Liquid-liquid distribution device

Abstract

Provided is a liquid-liquid distribution device for distributing a substance contained in a liquid-liquid system having two liquid phases, the liquid-liquid distribution device being capable of achieving phase mixing that attains a fine, stable emulsion state while suppressing entrainment. In a light liquid phase or a heavy liquid phase, or both of these phases, the direction in which liquid droplets move and the linear velocity of the liquid droplets are controlled by installing, within a structure in which two or more plates are vertically stacked, a flow path for shifting the two or more plates while changing the orientations thereof in a zigzagging manner.

Description

liquid-liquid distribution device

[0001] The present invention relates to a liquid-liquid distributor (column) for extracting, washing, or stripping a desired substance, or a combination of these, based on a partition reaction of a substance contained in a liquid-liquid system having two immiscible liquid phases. More specifically, the present invention relates to a liquid-liquid distributor configured in multiple stages or in a single stage, which can achieve phase mixing leading to a fine and stable emulsion state while suppressing entrainment when performing the above operations.

[0002] In the present invention, two or more plates are stacked one above the other either horizontally (see, for example, Figure 1(a) described below) or at an angle to the horizontal (see, for example, Figure 6(a) described below), and a zigzag flow path is installed in the device, through which each liquid phase moves while alternating left and right, thereby achieving both suppression of entrainment and phase mixing leading to a fine and stable emulsion state.

[0003] Liquid-liquid systems consisting of two immiscible liquid phases are widely used in fields such as chemistry. For example, liquid-liquid partitioning (also known as liquid-liquid extraction or solvent extraction), which utilizes the difference in the partitioning of substances between two liquid phases to separate, purify, recover, or remove substances, is extremely important as a method for separating and refining metals and organic compounds, supporting key industries such as the metallurgical and chemical industries, and as a separation and recovery technology for rare metals, which are essential in high-tech industries. Liquid-liquid partitioning is also an important technology in the bioindustry.

[0004] On the other hand, when attempting to continuously perform liquid-liquid distribution using a conventional liquid-liquid distribution device (e.g., a mixer settler), when two liquid phases separate (phase separation), entrainment (entrainment) is likely to occur, in which droplets (fine droplets) of one liquid phase are mixed into the other liquid phase. For example, if entrainment occurs in which an oil phase is entrained in an aqueous phase, oil will be mixed into the wastewater, increasing the environmental load. When mixing two liquid phases (phase mixing), if the phases are mixed finely until an emulsion state is reached, such entrainment is more likely to occur.

[0005] Common methods for bringing two liquid phases into a fine emulsion state are mechanical mixing, such as stirring using rotating impellers or stirring by shaking or vibration. In recent years, however, methods have also been developed for mixing the phases until a fine emulsion state is reached by ejecting droplets from a nozzle (see, for example, Patent Documents 1 and 2). However, regardless of which method is used, the more phase mixing is carried out until a finer emulsion state is reached, the more entrainment occurs. In other words, it has been thought that fine phase mixing and suppression of entrainment cannot be achieved at the same time.

[0006] Patent No. 5305382 Patent No. 5565719

[0007] When performing continuous forward extraction, washing, or stripping, or a combination of these operations based on the partition reaction of substances contained in a liquid-liquid system with two liquid phases, it is necessary to alternately and continuously repeat phase mixing and phase separation of the two liquid phases. To convert the phase mixture to a phase separation state, some kind of action is usually used. For example, settling (gravitational separation by standing) is used, which waits for natural phase separation to occur through the sedimentation and floating actions caused by gravity and buoyancy, or centrifugation is used, which promotes phase separation through the action of centrifugal force.

[0008] However, settling raises problems such as the inability to suppress entrainment and the fact that the phases are discharged without sufficient phase separation unless the settling time is unrealistically long. Also, centrifugation requires the application of a strong centrifugal force to the phase mixture, which results in a large energy load for generating that force.

[0009] On the other hand, when phase mixing and phase separation occur simultaneously, liquid-liquid partitioning can be completed quickly without waiting for gravity separation or the need for centrifugal force. However, even in such cases, fine phase mixing and suppression of entrainment cannot be achieved at the same time. This is similar to the case of gravity separation by settling.

[0010] Therefore, after extensive research into multi-stage liquid-liquid distributors in which phase mixing and phase separation occur simultaneously, we have invented a zigzag flow path mechanism that suppresses entrainment while achieving fine, stable emulsion phase mixing. This zigzag flow path mechanism works in both multi-stage multiple vessels and single-stage single vessels.

[0011] The liquid-liquid distributor of the present invention is characterized by a zigzag flow path through which each liquid phase alternates between left and right as it moves through a structure in which two or more plates are stacked horizontally (e.g., as shown in FIG. 1(a) below) or at an angle to the horizontal (e.g., as shown in FIG. 6(a) below). The zigzag flow path restricts the direction and linear velocity of droplet movement, suppressing entrainment while simultaneously achieving phase mixing leading to a fine, stable emulsion. While the zigzag flow path does not directly result in fine emulsion mixing, the presence of the zigzag flow path, which has a significant entrainment suppression effect, enables strong mixing of two liquid phases, even leading to a finer emulsion. In other words, the suppression of entrainment in the zigzag flow path and fine emulsion mixing are linked.

