installing two liquid phases (Part 7). [Figure 5(h1)] Relationship between the partition structure and the upper and lower communication points when installing two liquid phases (Part 8). [Figure 5(h2)] Relationship between the partition structure and the upper and lower communication points when installing two liquid phases (Part 8). [Figure 5(i1)] Relationship between the partition structure and the upper and lower communication points when installing two liquid phases (Part 9). [Figure 5(i2)] Relationship between the partition structure and the upper and lower communication points when installing two liquid phases (Part 9). [Figure 6(a)] A multi-chamber system that circulates heavy and light liquid phases (part 5). [Figure 6(b)] A multi-chamber system that circulates heavy and light liquid phases (part 6). [Figure 6(c)]A multi-chamber system that circulates heavy and light liquid phases (part 7). [Figure 6(d)] A multi-chamber system that circulates heavy and light liquid phases (part 8). [Figure 6(e)] A multi-chamber system that circulates only the light liquid phase (part 5). [Figure 6(f)] A multi-chamber system that circulates only the light liquid phase (part 6). [Figure 6(g)] A multi-chamber system that circulates only the light liquid phase (part 7). [Figure 6(h)] A multi-chamber system that circulates only the light liquid phase (part 8). [Figure 6(i)] A multi-chamber system that circulates only the heavy liquid phase (part 5). [Figure 6(j)] A multi-chamber system that circulates only the heavy liquid phase (part 6). [Figure 6(k)] A multi-chamber system that circulates only the heavy liquid phase (part 7). [Figure 6(l)] A multi-chamber system that circulates only the heavy liquid phase (part 8). [Figure 6(m)] A multi-chamber system in which the heavy liquid phase and the light liquid phase are passed through in a single pass (part 5). [Figure 6(n)] A multi-chamber system in which the heavy liquid phase and the light liquid phase are passed through in a single pass (part 6). [Figure 6(o)] A multi-chamber system (part 7) that passes the heavy liquid phase and the light liquid phase in a single pass. [Figure 6(p)] A multi-chamber system in which the heavy liquid phase and the light liquid phase are passed through in a single pass (part 8). [Figure 7(a1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 1). [Figure 7(a2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 1). [Figure 7(b1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 2). [Figure 7(b2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 2). [Figure 7(c1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 3). [Figure 7(c2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 3). [Figure 7(d1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 4). [Figure 7(d2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 4). [Figure 7(e1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 5). [Figure 7(e2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 5). [Figure 7(f1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 6). [Figure 7(f2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 6). [Figure 7(g1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 7). [Figure 7(g2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 7). [Figure 7(h1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 8). [Figure 7(h2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 8). [Figure 7(i1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 9). [Figure 7(i2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 9). [Figure 8(a)] A multi-chamber system that circulates heavy and light liquid phases (part 9). [Figure 8(b)] A multi-chamber system that circulates heavy and light liquid phases (part 10). [Figure 8(c)] A multi-chamber system that circulates heavy and light liquid phases (part 11). [Figure 8(d)] A multi-chamber system that circulates heavy and light liquid phases (part 12). [Figure 8(e)]A multi-chamber system that circulates only the light liquid phase (part 9). [Figure 8(f)] A multi-chamber system that circulates only the light liquid phase (part 10). [Figure 8(g)] A multi-chamber system that circulates only the light liquid phase (part 11). [Figure 8(h)] A multi-chamber system that circulates only the light liquid phase (part 12). [Figure 8(i)] A multi-chamber system that circulates only the heavy liquid phase (part 9). [Figure 8(j)] A multi-chamber system that circulates only the heavy liquid phase (part 10). [Figure 8(k)] A multi-chamber system that circulates only the heavy liquid phase (part 11). [Figure 8(l)] A multi-chamber system that circulates only the heavy liquid phase (part 12). [Figure 8(m)] A multi-chamber system in which the heavy liquid phase and the light liquid phase are passed through in a single pass (part 9). [Figure 8(n)] A multi-chamber system that passes the heavy and light liquid phases in a single pass (part 10). [Figure 8(o)] A multi-chamber system (part 11) that passes the heavy liquid phase and the light liquid phase in a single pass. [Figure 8(p)] A multi-chamber system (part 12) that passes the heavy liquid phase and the light liquid phase in a single pass. [Figure 9(a1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 10). [Figure 9(a2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 10). [Figure 9(b1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 11). [Figure 9(b2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 11). [Figure 9(c1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 12). [Figure 9(c2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 12). [Figure 9(d1)]The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 13). [Figure 9(d2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 13). [Figure 9(e1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 14). [Figure 9(e2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 14). [Figure 9(f1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 15). [Figure 9(f2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 15). [Figure 9(g1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 16). [Figure 9(g2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 16). [Figure 9(h1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 17). [Figure 9(h2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 17). [Figure 9(i1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 18). [Figure 9(i2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 18). [Figure 10(a)] A multi-chamber system that circulates heavy and light liquid phases (part 13). [Figure 10(b)] A multi-chamber system that circulates heavy and light liquid phases (part 14). [Figure 10(c)] A multi-chamber system that circulates heavy and light liquid phases (part 15). [Figure 10(d)] A multi-chamber system that circulates heavy and light liquid phases (part 16). [Figure 10(e)] A multi-chamber system that circulates only the light liquid phase (part 13). [Figure 10(f)] A multi-chamber system that circulates only the light liquid phase (part 14). [Figure 10(g)] A multi-chamber system that circulates only the light liquid phase (part 15). [Figure 10(h)] A multi-chamber system that circulates only the light liquid phase (part 16). [Figure 10(i)] A multi-chamber system that circulates only the heavy liquid phase (part 13). [Figure 10(j)] A multi-chamber system that circulates only the heavy liquid phase (part 14). [Figure 10(k)] A multi-chamber system that circulates only the heavy liquid phase (part 15). [Figure 10(l)] A multi-chamber system that circulates only the heavy liquid phase (part 16). [Figure 10(m)] A multi-chamber system (part 13) that passes the heavy liquid phase and the light liquid phase in a single pass. [Figure 10(n)] A multi-chamber system (part 14) that passes the heavy liquid phase and the light liquid phase in a single pass. [Figure 10(o)] A multi-chamber system (part 15) that passes the heavy liquid phase and the light liquid phase in a single pass. [Figure 10(p)] A multi-chamber system (part 16) that passes the heavy liquid phase and the light liquid phase in a single pass. [Figure 11(a1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 19). [Figure 11(a2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 19). [Figure 11(b1)] The relationship between the structure of the upper and lower partitions and the upper and lower connecting parts (Part 20) [Figure 11(b2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 20). [Figure 11(c1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 21). [Figure 11(c2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 21). [Figure 11(d1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 22). [Figure 11(d2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 22). [Figure 11(e1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 23). [Figure 11(e2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 23). [Figure 11(f1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 24). [Figure 11(f2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 24). [Figure 11(g1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 25). [Figure 11(g2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 25). [Figure 11(h1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 26). [Figure 11(h2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 26). [Figure 11(i1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 27). [Figure 11(i2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 27). [Figure 12(a)] A multi-chamber system that circulates heavy and light liquid phases (part 17). [Figure 12(b)] A multi-chamber system that circulates heavy and light liquid phases (part 18). [Figure 12(c)] A multi-chamber system that circulates heavy and light liquid phases (part 19). [Figure 12(d)] A multi-chamber system that circulates heavy and light liquid phases (part 20). [Figure 12(e)] A multi-chamber system that circulates only the light liquid phase (part 17). [Figure 12(f)] A multi-chamber system that circulates only the light liquid phase (part 18). [Figure 12(g)] A multi-chamber system that circulates only the light liquid phase (part 19). [Figure 12(h)]A multi-chamber system that circulates only the light liquid phase (part 20). [Figure 12(i)] A multi-chamber system that circulates only the heavy liquid phase (part 17). [Figure 12(j)] A multi-chamber system that circulates only the heavy liquid phase (part 18). [Figure 12(k)] A multi-chamber system that circulates only the heavy liquid phase (part 19). [Figure 12(l)] A multi-chamber system that circulates only the heavy liquid phase (part 20). [Figure 12(m)] A multi-chamber system (part 17) that passes the heavy liquid phase and the light liquid phase in a single pass. [Figure 12(n)] A multi-chamber system (part 18) that passes the heavy liquid phase and the light liquid phase in a single pass. [Figure 12(o)] A multi-chamber system (part 19) that passes the heavy liquid phase and the light liquid phase in a single pass. [Figure 12(p)] A multi-chamber system (part 20) that passes the heavy liquid phase and the light liquid phase in a single pass. [Figure 13(a1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 28). [Figure 13(a2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 28). [Figure 13(b1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 29). [Figure 13(b2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 29). [Figure 13(c1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 30). [Figure 13(c2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 30). [Figure 13(d1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 31). [Figure 13(d2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 31). [Figure 13(e1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 32). [Figure 13(e2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 32). [Figure 13(f1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 33). [Figure 13(f2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 33). [Figure 13(g1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 34). [Figure 13(g2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 34). [Figure 13(h1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 35). [Figure 13(h2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 35). [Figure 13(i1)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 36). [Fig. 13(i2)] The relationship between the structure of the upper and lower partition plates and the upper and lower connecting parts (Part 36). [Figure 14] The area of ​​the emulsion mixture when the mechanism in Figure 1(f) is in operation. [Figure 15] The area of ​​the emulsion mixture when the mechanism in Figure 2(f) is in operation. [Figure 16] The area of ​​emulsion mixture when the mechanism in Figure 4(e) is in operation. [Figure 17] The area of ​​emulsion mixture when the mechanism in Figure 6(e) is in operation. [Figure 18] The area of ​​emulsion mixture when the mechanism in Figure 8(e) is in operation. [Figure 19] The area of ​​emulsion mixture when the mechanism in Figure 10(e) is in operation. [Figure 20] The area of ​​emulsion mixture when the mechanism in Figure 12(e) is in operation. [Figure 21] A mechanism in which horizontal passage holes are installed in the partition plate shown in Figure 4(e) in addition to the area connecting the upper and lower chambers. [Figure 22]The area of ​​milky mixture when the mechanism in Figure 21 is in operation. [Figure 23] The mechanism of a conventional mixer-settler corresponds to Figure 8(m). DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0022] The present invention relates to an apparatus for extracting and recovering a specific substance based on liquid-liquid extraction, which is characterized in that in liquid-liquid extraction based on mechanical agitation in which a heavy liquid phase and a light liquid phase are placed in a container 1 or a room (mixer chamber 30) equipped with an agitator 2, the interface between the two liquid phases can be always maintained at the same position, the volume ratio of both phases in the container or room can be set regardless of the liquid transfer speed, the heavy liquid phase and the light liquid phase can be efficiently phase-mixed to grow a stable emulsion phase (two-liquid-phase emulsion mixed phase) over a wide range, the agitator blade rotation (strength of phase mixing) can be prevented from affecting the liquid transfer speed, the number of theoretical plates is increased by countercurrent contact between the heavy liquid phase and the light liquid phase, phase separation is improved by simultaneously progressing phase separation in the container 1 or room (mixer chamber 30) for phase mixing, and circulating liquid transfer can be facilitated by switching from liquid transfer by overflow (overflow) to liquid transfer by pressure action.

[0023] Conventional liquid-liquid extraction systems using mechanical stirring, such as the mixer-settler method, have problems such as the interface position being easily fluctuated, the volume ratio of the two liquid phases involved in the phase mixing being dependent on the ratio of the liquid feed rates of the two phases, the surrounding heavy liquid phase being entrained when the two liquid phases are mixed, and the rotation speed of the stirring blades 2 affecting the liquid feed rate. The present invention solves these problems of the conventional device systems, and in addition, it manifests innovative features that cannot be obtained with the conventional device systems. By using this system, it becomes possible to produce a specific substance more efficiently and effectively than with conventional devices.

[0024] The problem of the above-mentioned conventional device can be solved by using a mechanism in which the impeller part of the impeller 2 is arranged near the interface 100 between the heavy liquid phase 4 and the light liquid phase 5 and the heavy liquid phase 4 is fed from above the container 1 or the room (mixer chamber 30) that houses the impeller, and the light liquid phase 5 is fed from below. In addition, 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 is improved. In addition, the phase separation is simultaneously carried out in the container 1 or the room (mixer chamber 30) for phase mixing, so that the phase separation property is improved. Furthermore, by switching from overflow to pressure feeding, the circulation feeding can be made easier. In other words, not only can the problems of the conventional device be solved, but also innovative features that cannot be obtained in the conventional device are expressed, so that it becomes possible to extract and recover a specific substance based on liquid-liquid extraction more efficiently and effectively than in the conventional device.

[0025] First, as the most basic and simple mechanism of the present invention, reference is made to Fig. 1(a) to Fig. 1(t), but this is not limited thereto. A heavy liquid phase 4 and a light liquid phase 5 are placed in one vessel 1 equipped with an agitator 2, and the blade portion of the agitator 2 is arranged near the interface 100 between the two phases in the vessel. The agitator is rotated, and the heavy liquid phase 4 is introduced from above the vessel, and the light liquid phase 5 is introduced from below, so that the two phases coexist in an emulsion-mixed state and a phase-separated state, thereby performing liquid-liquid extraction. According to this mechanism, countercurrent contact of two liquid phases is possible, which could not be achieved by conventional liquid-liquid extraction using mechanical agitation, such as the mixer-settler method. In these figures, the heavy liquid phase 4 and the light liquid phase 5 are set to the same volume as an example, but this is not limited thereto. Figures 1(a), 1(b), 1(c), 1(d), 1(e), 1(f), 1(g), 1(h), 1(i), 1(j), 1(k), 1(l), 1(m), 1(n), and 1(o) are examples of mechanisms for circulating and pumping the heavy liquid phase 4 or the light liquid phase 5, or both, and Figures 1(p), 1(q), 1(r), 1(s), and 1(t) are examples of mechanisms for pumping both the heavy liquid phase 4 and the light liquid phase 5 in a single pass.

[0026] In Fig. 1(a), Fig. 1(b), Fig. 1(c), Fig. 1(d), and Fig. 1(e), both the heavy liquid phase 4 and the light liquid phase 5 are circulated. In Fig. 1(f), Fig. 1(g), Fig. 1(h), Fig. 1(i), and Fig. 1(j), the heavy liquid phase 4 is circulated while the light liquid phase 5 is circulated. As a method for discharging the heavy liquid phase 4, Fig. 1(f) and Fig. 1(g) are piping type, and Fig. 1(h), Fig. 1(i), and Fig. 1(j) are vessel passage type. The heavy liquid phase 4 is discharged from the upper position in both the piping type (Fig. 1(f) and Fig. 1(g)) and the vessel passage type (Fig. 1(h), Fig. 1(i), and Fig. 1(j)). In Fig. 1(k), Fig. 1(l), Fig. 1(m), Fig. 1(n), and Fig. 1(o), the heavy liquid phase 4 is circulated while the light liquid phase 5 is pumped in a single pass. As a method for discharging the light liquid phase 5, Fig. 1(k) and Fig. 1(l) show a piping system using a liquid pumping line 7, while Fig. 1(m), Fig. 1(n), and Fig. 1(o) show an in-vessel passage system using a light liquid phase passage 12.

[0027] In addition, the light liquid phase is discharged at an upper position in the piping system (FIGS. 1(k) and 1(l)), and at a lower position in the vessel passage system (FIGS. 1(m), 1(n), and 1(o)). In addition, in FIG. 1(k) and FIG. 1(l), if it is desired to manage the supply and discharge of the light liquid phase 5 at the same height, it is also possible to extend the discharge pipe from the upper to the lower position. In addition, a specific substance separated and refined in the oil phase (in most cases, the light liquid phase 5) can be recovered in a stripping liquid (in most cases, the heavy liquid phase) installed in a stripping vessel (not shown) by providing the stripping vessel in the oil phase feed line (in most cases, the light liquid phase 5 feed line 7). That is, similar to FIG. 1 of Patent Application No. 2019-113657 previously submitted by the same applicant, for example, the light liquid phase 5 extracted from the inlet of the liquid supply line 7 is sent from the bottom of a back-extraction vessel having a structure similar to that of the vessel 1 into the back-extraction liquid (heavy liquid phase 4), and the reset light liquid phase 5 obtained from above is returned to the liquid supply line 7 again, thereby recovering a specific substance in the back-extraction liquid.

[0028] Figures 1(p), 1(q), 1(r), 1(s), and 1(t) are examples of mechanisms for delivering both the heavy and light liquid phases in a single pass. In Figure 1(p), both the heavy and light liquid phases 4 and 5 are delivered in a single pass using a piping system. In Figure 1(q), the heavy liquid phase 4 is delivered using an in-vessel passage system and the light liquid phase 5 is delivered using a piping system, with the delivery being in a single pass. In Figure 1(r), the heavy liquid phase 4 is delivered using a piping system and the light liquid phase 5 is delivered using an in-vessel passage system, with the delivery being in a single pass. In Figures 1(s) and 1(t), both the heavy and light liquid phases 4 and 5 are delivered using an in-vessel passage system, with the delivery being in a single pass. In addition, FIG. 1(s) shows a configuration in which the passages within the vessel for the heavy liquid phase 4 and the light liquid phase 5 are shifted to one side of the vessel 1, while FIG. 1(t) shows a configuration in which the passages within the vessel for both phases are allocated to the left and right.

[0029] The heavy liquid phase 4 is discharged from an upward position in both the piping system (Figures 1(p) and 1(r)) and the vessel passage system (Figures 1(q), 1(s), and 1(t)). The light liquid phase 5 is discharged from an upward position in the piping system (Figures 1(p) and 1(q)), and from a downward position in the vessel passage system (Figures 1(r), 1(s), and 1(t)). In the cases of Figures 1(p) and 1(q), if it is desired to manage the supply and discharge of the light liquid phase 5 at the same height, it is also possible to extend the discharge pipe from the top to the bottom.

[0030] In addition, the position of the blade portion of the stirring blade 2 shown in Figures 1(a) to 1(t) can have a certain degree of width, and the device structure of the present invention is effective, for example, if it is within a range of about 2 to 3 times the thickness (height) of the blade portion above and below the interface 100 of the two liquid phases.

[0031] The mechanism shown in FIG. 1(a) to FIG. 1(t) is characterized in that the heavy liquid phase 4 and the light liquid phase 5 coexist in an emulsion state and in a phase-separated state, and functions by discharging or circulating the separated phases. In other words, phase separation is the key to the present invention, and it is important to ensure that the phase separation is performed. For example, the upper part or lower part or both of the container 1 are provided with a shape (projecting shape) having a larger cross-sectional area than the middle part of the container, thereby promoting phase separation of the heavy liquid phase 4 and the light liquid phase 5. In addition, when the cross-sectional area of ​​the center part of the container is increased for reasons such as the need to enlarge the blade part, the same effect can be obtained by narrowing the space between the projecting shape and the center part.

[0032] 2(a) to 2(t) show examples in which the upper and lower parts of the container 1 are provided with a shape (projecting shape) that has a larger cross-sectional area than the middle part of the container, but this is not limited to the above. Even with a container having such a shape, it is possible to have a flow path structure similar to the structure shown in Fig. 1(a) to 1(t).

[0033] In the mechanisms shown in Figures 1(a) to 1(t) and 2(a) to 2(t), the processing speed of liquid-liquid extraction can be increased by increasing the area where the heavy liquid phase 4 and the light liquid phase 5 are mixed in an emulsion, and the area where the two phases are separated can be increased to allow for phase separation. For example, if the container 1 is made even more elongated (vertically expanded) and the volume is increased (hereinafter referred to as the pronounced elongated shape), the area where the heavy liquid phase 4 and the light liquid phase 5 are in an emulsion state is expanded in the vertical direction, which increases the processing speed, provides more space for phase separation, and promotes phase separation of the two phases. In addition, the elongated shape is also advantageous in that it allows for a smaller floor space for installation.

[0034] Furthermore, since the countercurrent contact of the heavy liquid phase 4 and the light liquid phase 5 is a mechanism that can be expected to produce a high number of theoretical plates, if the elongated shape is made more pronounced, the selective separation ability will be improved in terms of the number of theoretical plates, making it possible to achieve a higher level of separation.

[0035] On the other hand, if the elongated shape of the vessel 1 is made more pronounced, the rotation axis of the agitator blade 2 must necessarily be lengthened. However, if the rotation axis is lengthened, the axis vibration and axis wobble will increase, and normal mechanical agitation may become impossible. Therefore, the axis vibration and axis wobble can be eliminated by installing an axis holder or bearing or a biaxial orthogonal gear. Two or all of the axis holder, bearing, and biaxial orthogonal gear may be used in combination. Examples of installing an axis holder or bearing or a biaxial orthogonal gear are shown in Figures 3(a) to 3(f), but are not limited to these.