[0012] As mentioned above, conventional liquid-liquid distributors have been unable to achieve phase mixing leading to a fine, stable emulsion state while suppressing entrainment (achieving both entrainment suppression and fine, stable phase mixing). The present invention provides a multi-stage or single-stage liquid-liquid distributor that solves this problem, enabling more efficient production of metal materials, chemical products, bioproducts, etc., while at the same time significantly reducing the environmental impact.

[0013] 1 is a configuration diagram showing an example of a mechanically stirred multi-stage liquid-liquid distributor having a left-right separated double zigzag channel on the light liquid phase side and a left-right separated double zigzag channel on the heavy liquid phase side. FIG. 2 is a configuration diagram showing an example of a mechanically stirred single-stage liquid-liquid distributor having a left-right separated double zigzag channel on the light liquid phase side and a left-right separated double zigzag channel on the heavy liquid phase side. FIG. 3 is a configuration diagram showing an example of a droplet jetting multi-stage liquid-liquid distributor having a left-right separated double zigzag channel on the light liquid phase side and a left-right separated double zigzag channel on the heavy liquid phase side. FIG. 4 is a configuration diagram showing an example of a droplet jetting single-stage liquid-liquid distributor having a one-way double zigzag channel on the light liquid phase outlet side and a one-way double zigzag channel on the heavy liquid phase outlet side. FIG. 5 is a configuration diagram showing an example of a droplet jetting single-stage liquid-liquid distributor having a left-right integrated double zigzag channel on the light liquid phase side and a left-right integrated double zigzag channel on the heavy liquid phase side. 1 is a configuration diagram showing an example of a mechanically stirred multi-stage liquid-liquid distributor having a light liquid phase side left-right separated three-time zigzag flow path and a heavy liquid phase side left-right separated two-time zigzag flow path. 2 is a configuration diagram showing an example of a mechanically stirred single-stage liquid-liquid distributor having a light liquid phase side left-right separated three-time zigzag flow path and a heavy liquid phase side left-right separated two-time zigzag flow path. 3 is a configuration diagram showing an example of a mechanically stirred multi-stage liquid-liquid distributor having a light liquid phase side left-right separated four-time zigzag flow path and a heavy liquid phase side left-right separated two-time zigzag flow path. 4 is a configuration diagram showing an example of a mechanically stirred single-stage liquid-liquid distributor having a light liquid phase side left-right separated four-time zigzag flow path and a heavy liquid phase side left-right separated two-time zigzag flow path. 5 is a configuration diagram showing an example of a mechanically stirred multi-stage liquid-liquid distributor having a light liquid phase side left-right separated two-time zigzag flow path and a heavy liquid phase side left-right separated two-time zigzag flow path. 1 is a configuration diagram showing an example of a mechanically stirred single-stage liquid distributor having a left-right integrated double-zigzag flow path on the light liquid phase side and a left-right integrated double-zigzag flow path on the heavy liquid phase side. 2 is a configuration diagram showing an example of a mechanically stirred multi-stage liquid distributor having a one-way double-zigzag flow path on the light liquid phase outlet side and a one-way double-zigzag flow path on the heavy liquid phase outlet side. 3 is a configuration diagram showing an example of a mechanically stirred single-stage liquid-liquid distributor having a one-way double-zigzag flow path on the light liquid phase outlet side and a one-way double-zigzag flow path on the heavy liquid phase outlet side. 4 is a configuration diagram showing an example of a mechanically stirred multi-stage liquid distributor having a two-way zigzag flow path on a one-way gradient plate on the light liquid phase outlet side and a two-way zigzag flow path on a one-way gradient plate on the heavy liquid phase outlet side.1 is a configuration diagram showing an example of a mechanically stirred single-stage liquid-liquid distributor having a double-zigzag flow path at a one-way gradient plate on the light liquid phase outlet side and a double-zigzag flow path at a one-way gradient plate on the heavy liquid phase outlet side. 2 is a diagram showing an example of a mechanically stirred multi-stage liquid-liquid distributor in which an interface position adjuster is combined with a one-way double-zigzag flow path at a one-way gradient plate on the light liquid phase outlet side and a one-way double-zigzag flow path at a one-way gradient plate on the heavy liquid phase outlet side. 3 is a diagram showing an example of a mechanically stirred multi-stage liquid-liquid distributor in which an interface position adjuster is combined with a one-way double-zigzag flow path at a one-way gradient plate on the light liquid phase outlet side and a one-way double-zigzag flow path at a one-way gradient plate on the heavy liquid phase outlet side. 4 is a diagram showing an example of a mechanically stirred single-stage liquid-liquid distributor in which an interface position adjuster is combined with a one-way double-zigzag flow path at a one-way gradient plate on the light liquid phase outlet side and a one-way double-zigzag flow path at a one-way gradient plate on the heavy liquid phase outlet side. 1 is a diagram showing an example of a mechanically stirred single-stage two-liquid distributor in which an interface position adjuster is combined with a double zigzag flow path on one side of the light liquid phase outlet and a double zigzag flow path on one side of the heavy liquid phase outlet; FIG. 2 is a structural diagram showing an example of a mechanically stirred multi-stage liquid-liquid distributor in which a suction / stirring amplifier is combined with a double zigzag flow path on one side of the light liquid phase outlet and a double zigzag flow path on one side of the heavy liquid phase outlet; FIG. 3 is a structural diagram showing an example of a mechanically stirred single-stage liquid-liquid distributor in which a suction / stirring amplifier is combined with a double zigzag flow path on one side of the light liquid phase outlet and a double zigzag flow path on one side of the heavy liquid phase outlet; FIG. 4 is a diagram showing an example of a mechanically stirred multi-stage liquid-liquid distributor in which an interface position adjuster and a suction / stirring amplifier are combined with a double zigzag flow path on one side of the light liquid phase outlet and a double zigzag flow path on one side of the heavy liquid phase outlet, as viewed from the heavy liquid phase side. 1A is a diagram showing an example of a mechanically stirred multi-stage liquid-liquid distributor in which an interface position adjuster and a suction / stirring amplifier are combined with a double zigzag flow path on one side of the light liquid phase outlet and a double zigzag flow path on one side of the heavy liquid phase outlet, as viewed from the light liquid phase side. FIG. 1B is a diagram showing an example of a mechanically stirred single-stage liquid-liquid distributor in which an interface position adjuster and a suction / stirring amplifier are combined with a double zigzag flow path on one side of the light liquid phase outlet and a double zigzag flow path on one side of the heavy liquid phase outlet, as viewed from the heavy liquid phase side. FIG. 1C is a diagram showing the formation of a reaction section and a buffer section and their regions in a steady state in the apparatus structure shown in FIG. 1A.FIG. 1(b) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 1(c). FIG. 1(c) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 1(d). FIG. 1(e) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 2(a). FIG. 2(b) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 3(a). FIG. 3(b) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 4(a). FIG. 4(b) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. FIG. 5(a) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 5(b) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 6(a) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 6(b) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 7(a) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 7(b) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 7(c) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 7(d) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 8(a) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 8(b) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 9(a) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG. 9(b), 9(c) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions in the device structure shown in FIG.9(d) is a diagram showing the formation of a reaction section and a buffer section in a steady state in the device structure shown in Fig. 9(d). Fig. 9(a) is a diagram showing the configuration of a mechanically stirred multi-stage liquid-liquid distributor without a zigzag flow path used for comparison with the device structure shown in Fig. 5(a). Fig. 9(b) is a diagram showing the configuration of a mechanically stirred single-stage liquid-liquid distributor without a zigzag flow path used for comparison with the device structure shown in Fig. 5(b).