[0036] In FIG. 3(a), the elongated shape of the vessel 1 is emphasized compared to the structure in FIG. 1(a), and a shaft holder or bearing is installed above the blade portion of the impeller 2 to eliminate shaft vibration and shaft wobble. The shaft holder here refers to a structure that limits the wobble of the rotating shaft (especially the movement in the left-right direction), and the rotating shaft and the shaft holder are not in contact at a point or on a surface. On the other hand, the bearing refers to a structure in which the rotating shaft and the bearing are in contact at a point or on a surface, that is, a rolling bearing or a sliding bearing. In FIG. 3(b), the elongated shape of the vessel 1 is emphasized compared to the structure in FIG. 2(a), and a shaft holder or bearing is installed above the blade portion of the impeller 2 as in FIG. 3(a). It is possible to install multiple shaft holders or bearings above the blade portion of the impeller 2.

[0037] The shaft holder or bearing can be installed below the blade portion after the rotation shaft of the impeller 2 is extended to below the impeller portion. For example, as shown in Fig. 3(c) or Fig. 3(d), the shaft holder or bearing can be installed near the bottom surface of the vessel 1, but this is not limited thereto. The shaft holder or bearing can be installed both above and below the impeller portion of the impeller 2, and multiple shaft holders or bearings can be installed above or below the impeller portion of the impeller 2, or both.

[0038] Instead of the shaft holder and the bearing, a biaxial orthogonal gear can be used. In FIG. 3(e), a biaxial orthogonal gear is installed above the blade of the agitator 2 in order to eliminate the axial vibration and axial wobble of the rotating shaft of the agitator 2 in the vessel 1 shown in FIG. 1(a) with a more prominent vertical shape. In FIG. 3(f), a biaxial orthogonal gear is installed similarly in the vessel 1 shown in FIG. 2(a) with a more prominent vertical shape. In these cases, the horizontal rotating shaft perpendicular to the vertical rotating shaft is fixed by a bearing installed on the vessel wall, but this is not limited. Even when a biaxial orthogonal gear is used, a plurality of biaxial orthogonal gears may be installed above the blade of the agitator 2, as in the case of using the shaft holder and the bearing. It is also possible to extend the rotating shaft of the agitator 2 to below the blade and install the biaxial orthogonal gear below the blade. In this case, two-axis orthogonal gears may be provided both above and below the blade portion of the agitating blade 2, and a plurality of two-axis orthogonal gears may be provided above or below the blade portion of the agitating blade 2, or both.

[0039] Furthermore, when using a two-axis orthogonal gear, it is not necessary to use the vertical rotation shaft as the power shaft, and if the horizontal rotation shaft is used as the power shaft and the vertical rotation shaft is fixed with a bearing, a motor for rotating the agitator 2 can be installed on the side of the vessel 1. In terms of maintenance and management of the agitator rotation motor, it may be more convenient to install it on the side of the vessel 1, which has a vertically long shape, rather than on the top of it.

[0040] As in the mechanism of the conventional device, the above-mentioned mechanism can be applied to a container structure separated into a mixer chamber 30 for mixing the heavy liquid phase 4 and the light liquid phase 5 and a settler chamber 40 for separating the two phases. Specifically, if communication parts are provided at two places between the ceiling surface and the partition plate of the container 1 storing 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 freely move between the two chambers, it can be treated 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 an emulsion state does not pass through the two communication parts above and below the partition plate between the mixer chamber 30 and the settler chamber 40. By providing the settler chamber 40, it is expected that the separation property and stability during operation can be improved. That is, the risk of the emulsion phase (two-liquid emulsion mixture phase) unexpectedly growing (expanding in range) is reduced, causing the emulsion phase to mix with the heavy and light liquid phases being discharged or circulated.

[0041] 4(a) to 4(p) show the mechanism of the present invention in a vessel structure in which the mixer chamber 30 and the settler chamber 40 are separated by one partition plate (M chamber / S chamber partition plate), but the present invention is not limited to this. Even in such a vessel structure, a flow path mechanism similar to the structure shown in FIG. 1(a) to FIG. 1(t) and the structure shown in FIG. 2(a) to FIG. 2(t) is possible. In addition to FIG. 4(a) to FIG. 4(p), a structure in which the vessel passages for both phases are allocated to the left and right (structures such as 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)) is also possible. However, in the sense that the settler chamber 40 is installed in order to improve the phase separation, it is not preferable to provide a vessel passage (passage for discharge or circulation) for the heavy liquid phase 4 or the light liquid phase 5 on the mixer chamber 30 side.

[0042] The relationship between the structure of the partition plate and the communication parts installed between the ceiling surface and the partition plate of the container 1 storing the mixer chamber 30 and the settler chamber 40 and between the bottom surface and the partition plate is shown in Fig. 5(a1), Fig. 5(b1)...Fig. 5(i1). The state in which the heavy liquid phase and the light liquid phase are installed there is shown in Fig. 5(a2), Fig. 5(b2)...Fig. 5(i2), respectively. Note that all of these figures are views of the mixer chamber 30 side from the settler chamber 40 side. The communication parts of the light liquid phase installed between the ceiling surface and the partition plate are obtained by a structure in which a part or all of the upper end of the partition plate is not in contact with the ceiling surface, or a structure in which a passage port is provided at the upper end of the partition plate. Similarly, the communication parts of the heavy liquid phase installed between the bottom surface and the partition plate are obtained by a structure in which a part or all of the lower end of the partition plate is not in contact with the bottom surface, or a structure in which a passage port is provided at the lower end of the partition plate.

[0043] The shapes of these communication parts are not limited to the shapes shown in Figures 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, etc. 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 a square, a triangle, etc.

[0044] In addition, the structure in which the upper or lower end of the partition plate is not in contact with the ceiling or bottom surface in part or in whole, and the structure in which the upper or lower end of the partition plate has a passage opening, can be used in combination. Figures 5(f1) to 5(i2) show examples of the combination of the two.

[0045] 4(a) to 4(p) are excellent mechanisms for forming a wide area of ​​a milky mixed state (emulsion phase) in the mixer chamber 30, but on the other hand, it is not necessarily easy to always keep the height (width) of the emulsion phase in the mixer chamber 30 constant without causing the emulsion phase to flow out into the settler chamber 40. In other words, the height of the emulsion phase in the mixer chamber may be prone to fluctuations, and in such cases, a structure that has a tolerance for such fluctuations or a structure that can control the fluctuations is preferable.

[0046] First, as a structure that allows for a margin of variation in the height of the emulsion phase, there is a method of making the mixer chamber 30 vertically long. In addition to improving phase separation by suppressing the outflow of the emulsion phase into the settler chamber 40, the emulsion phase grows taller, which has the advantage of promoting two-phase contact. On the other hand, as described above, if the mixer chamber 30 is vertically long, the rotation shaft of the stirring blade 2 becomes longer, which increases shaft vibration and shaft wobble, and normal mechanical stirring may become impossible. Therefore, for example, it is effective to eliminate shaft vibration and shaft wobble by installing a shaft holder or bearing (bearing) or a two-axis orthogonal gear as shown in Figures 3(a) to 3(f). It is also possible to use a combination of two or all of the shaft holder, bearing, and two-axis orthogonal gear.

[0047] On the other hand, the two upper and lower communication parts between the mixer chamber 30 and the settler chamber 40 are intended to allow the light liquid phase to pass between the two chambers at the upper communication part and the heavy liquid phase to pass between the two chambers at the lower communication part, and neither of them is originally intended to allow the emulsion phase to flow out to the settler chamber 40. However, a structure in which the emulsion phase does not move at all from the mixer chamber 30 is not necessarily preferable in that there is no escape route for the overgrown emulsion phase other than the above-mentioned upper and lower communication parts. Conversely, a structure in which part of the emulsion phase moves to the settler chamber 40 significantly suppresses fluctuations in the height (width) of the emulsion phase in the mixer chamber 30.

[0048] Therefore, as a structure capable of controlling the fluctuation in the height (width) of the emulsion phase, if a passage opening is provided in the partition plate at a height near the blade portion of the stirring blade 2 in addition to the upper and lower communicating portions, the emulsion phase flows out from the passage opening into the settler chamber 40, thereby suppressing the fluctuation in the height of the emulsion phase in the mixer chamber 30. However, with such a structure, the emulsion phase generated in the mixer chamber 30 immediately moves to the settler chamber 40, so that the development of the emulsion phase in the mixer chamber 30 is suppressed, and further, a large amount of the emulsion phase collects in the settler chamber 40, making phase separation in the settler chamber 40 difficult.

[0049] On the other hand, if the emulsion phase generated in the mixer chamber 30 is moved through a passage formed in the vertical direction, and then guided to a vertical passage port and then to the settler chamber 40, phase separation will proceed during the process, and the emulsion in the settler chamber 40 will be largely eliminated. Some examples of such container structures are shown below.

[0050] Instead of the partition plates shown in Figures 4(a) to 4(p), upper partition plates forming a communication portion for the light liquid phases of the mixer chamber 30 and the settler chamber 40 can be installed alternately in the upper part of the vessel 1 housing the mixer chamber 30 and the settler chamber 40, and lower partition plates forming a communication portion for the heavy liquid phases of the both chambers can be installed in the lower part of the vessel, thereby forming a passage through which the two emulsion-mixed liquid phases can move vertically and a vertical passage port.

[0051] An example in which the upper partition plate 20 is disposed closer to the mixer chamber 30 and the lower partition plate 21 is disposed closer to the settler chamber is shown in Figures 6(a) to 6(p), but is not limited to this. In addition, under the condition that the upper partition plate 20 and the lower partition plate 21 are disposed alternately, the upper partition plate and the lower partition plate may each be a plurality of plates. In this way, regardless of the difference in the number of partition plates to be disposed, a flow path structure similar to the structure shown in Figures 4(a) to 4(p) is possible.

[0052] The structure of the upper partition plate 20 (partition plate closer to the mixer chamber) and the shape of the communication part of the light liquid phase 5 formed thereby are shown in Fig. 7(a1), Fig. 7(b1)...Fig. 7(i1). The structure of the lower partition plate 21 (partition plate closer to the settler chamber) and the shape of the communication part of the heavy liquid phase 4 formed thereby are shown in Fig. 7(a2), Fig. 7(b2)...Fig. 7(i2). Here, Fig. 7(a1) and Fig. 7(a2), Fig. 7(b1) and Fig. 7(b2)...Fig. 7(i1) and Fig. 7(i2) show a pair of upper partition plate 20 and lower partition plate 21. The communication part of the light liquid phase 5 provided between the ceiling surface and the upper partition plate 20 is obtained by 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, or a structure in which a passage port is provided at the upper end of the upper partition plate 20. Similarly, the communication portion of the heavy liquid phase 4 provided between the bottom surface and the lower partition plate 21 is obtained by 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 by a structure in which a passage port is provided at the lower end portion of the lower partition plate 21.

[0053] The shapes of these communication parts are not limited to the shapes shown in Figures 7(a1) to 7(i2). That is, for a structure in which a part of the upper end of the upper partition plate 20 is not in contact with the ceiling surface, or a part of the lower end of the lower partition plate 21 is not in contact with the bottom surface, the shape is not limited to a rectangle, but may be a semicircle, 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 rectangle, a triangle, or the like.

[0054] In addition, a structure in which a part or all of the upper end of the upper partition plate 20 does not contact the ceiling surface and a structure in which a passage opening is provided at the lower end of the lower partition plate 21, and 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 part or all of the lower end of the lower partition plate 21 does not contact the bottom surface can be used in combination. Figures 7(f1) to 7(i2) show examples of configurations in which both are combined.

[0055] An example in which the lower partition plate 21 is disposed closer to the mixer chamber 30 and the upper partition plate 20 is disposed closer to the settler chamber 40 is shown in Figures 8(a) to 8(p), but is not limited to this. In addition, under the condition that the lower partition plate 21 and the upper partition plate 20 are disposed alternately, the lower partition plate and the upper partition plate may each be a plurality of plates. In this case, regardless of the difference in the number of partition plates to be disposed, a flow path structure similar to the structure shown in Figures 4(a) to 4(p) is possible.

[0056] The structure of the lower partition plate 21 (partition plate closer to the mixer chamber) and the shape of the communication part of the heavy liquid phase 4 formed thereby are shown in Fig. 9(a1), Fig. 9(b1)...Fig. 9(i1). The structure of the upper partition plate 20 (partition plate closer to the settler chamber) and the shape of the communication part of the light liquid phase 5 formed thereby are shown in Fig. 9(a2), Fig. 9(b2)...Fig. 9(i2). Here, Fig. 9(a1) and Fig. 9(a2), Fig. 9(b1) and Fig. 9(b2)...Fig. 9(i1) and Fig. 9(i2) show a pair of the lower partition plate 21 and the upper partition plate 20. The communication part of the heavy liquid phase provided between the bottom surface and the lower partition plate 21 is obtained by a structure in which a part or the whole of the lower end of the lower partition plate 21 is not in contact with the bottom surface, or a structure in which a passage port is provided at the lower end of the lower partition plate 21. Similarly, the light liquid phase communication portion provided between the ceiling surface and the upper partition plate 20 is obtained by 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 by a structure in which a passage port is provided at the upper end of the upper partition plate 20.

[0057] The shapes of these communication parts are not limited to the shapes shown in Figures 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 contact the ceiling surface, or a part of the lower end of the lower partition plate 21 does not contact the bottom surface, the shape is not limited to a rectangle, but may be a semicircle, 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 rectangle, a triangle, or the like.

[0058] In addition, a structure in which a part or all of the lower end of the lower partition plate 21 does not contact the bottom surface and 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 at the lower end of the lower partition plate 21 and a structure in which a part or all of the upper end of the upper partition plate 20 does not contact the ceiling surface can be used in combination. Figures 9(f1) to 9(i2) show examples of configurations in which both are combined.

[0059] 10(a) to 10(p) show an example in which a vertical passage and a vertical passage opening are formed by combining a short lower partition plate 21 and an upper partition plate 20 bent at two places, but this is not limited to this. Note that, provided that the lower partition plate 21 and the upper partition plate 20 are installed alternately, the lower partition plate and the upper partition plate may each be multiple pieces. In this case, too, regardless of the number and shape of the installed partition plates, a flow path structure similar to the structure shown in FIG. 4(a) to FIG. 4(p) is possible.

[0060] The structure of the lower partition plate 21 (a short partition plate) and the shape of the communication area for the heavy liquid phase formed thereby are shown in Figure 11(a1), Figure 11(b1)...Figure 11(i1). The structure of the upper partition plate 20 (a partition plate bent at two places) and the shape of the communication area for the light liquid phase formed thereby are shown in Figure 11(a2), Figure 11(b2)...Figure 11(i2). Figures 11(a1) and 11(a2), Figures 11(b1) and 11(b2)...Figure 11(i1) and 11(i2) show a pair of lower partition plate 21 and upper partition plate 20. Shown on the right side. The communication portion for the light liquid phase 5 provided between the ceiling surface and the upper partition plate is obtained by 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, or a structure in which a passage port is provided at the upper end of the upper partition plate 20. Similarly, the communication portion for the heavy liquid phase 4 provided between the bottom surface and the lower partition plate is obtained by 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, or a structure in which a passage port is provided at the lower end of the lower partition plate 21.

[0061] The shapes of these communication parts are not limited to the shapes shown in Figures 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 contact the ceiling surface, or a part of the lower end of the lower partition plate 21 does not contact the bottom surface, the shape is not limited to a rectangle, but may be a semicircle, a triangle, or other shape. 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 rectangle, a triangle, or other shape.

[0062] In addition, a structure in which a part or all of the lower end of the lower partition plate 21 does not contact the bottom surface and 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 at the lower end of the lower partition plate 21 and a structure in which a part or all of the upper end of the upper partition plate 20 does not contact the ceiling surface can be used in combination. Figures 11(f1) to 11(i2) show examples of configurations in which both are combined.

[0063] 12(a) to 12(p) show an example in which a vertical passage and a vertical passage port are formed by combining a short upper partition plate 20 and a lower partition plate 21 bent at two places, but this is not limited to this. Note that, provided that the upper partition plate 20 and the lower partition plate 21 are installed alternately, the upper partition plate and the lower partition plate may each be multiple pieces. In this case, too, regardless of the number and shape of the installed partition plates, a flow path structure similar to the structure shown in FIG. 4(a) to FIG. 4(p) is possible.

[0064] The structure of the upper partition plate 20 (a short partition plate) and the shape of the communication area for the heavy liquid phase formed thereby are shown in Figure 13(a1), 13(b1)...13(i1). The structure of the lower partition plate 21 (a partition plate bent at two places) and the shape of the communication area for the light liquid phase formed thereby are shown in Figure 13(a2), 13(b2)...13(i2). Figures 13(a1) and 13(a2), 13(b1) and 13(b2)...13(i1) and 13(i2) show a pair of upper partition plate 20 and lower partition plate 21. Shown on the right side. The communication portion for the light liquid phase provided between the ceiling surface and the upper partition plate 20 is obtained by 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, or a structure in which a passage port is provided at the upper end of the upper partition plate 20. Similarly, the communication portion for the heavy liquid phase provided between the bottom surface and the lower partition plate 21 is obtained by 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, or a structure in which a passage port is provided at the lower end of the lower partition plate 21.

[0065] The shapes of these communication parts are not limited to the shapes shown in Figures 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 contact the ceiling surface, or a structure in which a part of the lower end of the lower partition plate 21 does not contact the bottom surface, the shape is not limited to a rectangle, but may be a semicircle, a triangle, or other shape. 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 rectangle, a triangle, or other shape.

[0066] In addition, a structure in which a part or all of the upper end of the upper partition plate 20 does not contact the ceiling surface and a structure in which a passage opening is provided at the lower end of the lower partition plate 21, and 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 part or all of the lower end of the lower partition plate 21 does not contact the bottom surface can be used in combination. Figures 13(f1) to 13(i2) show examples of configurations in which both are combined.

[0067] 6(a) to 6(p), 8(a) to 8(p), 10(a) to 10(p), and 12(a) to 12(p) are examples in which two partition plates (upper partition plate 20 and lower partition plate 21) are installed between the mixer chamber 30 and the settler chamber 40, but the number of partition plates can be increased. That is, by arranging the upper partition plates 20 and the lower partition plates 21 alternately, such as three, four, five, or even more, it is possible to enhance the phase separation effect, but the container structure becomes more complicated.

[0068] The details of the container structure, flow path structure, etc. of the mechanism of the present invention have been described above. For convenience, a system using one container for stirring and mixing the heavy liquid phase 4 and the light liquid phase 5, as in the mechanisms shown in Figures 1(a) to 1(t) and 2(a) to 2(t), will be referred to as a single-chamber system. For convenience, a system using a container structure in which a chamber (mixer chamber 30) for stirring and mixing the heavy liquid phase 4 and the light liquid phase 5 and a chamber (settler chamber 40) for phase separation of the two phases are separated by a partition, as in the mechanisms shown in Figures 4(a) to 4(p), 6(a) to 6(p), 8(a) to 8(p), 10(a) to 10(p), and 12(a) to 12(p), will be referred to as a multi-chamber system.

[0069] The single-chamber system has a simple mechanism and functions stably under conditions where the liquid transfer speed of the two liquid phases and the rotation speed of the agitator blade 2 are kept constant. On the other hand, the height (width) of the emulsion phase may change suddenly due to unpredictable phenomena, such as a large change in the composition of the aqueous phase to be treated (in most cases, the heavy liquid phase) or the inclusion of solid components. To prepare for such cases, it is possible to provide some margin for fluctuations in the height (width) of the emulsion phase by making the vessel vertically long or providing a shape with a large cross-sectional area (projecting shape) on the top and bottom of the vessel 1. However, if the emulsion phase develops further beyond this upper limit, normal operation will immediately become impossible.

[0070] On the other hand, in the multi-chamber system, the development of the emulsion phase beyond the expected limit can be suppressed by providing a settler chamber 40. That is, the multi-chamber system is a system that maintains 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 system shown in Figures 4(a) to 4(p), the emulsion phase that has developed excessively in the mixer chamber 30 flows out toward the settler chamber 40 from the upper and lower communicating parts of the container through which the phase-separated heavy liquid phase 4 and light liquid phase 5 should pass, but if it is for a short period of time, it can be operated without causing significant turbidity in both phases. In addition, in the structure having a vertical passage port as shown in Figures 6(a) to 6(p), Figures 8(a) to 8(p), Figures 10(a) to 10(p), and Figures 12(a) to 12(p), phase separation progresses while the emulsion phase moves through the vertical passage port, so that the turbidity has already been largely eliminated by the time it reaches the settler chamber 40.

[0071] In either the single-chamber or multi-chamber system, the emulsion phase may not be easily formed by mechanical stirring based on the rotation of the stirring blade 2. In such a 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 a fine hole or a fine tube.