[0014] The present invention relates to a multi-stage or single-stage liquid-liquid distributor characterized in that the vessel for distributing liquids has a structure in which two or more plates are stacked one on top of the other, either horizontally or at an angle from the horizontal, and has a zigzag flow path through which each liquid phase moves while alternating left and right. The zigzag flow path can also be used in combination with an interface position adjuster or a suction / agitation amplifier, or both.

[0015] 1(a) to 9(d) show examples of zigzag flow paths 15, 16 in a multi-stage and single-stage liquid-liquid distribution device 1 and combinations of the zigzag flow paths 15, 16 with an interface position adjuster 3 or a suction / agitation amplifier 2, or both, but variations are not limited to those shown in these figures.

[0016] First, Figure 1(a) shows an example of a mechanically stirred multi-stage liquid-liquid distributor in which a left-right separated double zigzag flow path 15 (a flow path that changes direction alternately left and right twice) is installed on the light liquid phase side, and a left-right separated double zigzag flow path 16 is also installed on the heavy liquid phase side. In this mechanical stirring system, the two liquid phases are mixed using the rotation of the stirring blades 12. The zigzag flow paths 15, 16 are installed so as to be in close contact with the front and rear walls of the container. In addition, between adjacent stages, stage partition plates 19 that communicate from top to bottom are provided, and the stage partition plates 19 are also installed so as to be in close contact with the front and rear walls of the container.

[0017] It is preferable to operate the vessel in a state where the emulsion reaches the top of the zigzag flow path 16 on the heavy liquid phase side below the vessel and the emulsion reaches the bottom of the zigzag flow path 15 on the light liquid phase side above the vessel. However, if the emulsion does not develop well, the heavy liquid phase, the light liquid phase, or both may pass through. Therefore, to prevent this, a vertical plate 18 is installed. The vertical plate 18 is installed below the zigzag flow path 15 on the light liquid phase side and above the zigzag flow path 16 on the heavy liquid phase side, and the vessel is operated so that the edge of the vertical plate 18 is located within the range of the emulsion.

[0018] Furthermore, an overflow plate 17 is installed in the zigzag flow path 15 on the light liquid phase side. The light liquid phase cannot move to the adjacent stage unless it passes over the overflow plate 17. The overflow plate 17 acts as a weir and adjusts the interface position when the flow rate fluctuates or when the flow rate ratio between the heavy liquid phase and the light liquid phase is extremely high. The overflow plate 17 also prevents diffusive mixing with the light liquid phase of the adjacent stage when the device is stopped.