[0072] The following examples show the region of an emulsion mixture state that is generated by the mechanism shown in the present invention, and specific examples of an extraction and recovery device for a specific substance that is separated and purified by liquid-liquid extraction utilizing the generation of such an emulsion mixture state, but the present invention is not limited to the following examples. EXAMPLES

[0073] An area of ​​milky mixture.

[0074] As an example of the single-chamber mechanism shown in FIG. 1(a) to FIG. 1(t) of the present invention, FIG. 14 shows the region of the emulsion state (emulsion) generated by operating the mechanism of FIG. 1(f). As a result of an experiment using ion-exchanged water (pure water) or 0.1 M (mol dm-3) nitric acid aqueous solution as the heavy liquid phase and a solvent mainly composed of alkane (product name ShellSol D70) as the light liquid phase, a region in which two liquid phases were phase-separated (a region of light liquid phase above and a region of heavy liquid phase below) was generated above and below the region of the emulsion state, and the range (height) of the region of the emulsion state and the region of the phase separation was stably maintained. Note that the range (height) of the region of the emulsion state is affected by the rotation speed of the stirring blade 2 and the liquid delivery speed of the two liquid phases, but it was stably maintained as long as these speeds did not change. On the other hand, if the area of ​​the emulsion mixture becomes too large and the area of ​​the phase separation can no longer be adequately maintained (if the impeller rotation speed and liquid delivery speed are set to such an extent), the entire inside of container 1 becomes cloudy, and it becomes virtually impossible to perform liquid-liquid extraction.

[0075] In addition, a similar region of the emulsion mixture state was obtained for the mechanisms other than that shown in Fig. 1(f) (the mechanisms shown in Fig. 1(a) to Fig. 1(e) and Fig. 1(g) to Fig. 1(t). In other words, it was confirmed that the difference in the flow channel structure for delivering the light liquid phase 5 and the heavy liquid phase 4 does not affect the region of the emulsion mixture state.

[0076] In comparison with the mechanism of a conventional mixer-settler device, the emulsion mixed state region in the mechanism (single chamber mechanism) shown in Fig. 1(a) to Fig. 1(t) of the present invention corresponds to the mixer chamber, and the phase separated state region corresponds to the settler chamber. Therefore, by increasing the emulsion mixed state region, the processing speed of liquid-liquid extraction was increased. For example, by making the shape of the vessel 1 elongated while maintaining the bottom area, the processing speed could be increased without changing the installation floor area. In addition, the elongated shape is also effective in providing a margin for the phase separated state region, and it was found that not only could the emulsion mixed state region be increased, but also the phase separated state region could be sufficiently secured.

[0077] Furthermore, in order to suppress the emulsion mixture region and secure the phase separation region, a shape (projecting shape) having a larger cross-sectional area than the middle part of the container was provided on the upper or lower part or both of the container 1, and it was found that phase separation of the heavy liquid phase 4 and the light liquid phase 5 was promoted. Figure 15 shows an emulsion mixture region generated by operating a mechanism in which a shape with a large cross-sectional area is provided on the upper and lower parts of the container 1 as shown in Figure 2 (f). In this way, when the emulsion mixture region reaches the part with the large cross-sectional area, phase separation is promoted, so that the emulsion mixture region does not become too large and its growth can be suppressed. Note that a similar emulsion mixture region was obtained for the mechanisms other than Figure 2 (f) (the mechanisms shown in Figures 2 (a) to 2 (e) and Figures 2 (g) to 2 (t)). That is, it was confirmed that the difference in the flow path structure for sending the light liquid phase and the heavy liquid phase does not affect the emulsion mixture region, as in the mechanisms shown in Figures 1 (a) to 1 (f).

[0078] On the other hand, as the vertically elongated shape becomes more pronounced, the rotation axis of the agitator blade 2 becomes longer, resulting in increased axial vibration and axial wobble. However, by using an axis holder, bearing, or two-axis orthogonal gear, or a combination of these, as shown in Figures 3(a) to 3(f), the axial vibration and axial wobble were significantly suppressed.

[0079] Similar to the mechanism of the conventional device, the region of the emulsion mixture was confirmed for a container structure (multiple chamber mechanism) separated into a mixer chamber 30 for mixing and stirring the heavy liquid phase 4 and the light liquid phase 5, and a settler chamber 40 for phase separation of the two liquid phases. Figure 16 shows the region of the emulsion state that occurs when the mechanism of Figure 4(e) is operated. Note that in order to clarify the range of the mixer chamber 30 and the settler chamber 40 as referred to in the present invention, the range of the mixer chamber is clearly indicated by being surrounded by a dashed line.

[0080] The area of ​​the emulsion mixture shown in FIG. 16 spreads over the entire mixer chamber when the rotation speed or the liquid delivery speed of the stirring blade 2 or both become too high, similar to the area of ​​the emulsion mixture shown in FIG. 14. On the other hand, in the vessel structure of FIG. 4(e) having a settler chamber, the emulsion mixture (emulsion) moves from the mixer chamber 30 to the settler chamber 40 through the communication parts installed above and below the partition plate, and can be separated by gravity in the settler chamber 40. In that case, although the drainage becomes slightly turbid, it is possible to continue liquid-liquid extraction. In this respect, it can be said that the double-chamber type has an advantage over the single-chamber type. Even if the emulsion mixture (emulsion) flows into the settler chamber 40, the position of the interface between the two liquid phases hardly changes before and after operation, and the volume ratio (so-called O / A ratio) of the heavy liquid phase 4 and the light liquid phase 5 involved in the phase mixture is maintained.

[0081] Similar regions of the emulsion mixture state were obtained not only for the mechanism shown in Fig. 4(e) but also for the mechanisms shown in Fig. 4(a) to Fig. 4(d) and Fig. 4(f) to Fig. 4(p). That is, it was confirmed that, as with the mechanisms shown in Fig. 1(a) to Fig. 1(t) and Fig. 2(a) to Fig. 2(t), the difference in the flow channel structure for delivering the light liquid phase 5 and the heavy liquid phase 4 does not affect the region of the emulsion mixture state.

[0082] 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 all cases, the upper and lower communication parts functioned sufficiently, and no significant difference was observed. As shown on the right side of each figure, the multi-chamber mechanism needs to 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 liquid level of the light liquid phase 5 does not reach the communication part, the light liquid phase 5 cannot move to the settler chamber 40, and only the heavy liquid phase 4 moves to the settler chamber 40, so that the position of the interface between the two liquid phases in both chambers cannot be maintained. Note that, when the liquid level of the light liquid phase 5 is set to be located below the communication part and an emulsion mixed state (emulsion) is developed until it reaches the bottom of the mixer chamber 30, the ratio of the liquid delivery speeds of the two liquid phases corresponds to the volume ratio of both phases, as in the mechanism of the conventional device.

[0083] In the mechanism shown in Fig. 4(a) to Fig. 4(p), the range (height) of the emulsion mixed state depends on the rotation speed of the impeller 2 and the liquid transfer speed of both phases, as in the single-chamber system. In contrast, it was found that the range (height) of the emulsion mixed state can be maintained almost constant regardless of the change in the rotation speed of the impeller 2 and the liquid transfer speed of both phases by using a mechanism having a vertical passage for the movement of the emulsion mixed state (emulsion) formed by two partition plates (upper partition plate and lower partition plate) as shown in Fig. 6(a) to Fig. 6(p), Fig. 8(a) to Fig. 8(p), Fig. 10(a) to Fig. 10(p), and Fig. 12(a) to Fig. 12(p). That is, the fluctuation of the range (height) of the emulsion mixed state (emulsion) in the mixer chamber 30 was suppressed. However, since the mechanism having the vertical passage port is basically structured to move the emulsion mixture (emulsion) to the settler chamber 40, it was found that the phase separation ability is somewhat lower than that of the mechanisms shown in Figures 4(a) to 4(p). In this respect, no significant difference was observed among the mechanisms shown in Figures 6(a) to 6(p), 8(a) to 8(p), 10(a) to 10(p), and 12(a) to 12(p).

[0084] Regarding the mechanism shown in Fig. 6(a) to Fig. 6(p), the range (height) of the emulsion mixed state region is shown in Fig. 17, taking the flow path structure in Fig. 6(e) as a representative. In order to clarify the range of the mixer chamber 30 and the settler chamber 40 as referred to in the present invention, the range of the mixer chamber 30 is clearly shown surrounded by a dashed line. In this way, the range of the emulsion mixed state region is defined as the range of the mixer chamber 30 up to the outlet of the vertical passage port described above. Also, it is similar to Fig. 16 in that the communication part of the light liquid phase 5 is present near the ceiling surface of the vessel 1, and the communication part of the heavy liquid phase 4 is present near the bottom surface of the vessel 1.

[0085] In addition, a similar region of the emulsion mixture state was obtained for the mechanisms other than Fig. 6(e) (the mechanisms shown in Figs. 6(a) to 6(d) and Figs. 6(f) to 6(p)). That is, it was confirmed that the difference in the flow channel structure for delivering the light liquid phase 5 and the heavy liquid phase 4 does not affect the region of the emulsion mixture state, as in the mechanisms shown in Figs. 1(a) to 1(t), 2(a) to 2(t), and 4(a) to 4(p).

[0086] In addition, for the communication portion of the light liquid phase 5 formed by the upper partition plate located closer to the mixer chamber 30 and the communication portion of the heavy liquid phase 4 formed by the lower partition plate 21 located closer to the settler chamber 40, the structures shown in Figures 7(a1) to 7(i2) were used, and in both cases, the upper and lower communication portions functioned sufficiently, with no significant difference being observed.

[0087] Figure 18 shows the range (height) of the emulsion mixed state region for the mechanism shown in Figures 8(a) to 8(p) using the flow path structure in Figure 8(e) as a representative. As in Figures 16 and 17, the range of the mixer chamber 30 is clearly shown surrounded by a dashed line. As in Figures 16 and 17, Figure 18 is also similar to Figures 16 and 17 in that a communication portion for the light liquid phase is present near the ceiling surface of the vessel 1, and a communication portion for the heavy liquid phase 4 is present near the bottom surface of the vessel 1.

[0088] In addition, a similar region of the emulsion mixture state was obtained for the mechanisms other than Fig. 8(e) (the mechanisms shown in Figs. 8(a) to 8(d) and Figs. 8(f) to 8(p)). That is, it was confirmed that the difference in the flow channel structure for delivering the light liquid phase 5 and the heavy liquid phase 4 does not affect the region of the emulsion mixture state, as in the mechanisms shown in Figs. 1(a) to 1(t), 2(a) to 2(t), 4(a) to 4(p), and 6(a) to 6(p).

[0089] In addition, for the communication portion of the heavy liquid phase 4 formed by the lower partition plate 21 located closer to the mixer chamber 30 and the communication portion of the light liquid phase 5 formed by the upper partition plate 20 located closer to the settler chamber 40, the structures shown in Figures 9(a) to 9(i) were used, and in both cases, the upper and lower communication portions functioned sufficiently, with no significant difference being observed.

[0090] 10(a) to 10(p), the range (height) of the emulsion mixed state region is shown in FIG. 19, taking the flow path structure in FIG. 10(e) as a representative example. As in FIG. 16, FIG. 17, and FIG. 18, the range of the mixer chamber 30 is clearly shown surrounded by a dashed line. As in FIG. 19, the light liquid phase 5 has a communication portion near the ceiling surface of the vessel 1, and the heavy liquid phase 4 has a communication portion near the bottom surface of the vessel 1, similar to FIG. 16, FIG. 17, and FIG. 18.

[0091] In addition, a similar region of the emulsion mixture state was obtained for the mechanisms other than Fig. 10(e) (the mechanisms shown in Figs. 10(a) to 10(d) and Figs. 10(f) to 10(p)). That is, it was confirmed that the difference in the flow channel structure for delivering the light liquid phase 5 and the heavy liquid phase 4 does not affect the region of the emulsion mixture state, as in the mechanisms shown in Figs. 1(a) to 1(t), the mechanisms shown in Figs. 2(a) to 2(t), the mechanisms shown in Figs. 4(a) to 4(p), the mechanisms shown in Figs. 6(a) to 6(p), and the mechanisms shown in Figs. 8(a) to 8(p).

[0092] Furthermore, the communication portion between the light liquid phase 5 and the heavy liquid phase 4 formed by 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), as in the structures shown in Figures 11(a1) to 11(i2), functioned sufficiently as an upper and lower communication portion in all cases, and no significant differences were observed.

[0093] 12(a) to 12(p), the range (height) of the emulsion mixed state region is shown in FIG. 20, taking the flow path structure in FIG. 12(e) as a representative example. As in FIG. 16, FIG. 17, FIG. 18, and FIG. 19, the range of the mixer chamber 30 is clearly shown surrounded by a dashed line. As in FIG. 20, the light liquid phase 5 has a communication portion near the ceiling surface of the vessel 1, and the heavy liquid phase 4 has a communication portion near the bottom surface of the vessel 1, similar to FIG. 16, FIG. 17, FIG. 18, and FIG. 19.

[0094] In addition, a similar region of the emulsion mixture state was obtained for the mechanisms other than that shown in Fig. 12(e) (the mechanisms shown in Figs. 12(a) to 12(d) and Figs. 12(f) to 12(p)). That is, it was confirmed that the difference in the flow channel structure for delivering the light liquid phase 5 and the heavy liquid phase 4 does not affect the region of the emulsion mixture state, as in the mechanisms shown in Figs. 1(a) to 1(t), 2(a) to 2(t), 4(a) to 4(p), 6(a) to 6(p), 8(a) to 8(p), and 10(a) to 10(p).

[0095] In addition, the communication area between the light liquid phase 5 and the heavy liquid phase 4 formed by the structure and arrangement of the lower partition plate (left side of each figure) and the structure and arrangement of the upper partition plate (right side of each figure), such as the structure shown in Figure 13 (a1) to Figure 13 (i2), functioned sufficiently as a vertical communication area in all cases, and no significant difference was observed. Comparative Example 1

[0096] A system in which one of the communication areas for the heavy liquid phase or the light liquid phase in a multi-chamber system is missing.

[0097] The present invention is characterized in that in the container 1 or chamber (mixer chamber 30) where two liquid phases are mixed, an area of ​​an emulsion mixture state and an area of ​​a phase-separated state coexist, and in a multi-chamber system having the mixer chamber 30 and the settler chamber 40, both the phase-separated heavy liquid phase 4 and the light liquid phase 5 communicate with each other. For comparison, a case where only either the heavy liquid phase 4 or the light liquid phase 5 communicates with each other was examined.

[0098] First, in the case where only the phase-separated heavy liquid phase 4 has a communication part, the mechanism shown in Fig. 4(e) was used to study the operation in a state where the liquid level of the light liquid phase 5 does not reach the communication part between the ceiling surface of the vessel and the partition plate. 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 that the position of the interface between the two liquid phases in both chambers cannot be maintained.

[0099] Next, in the case where only the phase-separated light liquid phase 5 has a communication part, the mechanism shown in FIG. 4(e) was modified and examined. That is, the mechanism shown in FIG. 4(e) having a communication part between the bottom surface of the vessel 1 and the partition plate was modified to a mechanism in which the entire lower end of the partition plate is joined to the vessel bottom surface. Using this modified mechanism, the system was operated in a state in which the liquid level of the light liquid phase 5 reached the communication part between the vessel ceiling surface and the partition plate. As a result, only the light liquid phase 5 moved to the settler chamber while the heavy liquid phase 4 was unable to move to the settler chamber, and the position of the interface between the two liquid phases in both chambers could not be maintained. Comparative Example 2

[0100] In a double-chamber system, a horizontal passage hole is provided in addition to the connecting area between the upper and lower chambers.

[0101] In the double-chamber system shown in Figures 4(a) to 4(p), the range (height) of the emulsion mixture (emulsion) is affected by the rotation speed of the impeller 2 and the liquid delivery speed of both phases, as in the single-chamber system, but in order to suppress these effects, it is effective to provide a passageway between the mixer chamber 30 and the settler chamber 40 for the emulsion mixture to move. Therefore, a perforated partition plate 24 having a passageway (horizontal passageway) other than the upper and lower chamber communication area was installed on the partition plate shown in Figure 4(e). The structure is shown in Figure 21.

[0102] In the mechanism shown in Fig. 21, it was possible to suppress the influence of the rotation speed of the impeller 2 and the liquid delivery speed of both phases on the range (height) of the area of ​​the emulsion mixture state (emulsion). However, on the other hand, it was found that the emulsion mixture phase (emulsion phase) generated near the impeller part of the impeller 2 in the mixer chamber 30 immediately moves to the settler chamber 40 through the horizontal passage port, so that the emulsion phase cannot develop sufficiently in the mixer chamber 30, and further, a large amount of emulsion flows into the settler chamber 40, adversely affecting phase separation. Fig. 22 shows the appearance of the emulsion mixture state (emulsion) when the mechanism in Fig. 21 is operated. EXAMPLES

[0103] Confirmation of the invariance of the interface position between two liquid phases in a dual-chamber system.

[0104] In the multi-chamber system shown in the present invention, the position of the interface between the two liquid phases was always at the same position in the mixer chamber 30 and the settler chamber 40. Moreover, regardless of fluctuations in the liquid delivery speeds of both phases and no matter how long the system was operated, the position remained unchanged. Specifically, the invariance of the interface position between the two liquid phases was confirmed for the systems shown in Figures 4(a) to 4(p), 6(a) to 6(p), 8(a) to 8(p), 10(a) to 10(p), and 12(a) to 12(p).

[0105] On the other hand, the mechanism of the conventional device is also a double-chamber type consisting of a mixer chamber and a settler chamber, but the interface position between the two liquid phases does not necessarily coincide in both chambers. In addition, the interface position changes due to fluctuations in the liquid delivery speed of both phases, and the interface position gradually changes with long-term operation, so it is known that daily adjustment work is required. EXAMPLES

[0106] Confirmation of the independence of the ratio of the liquid flow rates of the two liquid phases and the O / A ratio.

[0107] In the mechanism of the present invention, the liquid delivery speed of the heavy liquid phase 4 and the light liquid phase 5 could be set independently of the volume ratio of the two phases involved in the phase mixing (so-called O / A ratio). Specifically, for the mechanisms shown in Figures 1(a) to 1(t), 2(a) to 2(t), 4(a) to 4(p), 6(a) to 6(p), 8(a) to 8(p), 10(a) to 10(p), and 12(a) to 12(p), the ratio of the liquid delivery speed of the heavy liquid phase 4 to the liquid delivery speed of the light liquid phase 5 was changed from 1:1 to 1:10, but it was found that the position of the interface between the two liquid phases in the vessel 1 or room (mixer chamber 30) housing the agitator blade 2 did not change before and after operation. That is, the independence of the liquid delivery speed ratio of the two liquid phases and the O / A ratio was confirmed. EXAMPLES

[0108] The occurrence and stability of emulsion mixtures.

[0109] For the mechanism shown in FIG. 8(m), an experiment was conducted on the occurrence and stability of an emulsion mixture state using ion-exchanged water (pure water) or a 0.1 M aqueous solution of nitric acid as the heavy liquid phase 4 and the above-mentioned alkane-based solvent (ShellSol D70), toluene, methyl isobutyl ketone (MIBK), or n-octanol as the light liquid phase 5. As described later, in the mechanism of the conventional device, it took a considerable amount of time (usually several minutes to several hours) for the emulsion mixture state of the heavy liquid phase 4 and the light liquid phase 5 to stabilize, but in the mechanism of the present invention, both phases could be instantly brought into an emulsion mixture state (within a few seconds to about one minute). That is, by rotating the blade part of the stirring blade 2 installed near the interface between the two liquid phases while feeding and introducing the heavy liquid phase 4 from the top of the container 1 or room (mixer chamber 30) for phase mixing and the light liquid phase 5 from the bottom, it was possible to instantly bring both phases into an emulsion mixture state (emulsion).

[0110] As will be described later, it was found that the rotation speed of the stirring blades 2 required to obtain a stable emulsion mixture state can be much slower than in the case of the conventional device (about two-thirds to half the rotation speed of the conventional device). Furthermore, it was confirmed by droplet observation with a high-speed camera that the emulsion mixture state obtained by the mechanism of the present invention is denser and more homogeneous than that of the conventional device. The difference in the emulsion mixture state was obvious to the naked eye, and no change was observed during operation even after a long period of time. On the other hand, the emulsion mixture state generated by the conventional device sometimes changed over a long period of time.

[0111] Depending on the type of extraction solvent phase (in most cases, the light liquid phase), it may be difficult to form an emulsion phase only by mechanical stirring based on the rotation of the stirring blades. This tendency was particularly evident when a polar organic solvent such as n-octanol was used. In such cases, it was found that the formation of the emulsion phase was promoted by sending the heavy liquid phase, the light liquid phase, or both through a nozzle having a fine hole or a fine tube. Comparative Example 3

[0112] Comparison of the occurrence and stability of emulsion mixture with conventional devices.