[0019] The dotted arrows indicate the flows of the heavy and light liquid phases from the inlet side inside the device vessel. The countercurrent contact between the heavy and light liquid phases realizes highly efficient multi-stage liquid-liquid distribution.

[0020] 1(b) shows an example of a mechanically stirred single-stage liquid-liquid distributor in which a left-right separated double zigzag flow path 15 is installed on the light liquid phase side and a left-right separated double zigzag flow path 16 is installed on the heavy liquid phase side. The vessel structure is the same as that of each stage of the multi-stage liquid-liquid distributor 1, and vertical plates 18 are installed in each of the zigzag flow paths 15, 16 to prevent liquid from passing through. The flows of the heavy liquid phase and the light liquid phase inside the vessel are indicated by dotted arrows.

[0021] FIG. 1(c) shows an example of a droplet-jetting type multi-stage liquid-liquid distributor in which a left-right separated double-zigzag flow path is installed on the light liquid phase side and a left-right separated double-zigzag flow path is installed on the heavy liquid phase side. In the droplet-jetting type, the two liquid phases are mixed by ejecting droplets from nozzles 21 and 22. A nozzle 21 for ejecting the heavy liquid phase and a nozzle 22 for ejecting the light liquid phase are installed on each stage, and each liquid phase is delivered to each nozzle 21 and 22 by a pump 20. The vessel structure is similar to that of the multi-stage liquid-liquid distributor 1 shown in FIG. 1(a), with left-right separated double-zigzag flow paths on both the light liquid phase side and the heavy liquid phase side, and a stage partition plate 19, a vertical plate 18, and an overflow plate 17 are also installed in the same manner. The flow of the heavy liquid phase and the light liquid phase from the inlet side within the vessel is indicated by dotted arrows.

[0022] 1(d) shows an example of a droplet jet type single-stage liquid-liquid distributor 1 in which a double zigzag flow path 15 is installed on the outlet side of the light liquid phase and a double zigzag flow path 16 is installed on the outlet side of the heavy liquid phase. The inlet side has a simple structure without a zigzag flow path on the inlet side, since both the light liquid phase and the heavy liquid phase are introduced from nozzles 22 and 21, respectively. The flows of the heavy liquid phase and the light liquid phase inside the device vessel are indicated by dotted arrows.

[0023] Figure 1(e) shows an example of a droplet-jet type single-stage liquid-liquid distributor in which a left-right integrated double zigzag flow path 15 is installed on the light liquid phase side and a left-right integrated double zigzag flow path 16 is installed on the heavy liquid phase side. This device is characterized by the ability to lengthen the zigzag flow path on both the light and heavy liquid phase sides. The flows of the heavy and light liquid phases within the device vessel are indicated by dotted arrows.

[0024] Figure 2(a) shows an example of a mechanically stirred multi-stage liquid-liquid distributor in which a left-right separated three-times zigzag flow path 15 (a flow path that alternates between left and right three times) is installed on the light liquid phase side, and a left-right separated two-times zigzag flow path 16 (a flow path that alternates between left and right two times) is installed on the heavy liquid phase side. The stage partition plate 19, vertical plate 18, and overflow plate 17 are installed in the same manner as in Figure 1(a). The flows of the heavy liquid phase and light liquid phase from the inlet side within the apparatus vessel are indicated by dotted arrows, respectively.

[0025] 2(b) shows an example of a mechanically stirred single-stage liquid-liquid distributor in which a left-right separated three-time zigzag flow path 15 is installed on the light liquid phase side and a left-right separated two-time zigzag flow path 16 is installed on the heavy liquid phase side. The vessel structure is the same as that of each stage of the multi-stage liquid-liquid distributor, and each zigzag flow path is equipped with a vertical plate 18 to prevent flow through. The flows of the heavy liquid phase and the light liquid phase inside the vessel are indicated by dotted arrows.

[0026] Figure 3(a) shows an example of a mechanically stirred multi-stage liquid-liquid distributor in which a four-time zigzag flow path 15 (a flow path that alternates between left and right and changes direction four times) is installed on the light liquid phase side, and a two-time zigzag flow path 16 is installed on the heavy liquid phase side. The stage partition plate 19, vertical plate 18, and overflow plate 17 are installed in the same manner as in Figures 1(a) and 2(a). The dotted arrows indicate the flow from the inlet side of the heavy liquid phase and the light liquid phase within the device vessel. Increasing the number of flow direction changes can more reliably suppress entrainment, but on the other hand, pressure loss may increase.

[0027] 3(b) shows an example of a mechanically stirred single-stage liquid-liquid distributor in which a four-fold zigzag flow path 15 with left-right separation is installed on the light liquid phase side and a two-fold zigzag flow path 16 with left-right separation is installed on the heavy liquid phase side. The vessel structure is the same as that of each stage of the multi-stage liquid-liquid distributor, and vertical plates 18 are installed in each of the zigzag flow paths 15, 16 to prevent liquid from passing through. The flows of the heavy liquid phase and the light liquid phase within the vessel are indicated by dotted arrows.

[0028] Figure 4(a) shows an example of a mechanically stirred multi-stage liquid-liquid distributor in which a left-right integrated double zigzag flow path 15 is installed on the light liquid phase side and a left-right integrated double zigzag flow path 16 is installed on the heavy liquid phase side. The stage partition plate 19, vertical plate 18, and overflow plate 17 are installed in the same manner as in Figures 1(a), 2(a), and 3(a). The dotted arrows indicate the flow of the heavy liquid phase and the light liquid phase from the inlet side within the device vessel. The left-right integrated zigzag flow path has the advantage of allowing for a longer flow path length, which is expected to have a greater entrainment suppression effect than the left-right separated type. However, on the other hand, the liquid phases are more likely to pass through without any separation than the left-right separated type, making the installation of the vertical plate 18 more important.

[0029] 4(b) shows an example of a mechanically stirred single-stage liquid-liquid distributor in which a left-right integrated double zigzag flow path 15 is installed on the light liquid phase side and a left-right integrated double zigzag flow path 16 is installed on the heavy liquid phase side. The vessel structure is the same as that of each stage of the multi-stage liquid-liquid distributor, and vertical plates 18 are installed in each zigzag flow path 15, 16 to prevent liquid from passing through. The flows of the heavy liquid phase and the light liquid phase inside the vessel are indicated by dotted arrows.

[0030] Figure 5(a) shows an example of a mechanically stirred multi-stage liquid-liquid distributor in which a double zigzag flow path 15 is installed only in the outlet direction of the light liquid phase side (light liquid phase outlet side), and a double zigzag flow path 16 is installed only in the outlet direction of the heavy liquid phase side (heavy liquid phase outlet side). The stage partition plate 19, vertical plate 18, and overflow plate 17 are installed in the same manner as in Figures 1(a), 2(a), 3(a), and 4(a). The dotted arrows indicate the flow of the heavy liquid phase and light liquid phase from the inlet side within the device vessel. By not providing a zigzag flow path toward the inlet, the flow path length can be longer than in a system in which zigzag flow paths are installed separately on the left and right sides of the vessel (left-right separation type). This system is based on the idea that a zigzag flow path on the inlet side is unnecessary when each liquid phase is sufficiently phase-separated at the outlet side (entrainment is sufficiently suppressed) and backflow from the inlet to the outlet is controlled.

[0031] 5(b) shows an example of a mechanically stirred single-stage liquid-liquid distributor in which a double zigzag flow path 15 is installed only in the direction of the outlet on the light liquid phase side (light liquid phase outlet side), and a double zigzag flow path 16 is installed only in the direction of the outlet on the heavy liquid phase side (heavy liquid phase outlet side). The vessel structure is the same as that of each stage of a multi-stage liquid-liquid distributor, and each zigzag flow path 15, 16 is equipped with a vertical plate 18 to prevent liquid from passing through. The flow of the heavy liquid phase and the light liquid phase inside the vessel is indicated by dotted arrows.

[0032] Figure 6(a) shows an example of a mechanically stirred multi-stage liquid-liquid distributor, similar to Figure 5(a), in which a double zigzag flow path 15 is installed only in the direction of the light liquid phase outlet (light liquid phase outlet side), and a double zigzag flow path 16 is installed only in the direction of the heavy liquid phase outlet (heavy liquid phase outlet side). The stage partition plate 19, vertical plate 18, and overflow plate 17 are installed in the same manner as in Figures 1(a), 2(a), 3(a), 4(a), and 5(a). The flow of the heavy liquid phase and the light liquid phase from the inlet side within the apparatus vessel is indicated by dotted arrows. The only difference from Figure 5(a) is that the plates forming the zigzag flow paths 15, 16 are plates with a slope from the horizontal (gradient plates). The slope from the horizontal here is preferably, but not limited to, an angle of approximately 2 to 20 degrees (the appropriate slope angle varies depending on the wettability, viscosity, specific gravity, etc. of the liquid phase).

[0033] When the heavy liquid phase flows from left to right, the lower plate in the double zigzag flow path 16 installed at the bottom of the container (on the heavy liquid phase side) is inclined downward from left to right, and the upper plate is inclined upward from left to right. When the light liquid phase flows from right to left, the lower plate in the double zigzag flow path 15 installed at the top of the container (on the light liquid phase side) is inclined downward from right to left, and the upper plate is inclined upward from right to left. This inclination allows the liquid phase (droplets) left behind on the plates after phase separation to slide down due to gravity and buoyancy and naturally return to the emulsion, preventing them from remaining in the container.

[0034] Figure 6(b) shows an example of a mechanically stirred single-stage liquid-liquid distributor in which a double zigzag flow path 15 is installed only in the direction of the outlet on the light liquid phase side (light liquid phase outlet side), and a double zigzag flow path 16 is installed only in the direction of the outlet on the heavy liquid phase side (heavy liquid phase outlet side).The only difference from Figure 5(b) is that the plates forming the zigzag flow path are plates with a slope from horizontal (gradient plates).The vessel structure is the same as each stage of the multi-stage liquid-liquid distributor, and each zigzag flow path 15, 16 is equipped with a vertical plate 18 to prevent flow through.The flow of the heavy liquid phase and the light liquid phase inside the vessel is indicated by dotted arrows.