[0113] A mechanism corresponding to the conventional device shown in FIG. 23 was fabricated and compared with the mechanism of the present invention shown in FIG. 8(m). The heavy liquid phase 4 and the light liquid phase 5 used were the same as those in Example 4. In the mechanism of FIG. 8(m), both phases could be made into an emulsion state in a few seconds to about one minute, whereas in the mechanism of FIG. 23, it took several minutes to several hours for the emulsion state of both phases to stabilize. In addition, in the mechanism of FIG. 23, in order to obtain a stable emulsion state, it was necessary to increase the rotation speed of the stirring blade 2 by 1.5 to 2 times compared to the mechanism of FIG. 8(m). In the conventional device, it was necessary to reach a homogeneous emulsion state throughout the mixer chamber, and if the rotation speed of the stirring blade 2 was insufficient, a heterogeneous emulsion phase in which dense and sparse areas of the emulsion state were mixed was generated, causing the interface position between the two liquid phases to fluctuate. In addition, depending on the solvent, there were cases where a stable emulsion state was not reached. In particular, there was a tendency for the emulsion phase to be difficult to develop for highly polar solvents such as alcohol. EXAMPLES

[0114] Confirmation of the independence of the rotation speed of the agitator and the liquid delivery speed of the two liquid phases.

[0115] In the conventional device (double-chamber type), increasing the rotation speed of the agitator impeller 2 generates stronger shear forces, which makes it easier for tiny droplets to form that are less likely to coalesce, making it difficult for the emulsion phase to separate. As a result, it is necessary to suppress the migration of the emulsion phase to the settler chamber; however, since the liquid delivery speed also increases in response to an increase in the rotation speed of the agitator impeller 2, the migration of the emulsion phase to the settler chamber is actually promoted.

[0116] It was found that in the mechanism of the present invention, the liquid transfer speeds of the heavy liquid phase and the light liquid phase can be set completely independent of the rotation speed of the stirring blade 2. Specifically, the relationship between the rotation speed of the stirring blade 2 and the liquid transfer speeds of the two liquid phases was examined for the mechanisms shown in Figures 1(a) to 1(t), 2(a) to 2(t), 4(a) to 4(p), 6(a) to 6(p), 8(a) to 8(p), 10(a) to 10(p), and 12(a) to 12(p), and the independence of the two was confirmed. EXAMPLES

[0117] Confirmation of improvement in compatibility.

[0118] In the mechanism of the present invention, it was found that the phase separation is improved by simultaneously carrying out phase separation in the container 1 or room (mixer chamber 30) for mechanical stirring. Specifically, when the mechanisms shown in Figures 1(a) to 1(t), 2(a) to 2(t), 4(a) to 4(p), 6(a) to 6(p), 8(a) to 8(p), 10(a) to 10(p), and 12(a) to 12(p) were compared with the conventional device shown in Figure 23, it was confirmed that the phase separation was significantly improved. In addition, high phase separation means that the processing speed can be increased, and when the same processing speed as that in the case of using the mechanism of the present invention was set for the mechanism of Figure 23, the settler chamber 40 immediately became extremely cloudy, making drainage difficult. EXAMPLES

[0119] Rare earth element extraction and separation experiment.

[0120] According to the mechanism shown in FIG. 4(e) of the present invention, an experiment was conducted to extract and separate two rare earth elements, neodymium (Nd) and samarium (Sm), from an aqueous nitric acid solution using alkyldiamideamine (ADAAM). Specifically, a ShellSol D70 solution containing 0.25M (mol dm-3) ADAAM was used as the light liquid phase, and neodymium (Nd) and samarium (Sm) dissolved in a 1.5 M aqueous nitric acid solution (heavy liquid phase) were extracted and separated into the light liquid phase. ADAAM is a molecular extractant with excellent selective separation ability between rare earth elements, and is particularly suitable for separating middle rare earth elements, such as separating Nd and Sm, which are adjacent to each other in the periodic table.

[0121] For comparison, a batch experiment (batch-type experiment) was conducted in a test tube using the same heavy liquid phase (aqueous phase) and light liquid phase (oil phase) as described above. Equal volumes of heavy liquid phase 4 and light liquid phase 5 were placed in a stoppered test tube and thoroughly shaken using a vertical shaker to reach extraction equilibrium, after which the two liquid phases were separated using a centrifuge. The extraction equilibrium was considered to have been reached when the distribution ratio (the concentration of rare earth elements in the oil phase divided by the concentration of rare earth elements in the aqueous phase) no longer changed with respect to the shaking time.

[0122] Regarding the extraction and separation of Nd and Sm using the molecular extractant ADAAM, the results of an experiment using the setup shown in Figure 4(e) are compared with the results of a batch experiment in a test tube. The results of the experiment using the setup in Figure 4(e) were a distribution ratio of Nd of 8.5 and a distribution ratio of Sm of 0.38. On the other hand, the results of the batch experiment were a distribution ratio of Nd of 5.9 and a distribution ratio of Sm of 0.42.

[0123] The separation factor of Nd from Sm (the distribution ratio of Nd divided by the distribution ratio of Sm) was 22.4 in the experiment using the setup in Figure 4(e) and 14.1 in the batch experiment. Since the results of the batch experiment were obtained at extraction equilibrium, it was found that the separation factor obtained with the setup in Figure 4(e) was larger than that at extraction equilibrium. This result is believed to be due to the improvement of the theoretical plate number through countercurrent contact of the heavy liquid phase (aqueous phase) and the light liquid phase (oil phase) based on the counterflow of both phases.

[0124] In addition, an experiment was also conducted using the conventional device with the structure shown in Figure 23, using the same heavy liquid phase (water phase) and light liquid phase (oil phase) as described above, and the distribution ratio of Nd was 3.2 and that of Sm was 0.23. In other words, the separation factor of Nd from Sm was 13.9, which was almost the same value as the result of the batch experiment (result at extraction equilibrium). EXAMPLES

[0125] Adaptability for circulating fluid flow.

[0126] It was found that the conventional liquid transfer mechanism by overflow is not suitable for circulating liquid transfer, whereas the liquid transfer mechanism by pressure action of the present invention is highly adaptable for circulating liquid transfer. Specifically, it was confirmed that the heavy liquid phase 4 or the light liquid phase 5, or both phases can be easily circulated by the mechanisms shown in Figures 1(a) to 1(o), 2(a) to 2(o), 4(a) to 4(l), 6(a) to 6(l), 8(a) to 8(l), 10(a) to 10(l), and 12(a) to 12(l).

[0127] In addition to facilitating circulatory liquid transfer by switching from liquid transfer by overflow to liquid transfer by pressure action, the volume ratio (so-called O / A ratio) of the heavy liquid phase 4 and the light liquid phase 5 involved in the phase mixing can be set independently of the liquid transfer speed in the mechanism of the present invention, which is another factor that facilitates circulatory liquid transfer. In other words, since the ratio of the liquid transfer speeds of the two liquid phases can be freely set without changing the O / A ratio, it has been found that, for example, processing can be carried out while permanently maintaining a stable emulsion phase under conditions in which the liquid transfer speed for circulating the light liquid phase 5 (in most cases, an oil phase) is significantly increased compared to the liquid transfer speed when the heavy liquid phase 4 (in most cases, an aqueous phase) is transferred in a single pass manner.

[0128] The circulation liquid transfer adaptive mechanism has various advantages. For example, it was confirmed that the circulation liquid transfer mechanism of the present invention described above is effective when dealing with systems with slow extraction speeds or low extraction rates, and can also be used for the multi-stage effect produced by integrating forward extraction, washing, and back extraction and synchronously transferring the liquid in circulation, and for multi-stage synchronous circulation liquid transfer (Patent Application No. 2019-113657). In addition, in cases of difficult separation or precision separation that require multiple stages, it was also found that the use of multi-stage synchronous circulation liquid transfer can significantly downsize the equipment system compared to the multi-stage method (multi-stage number of containers) of the conventional mixer-settler method.

[0129] Based on the results shown in the above-mentioned Examples and Comparative Examples, the following can be considered. First, this mechanism allows a stable emulsion phase to grow more efficiently and over a wider range than the mechanism of the conventional device. That is, the heavy liquid phase introduced from above reaches the emulsion phase only after passing through the light liquid phase without coming into contact with other heavy liquids, and the light liquid phase introduced from below reaches the emulsion phase only after passing through the heavy liquid phase without coming into contact with other light liquids. Therefore, the volume ratio of the heavy liquid phase to the light liquid phase in the emulsion phase can be stably maintained at a nearly constant state at all times.

[0130] Furthermore, since the heavy liquid phase flows from top to bottom and the light liquid phase flows from bottom to top, the two phases necessarily come into countercurrent contact, which increases the theoretical plate number, as in many column-type extraction devices (e.g., spray columns, pulse columns, emulsion flow).

[0131] In the conventional device, the heavy and light liquid phases are mixed and stirred and sent in one direction from the mixer chamber to the settler chamber by overflow, so the ratio of the liquid sending speeds of the heavy and light liquid phases is the volume ratio of the two liquid phases in the mixer chamber. In other words, it is not possible to change the volume ratio of the two phases involved in the phase mixing while maintaining the ratio of the liquid sending speeds of the heavy and light liquid phases, and it is not possible to change the ratio of the liquid sending speeds while maintaining the volume ratio of the two phases.

[0132] That is, the degree of freedom in operation is small in that the operation can only be performed within the bounds (restrictions) that the volume ratio of the heavy liquid phase to the light liquid phase and the ratio of the liquid feed rates of both phases are the same. On the other hand, in the single-chamber system of the present invention, for example, a region where an emulsion phase is generated and a region where an emulsion phase is eliminated coexist in one container used for stirring and mixing two liquid phases, so that one container serves as both a mixer chamber and a settler chamber as in the conventional device. In this case, the volume ratio of the two liquid phases present in the container is independent of the liquid feed rate. Also, in the case of the mixer chamber in the multi-chamber system of the present invention, unlike the mixer chamber of the conventional device, the region where an emulsion phase is generated and a region where an emulsion phase is eliminated coexist in the mixer chamber and communicate with the settler chamber as in the single-chamber system, so that the volume ratio of the two liquid phases present in the mixer chamber in the system of the present invention is independent of the liquid feed rate (details will be described later).