[0035] 7(a) and 7(b) show examples of a mechanically agitated multistage liquid-liquid distributor that combines the structure of FIG. 5(a) with an interface position adjuster 3. Even in a vessel structure with a zigzag flow path, if the flow rate fluctuates or the flow rate ratio between the heavy liquid phase and the light liquid phase is extreme, it may be necessary to adjust the interface position. Therefore, by providing a weir at the upstream of the flow, the flow rate and liquid level can be adjusted. The interface position adjuster 3 is designed to suppress fluctuations in the interface position by providing an overflow plate 17, which acts as a weir, at the upstream of the liquid phase flow.

[0036] The interface position adjuster shown in Figures 7(a) and 7(b) is an overflow plate 17 installed at the upstream of the heavy liquid phase. On the other hand, it is easy to install an overflow plate at the upstream of the light liquid phase. In fact, Figures 1(a), 1(c), 2(a), 3(a), 4(a), 5(a), and 6(a) show examples in which an overflow plate 17 for adjusting the flow rate and liquid level of the light liquid phase is installed on an extension of a tiered partition plate 19. Thus, the vessel structures are different between the heavy liquid phase side, where the interface position adjuster is installed as an independent system, and the light liquid phase side, where the overflow plate 17 is simply an upward extension of the tiered partition plate 19. Therefore, the heavy liquid phase side and the light liquid phase side are shown as separate diagrams in Figures 7(a) and 7(b), respectively. Figure 7(a) shows a configuration diagram of the heavy liquid phase side, and Figure 7(b) shows a configuration diagram of the light liquid phase side. The tier partition plate 19, vertical plate 18, and light liquid phase side overflow plate 17 are installed in the same manner as in Figures 1(a), 2(a), 3(a), 4(a), 5(a), and 6(a). The flows of the heavy liquid phase and light liquid phase inside the apparatus vessel are indicated by dotted arrows in the drawings showing the heavy liquid phase side and the light liquid phase side separately.

[0037] Figures 7(c) and 7(d) show examples of a mechanically stirred single-stage liquid-liquid distributor in which an interface position adjuster 3 is combined with the structure of Figure 5(b). Similar to Figures 7(a) and 7(b), the heavy liquid phase side and the light liquid phase side are shown separately. Figure 7(c) shows a diagram of the heavy liquid phase side, and Figure 7(d) shows a diagram of the light liquid phase side. The vessel structure is the same as that of each stage of the multi-stage liquid-liquid distributor combined with the heavy liquid phase interface position adjuster 3 shown in Figures 7(a) and 7(c), and each zigzag flow path is equipped with a vertical plate 18 to prevent flow through. The flow of the heavy liquid phase and the light liquid phase within the vessel of the apparatus on the individually depicted heavy liquid phase side and light liquid phase side is indicated by dotted arrows, respectively.

[0038] 7(a) to 7(d) can also be applied to droplet jet type multi-stage and single-stage liquid-liquid distributors. Although not shown in this specification, the structure is similar to that shown in these figures. This is because the structure of the interface position regulator does not depend on the phase mixing method, and the same structure can be applied to droplet jet type liquid-liquid distributors.

[0039] By combining an interface position adjuster with a zigzag flow path, the interface position does not change in response to fluctuations in flow rate. Furthermore, even if the difference in flow rate between the light and heavy liquid phases is extremely large, the normal interface position can always be maintained.

[0040] Figure 8(a) shows an example of a mechanically agitated multistage liquid-liquid distributor that combines a suction / agitation amplifier 2 with a double-zigzag flow path installed on the light liquid phase side and the heavy liquid phase side. The stage divider 19, vertical plate 18, and light liquid phase overflow plate 17 are installed in the same manner as in Figures 1(a), 2(a), 3(a), 4(a), 5(a), 6(a), 7(a), and 7(b). The suction / agitation amplifier here refers to a mechanism for amplifying the effect of suctioning the light liquid phase, the heavy liquid phase, or both, and the effect of mixing the two phases. Specifically, this mechanism has a structure in which an agitator blade is installed inside a cylindrical structure, or on the outside of the cylindrical structure near its upper or lower end, or both. The cylindrical structure is equipped with an Ω (ohm)-shaped partition plate 10 (Ω-shaped, facing left when viewed from above the container) for directing the light liquid phase into the cylindrical structure. The vertical dashed lines in Figure 8(a) indicate the positions where the Ω-shaped partitions 10 are fixed to the front and rear walls of the vessel, and at these positions, the light liquid phase can pass through the center of the vessel (the center when viewed from above) but cannot move beyond the Ω-shaped head portion located beyond. The cylindrical structure is completely fitted into the head portion of the Ω-shaped partition 10.

[0041] Figure 8(b) shows an example of a mechanically agitated single-stage liquid-liquid distributor that combines a suction / agitation amplifier 2 with two zigzag flow paths 15, 16 installed on the light liquid phase side and heavy liquid phase side. The vessel structure is the same as each stage of the multi-stage liquid-liquid distributor shown in Figure 8(a), and vertical plates 18 are installed in each zigzag flow path 15, 16 to prevent liquid from passing through. The flows of the heavy liquid phase and light liquid phase inside the vessel are indicated by dotted arrows.

[0042] By combining the suction / agitation amplifier 2 with the zigzag flow path, a fine phase mixing state can be obtained without increasing the rotation speed of the agitator blade. In addition, because the shear force is not too strong, very fine droplets are not generated, and a highly dense droplet group can be obtained.