[0133] That is, in the mechanism of the conventional device, if the ratio of the liquid delivery 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 in the mixer chamber does not change. Similarly, if the heavy 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 both consistent, the volume ratio of the two liquid phases in the container does not change. In fact, the heavy liquid phase and the light liquid phase are introduced separately and mixed in the container, but are again discharged separately in a state separated into the heavy liquid phase and the light liquid phase, so the introduction speed and discharge speed of both phases are always consistent. In other words, since the inflow and outflow of both phases are controlled at the inlet (inlet) and the outlet (discharge port) (because the volume of each liquid phase is discharged equal to the volume introduced), the volume ratio of both phases installed in the container is maintained without being affected by the magnitude of the liquid delivery speed. In this case, the liquid delivery speed by the pump or the like is both the introduction speed and the discharge speed. In other words, the liquid flow rate of the heavy liquid phase (=introduction rate = discharge rate) and the liquid flow rate of the light liquid phase (=introduction rate = discharge rate) can be freely set regardless of the volume ratio of the two phases. This also means that the position of the interface between the heavy liquid phase and the light liquid phase in the vessel is independent of the liquid flow rates of the two phases.

[0134] In addition, when the liquid is sent from the mixer chamber to the settler chamber in one direction by overflow, the heavy liquid phase and the light liquid phase are introduced into the mixer chamber separately, but the two phases move from the mixer chamber to the settler chamber without being separated. Therefore, at the outlet from the mixer chamber (the inlet to the settler chamber), individual control of each liquid phase does not work, and the volume of the heavy liquid phase (or the light liquid phase) introduced into the mixer chamber does not necessarily match the volume of the heavy liquid phase (or the light liquid phase) moving from the mixer chamber to the settler chamber. For example, when the operation is started after the heavy liquid phase and the light liquid phase are installed in the mixer chamber, if the ratio of the liquid sending speeds of the two phases and the volume ratio of the two phases at the time of installation are different, the volume ratio of the two phases in the mixer chamber will gradually change. Therefore, in the mechanism of the conventional device (overflow method), the operation is usually started from the state where the mixer chamber is empty.

[0135] In addition, the mechanism of the present invention, in which an area where an emulsion phase is generated and an area where an emulsion phase has disappeared coexist in one container used for stirring and mixing the heavy liquid phase and the light liquid phase, is also superior to the mechanism of the conventional device in terms of phase separation. In the mechanism of the conventional device, the volume ratio of the heavy liquid phase and the light liquid phase at the time of introduction into the mixer chamber needs to be maintained in the emulsion phase moving from the mixer chamber to the settler chamber, and it is preferable that both phases are stirred and mixed homogeneously throughout the mixer chamber, but this is also the cause of poor phase separation. In contrast, in the mechanism of the present invention, in which phase mixing and phase separation by mechanical stirring proceed simultaneously in one container, homogeneous stirring and mixing throughout the container is not necessary, and phase separation occurs from the beginning, so phase separation is significantly improved compared to the conventional device.

[0136] 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 delivered in a single pass manner, but may be delivered in a circulation manner. Conventional liquid delivery mechanisms by overflow are not suitable for circulation delivery, but the mechanism of the present invention is rather suitable for circulation delivery. Circulation delivery is effective when dealing with systems with slow extraction rates or low extraction rates. In addition, such a circulation delivery adaptive mechanism can also be used for the multi-stage effect that occurs when forward extraction, washing, and back extraction are integrated and synchronous circulation delivery is performed, and synchronous circulation delivery multi-stage (Patent Application 2019-113657). In cases of difficult separation or precision separation that requires multiple stages, the use of synchronous circulation delivery multi-stage allows the device system to be significantly downsized compared to the multi-stage method (multi-stage number of containers) of conventional devices.

[0137] The mechanism having the above-mentioned many excellent features can be applied to a container structure separated into a mixer chamber for stirring and mixing the heavy liquid phase and the light liquid phase, and a settler chamber for phase separation, in the same manner as the mechanism of the conventional device. In other words, if communication parts are provided at two places between the ceiling surface and the partition plate of the container that houses the mixer chamber and the settler chamber, and between the bottom surface and the partition plate, so that the heavy liquid phase and the light liquid phase can freely move between the two chambers, it can be treated in the same way as a container structure that is not divided into a mixer chamber and a settler chamber. In this respect, it is fundamentally different from the mechanism of the conventional device in which the stirred and mixed heavy liquid phase and light liquid phase are unidirectionally transferred from the mixer chamber to the settler chamber through a single route by overflow (the two phases cannot move between the mixer chamber and the settler chamber).

[0138] In other words, the only differences between the mechanism of the conventional device and the mechanism of the device of the present invention are the arrangement of the impeller parts of the stirring impeller, the structure of the partition plate, and the positions of the inlet ports of the heavy liquid phase and the light liquid phase, and it is easy to modify the mechanism of the conventional device based on the concept of the present invention. In the mechanism of the conventional device, the positions of the liquid level (interface between the light liquid phase and the gas phase) and the interface between the two liquid phases are often different in the mixer chamber and the settler chamber, and in particular, the position of the interface between the two liquid phases tends to gradually fluctuate as the operation continues, so that the position must be adjusted periodically or as needed. However, if the conventional device is modified according to the present invention, the heavy liquid phase and the light liquid phase in a phase-separated state can freely move between the mixer chamber and the settler chamber, so that the positions (heights) of the liquid levels in both chambers are the same, and the interface between the two liquid phases in the settler chamber is always maintained at the same position without fluctuating, so that adjustment work is not required.

[0139] In the mechanism of the conventional device (overflow type), the volume ratio of the heavy liquid phase to the light liquid phase in the mixer chamber (so-called O / A ratio) corresponds to the ratio of the liquid delivery speeds. Therefore, if you want to more efficiently and effectively mix and mix two liquid phases by arranging the blade part of the impeller near the interface between the two phases, it is necessary to adjust the length of the impeller's rotating shaft according to the liquid delivery speed conditions. On the other hand, if the structure of the partition plate is improved so that the heavy liquid phase and the light liquid phase in a phase-separated state can freely move between the mixer chamber and the settler chamber, such adjustment of the length of the rotating shaft according to the operating conditions becomes unnecessary. For example, the interface position in the mixer chamber can be maintained at the position when the volume ratio of the heavy liquid phase to the light liquid phase is 1:1, while the liquid delivery speeds of both phases can be set independently and freely.

[0140] In addition, in the mechanism of the present invention, the strength of phase mixing and the liquid delivery speed are completely independent. In conventional devices, the rotation speed of the agitating blades affects the liquid delivery speed, so complicated adjustment work that requires skill is required to consider the linkage between the two, but in the device of the present invention, the rotation speed of the agitating blades and the liquid delivery speed are independent, so the adjustment work is greatly reduced.

[0141] In the above description, the upper and / or lower parts of the container are formed with a larger cross-sectional area (projecting shape) than the middle part of the container, thereby promoting phase separation between the heavy and light liquid phases. However, it is also possible to promote the phase separation by partially expanding the cross-sectional area of ​​the middle part of the container more than the cross-sectional areas of the upper and lower parts and attaching a stirring blade with a large diameter thereto. [Industrial Applicability]

[0142] The present invention relates to an extraction and recovery device for a specific substance that is 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 by the difference in the distribution of substances between two immiscible liquid phases, and is widely used industrially. In particular, it is often used for so-called advanced separations, such as separation between substances that are said to be difficult to separate because of similar chemical properties, and high-precision separations that require highly pure substances.

[0143] In industrial liquid-liquid extraction, mechanical stirring is generally used for the phase mixing of a heavy liquid phase (often an aqueous phase) and a light liquid phase (often an oil phase). For example, the mixer-settler method is a method that is said to be synonymous with liquid-liquid extraction, but the device has problems such as difficulty in handling, poor phase separation, low degree of freedom in setting the volume ratio of the two liquid phases involved in the phase mixing (so-called O / A ratio), and large-scale systems for advanced separation requiring multiple stages. By using the device of the present invention, the above problems of the current liquid-liquid extraction using mechanical stirring can be solved, and it is considered that the industrial applicability of liquid-liquid extraction will be further expanded. [Explanation of symbols]

[0144] 1: Container 2: Mixing blade 3: Anti-turbidity partition 4: Heavy liquid phase 5: Light liquid phase 6: Heavy liquid phase delivery line 7: Light liquid phase delivery line 8: Heavy liquid phase pump 9: Light 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 room / S room partition 16: Ceiling surface / partition panel connection area 17: Bottom / Partition connection area 18: Passage opening at the top end of the partition plate 19: Passage hole at the bottom end of the partition plate 20: Upper partition plate 21: Lower partition plate 22: Vertical passage 23: Area of ​​milky mixture 24: Perforated M / S room partition board 25: Horizontal passage 26: Upper joint partition plate 27: Lower joint partition plate 30: Mixer room 40: Settler Room 100: Interface

Claims

1. a first vessel in which a heavy liquid phase and a light liquid phase are placed; a first liquid introducing means for introducing a heavy liquid phase from above the first container; a second liquid introducing means for introducing a light liquid phase from below the first vessel; a stirring means having a stirring blade located at the tip of a rotating shaft having a blade portion for stirring the heavy liquid phase and the light liquid phase in the first vessel; a second vessel in which a stripping solution for recovering the specific substance is placed; a first pipe connected to an upper portion of the first vessel and a lower portion of the second vessel for transferring a light liquid phase present in an upper portion of the first vessel into a stripping liquid in the second vessel; A second pipe for returning the light liquid phase from the upper part of the second vessel to the lower part of the first vessel, The heavy liquid phase and the light liquid phase in the first vessel are arranged to have the same volume as each other, and further The blade portion of the stirring blade is disposed at a distance of up to three times the thickness of the blade portion in either the up or down direction from the interface between the heavy liquid phase and the light liquid phase in the first container, This apparatus for extracting and recovering a specific substance based on liquid-liquid extraction is characterized in that, while rotating the stirring blade, a heavy liquid phase is introduced from above the first container and a light liquid phase is introduced from below, thereby causing both phases to coexist in the first container in an emulsion state and a phase-separated state, and the light liquid phase containing a specific substance that is present in the upper part of the first container in a phase-separated state is fed from below into the second container containing the heavy liquid phase, which is a stripping liquid, and the reset light liquid phase obtained from above the second container is returned to the first container, and the specific substance is recovered in the stripping liquid.

2. 2. The apparatus for extracting and recovering a specific substance based on liquid-liquid extraction according to claim 1, characterized in that the cross-sectional area of ​​the upper or lower part, or both, of the container is larger than the cross-sectional area of ​​the middle part of the container in order to promote phase separation between the heavy liquid phase and the light liquid phase.

3. 3. The apparatus for extracting and recovering a specific substance based on liquid-liquid extraction according to claim 1 or 2, wherein the first liquid introducing means, the second liquid introducing means, or both of them are provided with a nozzle having a fine hole or a fine tube. End

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