[0043] Figures 9(a) and 9(b) show examples of a mechanically agitated multistage liquid-liquid distributor that combines an interface position adjuster 3 and a suction / agitation amplifier 2 with two-fold zigzag flow paths installed on the light and heavy liquid phase sides. As with Figures 7(a) and 7(b), the heavy and light liquid phase sides are shown in separate diagrams. In these separate diagrams, the flows of the heavy and light liquid phases within the device vessel are indicated by dotted arrows. The tiered partition plate 19, vertical plate 18, and light liquid phase overflow plate 17 are installed in the same manner as in Figures 1(a), 2(a), 3(a), 4(a), 5(a), 6(a), 7(a), 7(b), and 8(a).

[0044] Figures 9(c) and 9(d) show examples of a mechanically agitated single-stage liquid-liquid distributor that combines an interface position adjuster 3 and a suction / agitation amplifier 2 with two zigzag flow paths 15, 16 installed on the light liquid phase side and heavy liquid phase side. As with Figures 9(a) and 9(b), the heavy liquid phase side and the light liquid phase side are depicted separately. The vessel structure is the same as that of each stage shown in Figures 9(a) and 9(b), and each zigzag flow path 15, 16 is equipped with a vertical plate 18 to prevent flow through. The flow of the heavy liquid phase and the light liquid phase within the vessel on the individually depicted heavy liquid phase side and light liquid phase side is indicated by dotted arrows, respectively.

[0045] By combining an interface position adjuster and a suction / agitation amplifier with a zigzag flow path, both of the above-mentioned effects (the effect of the interface position adjuster and the effect of the suction / agitation amplifier) ​​can be obtained simultaneously.

[0046] The formation of the reaction section 14 and the buffer section 13 in the steady state in the device structures shown in Figures 1(a) to 1(e) and the appearance of these regions are shown in Figures 10 to 14. The formation of the reaction section 14 and the buffer section 13 in the steady state in the device structures shown in Figures 2(a) and 2(b), 3(a) and 3(b), 4(a) and 4(b), 5(a) and 5(b), and 6(a) and 6(b) and the appearance of these regions are shown in Figures 15 and 16, 17 and 18, 19 and 20, 21 and 22, and 23 and 24, respectively. 25(a) (heavy liquid phase side) and 25(b) (light liquid phase side) show the formation of the reaction section 14 and buffer section 13 in the steady state for the heavy liquid phase side and light liquid phase side apparatus structures shown in Figures 7(a) and 7(b), respectively, and Figures 26(a) (heavy liquid phase side) and 26(b) (light liquid phase side) show the formation of the reaction section 14 and buffer section 13 in the steady state for the heavy liquid phase side and light liquid phase side apparatus structures shown in Figures 7(c) and 7(d), respectively. 27 and 28 show the formation of the reaction section 14 and buffer section 13 in the steady state for the apparatus structures shown in Figures 8(a) and 8(b), respectively. Furthermore, the formation of the reaction section 14 and buffer section 13 in the steady state and the state of the area thereof for the heavy liquid phase side and light liquid phase side apparatus structures shown in Figures 9(a) and 9(b) are shown in Figures 29(a) (heavy liquid phase side) and 29(b) (light liquid phase side), and the formation of the reaction section 14 and buffer section 13 in the steady state and the state of the area thereof for the heavy liquid phase side and light liquid phase side apparatus structures shown in Figures 9(c) and 9(d) are shown in Figures 30(a) (heavy liquid phase side) and 30(b) (light liquid phase side).

[0047] In both of the above cases, in the steady state, a fine and stable emulsion phase mixture was maintained in the reaction section 14, and phase separation without entrainment was maintained in the buffer section 13.

[0048] A liquid-liquid distribution experiment was conducted using a multistage liquid-liquid distribution device with a zigzag flow path structure, as shown in Figures 9(a) and 9(b), that combined an interface position adjuster 3 and a suction / agitation amplifier 2. Specifically, a sulfuric acid aqueous solution containing approximately 3,000 ppm cobalt and approximately 8,000 ppm nickel was neutralized with sodium hydroxide, and cobalt and nickel were separated and purified using the phosphoric acid extractant PC88A. The PC88A was diluted with the alkane solvent D80 to a concentration of 20 vol%. The residence times of the light liquid phase (20 vol% PC88A / D80) and the heavy liquid phase (cobalt- and nickel-containing aqueous solution) in the device were both 20 minutes, and the extraction rates of cobalt and nickel were determined while varying the pH from 1 to 5. All values ​​were approximately equal to those at chemical equilibrium.

[0049] Furthermore, in the liquid-liquid distribution experiment, no entrainment occurred and the phase mixture was maintained in a fine, stable emulsion state.

[0050] A multi-stage liquid-liquid distributor shown in Figure 31 and a single-stage liquid-liquid distributor shown in Figure 32 were fabricated, and their ability to suppress entrainment while maintaining a fine, stable emulsion state was compared with the zigzag flow path of the present invention. The devices shown in Figures 31 and 32 also have flow paths using horizontal plates, but they do not have zigzag flow paths consisting of two or more plates. The systems shown in Figures 31 and 32 were compared with the similarly structured zigzag flow path systems shown in Figures 5(a) and 5(b) (which have one more horizontal plate on each side), and the systems shown in Figures 31 and 32 were found to be significantly less effective at suppressing entrainment while maintaining a fine, stable emulsion state than the systems shown in Figures 5(a) and 5(b).

[0051] The present invention applies a zigzag flow path mechanism to multi-stage and single-stage liquid-liquid distributors in which phase mixing and phase separation occur simultaneously, thereby achieving both suppression of entrainment and fine, stable emulsion phase mixing. Generally, these are in an exchange relationship, and when attempting to perform phase mixing in a fine, stable emulsion state, entrainment is likely to occur, while when attempting to suppress entrainment, phase mixing in a fine, stable emulsion state becomes difficult.

[0052] If the present invention can achieve both suppression of entrainment and phase mixing in a fine, stable emulsion state, the efficiency of liquid-liquid distribution will be significantly improved, which is expected to bring about innovation in a wide variety of industrial fields that use two-liquid phase systems, such as metals, chemistry, biology, and semiconductors.

[0053] DESCRIPTION OF SYMBOLS 1...Liquid-liquid distributor 2...Suction / stirring amplifier 3...Interface position adjuster 10...Ω-shaped partition plate 11...Cylinder 12...Stirring blade 13...Buffer section 14...Reaction section 15...Zigzag flow path on the light liquid phase side 16...Zigzag flow path on the heavy liquid phase side 17...Overflow plate 18...Vertical plate 19...Step partition plate 20...Pump 21...Nozzle for heavy liquid phase 22...Nozzle for light liquid phase

Claims

1. A liquid-liquid distribution device comprising a multi-stage vessel for carrying out forward extraction, washing or back-extraction, or a combination of these, based on the partition reaction of a substance contained in a liquid-liquid system having two liquid phases, a light liquid phase and a heavy liquid phase, and a pump for transporting each of the liquid phases, the liquid-liquid distribution device comprising: a multi-stage vessel; and a pump for transporting each of the liquid phases, the multi-stage vessel having a zigzag flow path in which two or more plates are stacked horizontally or at an incline from the horizontal and spaced apart from one another, and which is installed at the inlet portion of each stage for the light liquid phase and the heavy liquid phase to each stage or at the outlet portion of each stage, or both, for transporting each liquid phase while alternating left and right; and a tier partition plate that communicates vertically with adjacent stages within the vessel, the liquid-liquid distribution device comprising: a reaction section within each of the stages separated by the tier partition plate where the partition reaction of the substance progresses through phase mixing of the light liquid phase and the heavy liquid phase; and a buffer section within which the phase-separated light liquid phase and the heavy liquid phase exist across adjacent stages above and below the vessel, via the reaction section.

2. A liquid-liquid distributor according to claim 1, characterized in that the phase mixing of the light liquid phase and the heavy liquid phase is carried out by mechanical stirring using a stirring blade or by ejecting droplets from a nozzle, or both.

3. A liquid-liquid distributor as claimed in claim 1 or 2, further comprising an interface position adjuster that suppresses fluctuations in the interface position by installing an overflow plate that acts as a weir ahead of the liquid phase flow.

4. A liquid-liquid distributor as claimed in any one of claims 1 to 3, further comprising a suction / agitation amplifier for amplifying the effect of suctioning the light liquid phase or the heavy liquid phase or both and the effect of mixing the two phases.

5. A liquid-liquid distribution device comprising a single vessel for carrying out forward extraction, washing or back-extraction based on a partition reaction of a substance contained in a liquid-liquid system having two liquid phases, a light liquid phase and a heavy liquid phase, and a pump for transporting each liquid phase, wherein the liquid-liquid distribution device is provided at the inlet or outlet portion or both of the vessel, and wherein the liquid phases are transported into the vessel while alternately changing direction, and the liquid-liquid distribution device comprises a zigzag flow path having a structure in which two or more plates are stacked horizontally or at an angle from the horizontal and spaced apart from one another, and wherein the vessel is provided with a reaction section inside which the partition reaction proceeds by phase mixing of the light liquid phase and the heavy liquid phase, and buffer sections above and below the vessel where the phase-separated light liquid phase and heavy liquid phase are present via the reaction section, and the phase-separated light liquid phase is discharged through the zigzag flow path located at the top of the vessel, and the phase-separated heavy liquid phase is discharged from the reaction section to the outside through the zigzag flow path located at the bottom of the vessel.

6. A liquid-liquid distributor according to claim 5, characterized in that the phase mixing of the light liquid phase and the heavy liquid phase is carried out by mechanical stirring using a stirring blade, or by ejecting droplets from a nozzle, or both.

7. A liquid-liquid distributor as claimed in claim 5 or 6, further comprising an interface position adjuster that suppresses fluctuations in the interface position by installing an overflow plate that acts as a weir ahead of the liquid phase flow.

8. A liquid-liquid distributor according to any one of claims 5 to 7, further comprising a suction / agitation amplifier for amplifying the effect of sucking the light liquid phase or the heavy liquid phase, or both, and the effect of mixing the two phases.

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