Liquid-liquid distribution device

Abstract

To provide a liquid-liquid distribution device which is a device for distributing a substance contained in a liquid-liquid system having two liquid phases and can realize phase mixing leading to a fine and stable emulsion state while suppressing entrainment.SOLUTION: In a light liquid phase or a heavy liquid phase or both of them, a direction in which liquid droplets move and 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 directions thereof in a zigzagging manner.SELECTED DRAWING: Figure 6(a)

Description

[Technical Field]

[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 on top of the other horizontally (see, for example, Figure 1(a) below) or at an angle to the horizontal (see, for example, Figure 6(a) below), and a zigzag flow path is installed within 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, stable emulsion state. [Background technology]

[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, or recover and 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 perform continuous liquid-liquid distribution using a conventional liquid-liquid distribution device (e.g., a mixer settler), when two liquid phases separate (phase separation), entrainment (entrainment) occurs, 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, causing a significant environmental burden. When mixing two liquid phases (phase mixing), if the phases are mixed finely until an emulsion state is formed, such entrainment is more likely to occur.

[0005] Common methods for bringing two liquid phases into a fine emulsion 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 to a fine emulsion by ejecting droplets from a nozzle (see, for example, Patent Documents 1 and 2). However, regardless of which method is used, the more phases are mixed to reach a finer emulsion, 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. [Prior art documents] [Patent documents]

[0006] [Patent Document 1] Patent No. 5305382 [Patent Document 2] Patent No. 5565719 Summary of the Invention [Problem to be solved by the invention]

[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. [Means for solving the problem]

[0011] The liquid-liquid distributor of the present invention is characterized by a zigzag flow path within a container, in which two or more plates are stacked horizontally (e.g., as shown in Figure 1(a) below) or at an angle from the horizontal (e.g., as shown in Figure 6(a) below), through which each liquid phase alternates between left and right. 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. [Effects of the Invention]

[0012] As mentioned above, conventional liquid-liquid distributors have not been able 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 load. [Brief explanation of the drawings]

[0013] [Figure 1(a)] FIG. 1 is a structural diagram showing an example of a mechanically stirred multi-stage liquid-liquid distributor having a left-right separated double zigzag flow path on the light liquid phase side and a left-right separated double zigzag flow path on the heavy liquid phase side. [Figure 1(b)] FIG. 1 is a structural diagram showing an example of a mechanically stirred single-stage liquid-liquid distributor having a left-right separated double zigzag flow path on the light liquid phase side and a left-right separated double zigzag flow path on the heavy liquid phase side. [Figure 1(c)] FIG. 1 is a structural diagram showing an example of a droplet ejection type multi-stage liquid-liquid distributor having a left-right separated double zigzag flow path on the light liquid phase side and a left-right separated double zigzag flow path on the heavy liquid phase side. [Figure 1(d)] FIG. 1 is a diagram showing an example of a droplet ejection type 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. [Figure 1(e)] FIG. 1 is a diagram showing an example of a droplet ejection type single-stage liquid-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. [Figure 2(a)] FIG. 1 is a structural diagram showing an example of a mechanically stirred multi-stage liquid-liquid distributor having a left-right separated three-fold zigzag flow path on the light liquid phase side and a left-right separated two-fold zigzag flow path on the heavy liquid phase side. [Figure 2(b)] FIG. 1 is a structural diagram showing an example of a mechanically stirred single-stage liquid-liquid distributor having a left-right separated three-fold zigzag flow path on the light liquid phase side and a left-right separated two-fold zigzag flow path on the heavy liquid phase side. [Figure 3(a)] FIG. 1 is a structural diagram showing an example of a mechanically stirred multi-stage liquid-liquid distributor having a four-fold zigzag flow path with left and right separation on the light liquid phase side and a two-fold zigzag flow path with left and right separation on the heavy liquid phase side. [Figure 3(b)] FIG. 1 is a diagram showing an example of a mechanically stirred single-stage liquid-liquid distributor having a four-fold zigzag flow path with left and right separation on the light liquid phase side and a two-fold zigzag flow path with left and right separation on the heavy liquid phase side. [Figure 4(a)] FIG. 1 is a structural diagram showing an example of a mechanically stirred multi-stage liquid-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. [Figure 4(b)] FIG. 1 is a structural 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. [Figure 5(a)] FIG. 1 is a structural 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. [Figure 5(b)] FIG. 1 is a 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. [Figure 6(a)]A schematic diagram showing an example of a mechanically stirred multi-stage liquid distribution device having a double zigzag flow path at the one-way gradient plate on the light liquid phase outlet side and a double zigzag flow path at the one-way gradient plate on the heavy liquid phase outlet side. [Figure 6(b)] A schematic diagram showing an example of a mechanically stirred single-stage liquid-liquid distribution device having a double zigzag flow path at the one-way gradient plate on the light liquid phase outlet side and a double zigzag flow path at the one-way gradient plate on the heavy liquid phase outlet side. [Figure 7(a)] This is a diagram showing an example of a mechanically stirred multi-stage liquid-liquid distributor that combines 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 with an interface position adjuster, as seen from the heavy liquid phase side. [Figure 7(b)] This is a diagram showing an example of a mechanically stirred multi-stage liquid-liquid distributor that combines 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 with an interface position adjuster, as seen from the light liquid phase side. [Figure 7(c)] This is a diagram showing an example of a mechanically stirred single-stage liquid-liquid distributor that combines 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 with an interface position adjuster, as seen from the heavy liquid phase side. [Figure 7(d)] This is a diagram showing an example of a mechanically stirred, single-stage two-liquid distribution device that combines 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 with an interface position adjuster, as seen from the light liquid phase side. [Figure 8(a)] This is a diagram showing an example of a mechanically stirred multi-stage liquid-liquid distributor that combines 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 with a suction / stirring amplifier. [Figure 8(b)] This is a diagram showing an example of a mechanically stirred single-stage liquid-liquid distributor that combines 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 with a suction / stirring amplifier. [Figure 9(a)] An example of a mechanically stirred multi-stage liquid-liquid distributor that combines 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 with an interface position adjuster and a suction / stirring amplifier, as seen from the heavy liquid phase side. [Figure 9(b)]An example of a mechanically stirred multi-stage liquid-liquid distributor, seen from the light liquid phase side, which combines 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 with an interface position adjuster and a suction / stirring amplifier. [Figure 9(c)] An example of a mechanically stirred single-stage liquid-liquid distributor that combines 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 with an interface position adjuster and a suction / stirring amplifier, as seen from the heavy liquid phase side. [Figure 9(d)] An example of a mechanically stirred single-stage liquid-liquid distributor that combines 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 with an interface position adjuster and a suction / stirring amplifier, as seen from the light liquid phase side. [Figure 10] FIG. 2 is a diagram showing the formation and regions of a reaction section and a buffer section in a steady state in the device structure shown in FIG. 1(a). [Figure 11] FIG. 1(b) is a diagram showing the formation and regions of the reaction section and buffer section in the steady state in the device structure shown in FIG. [Figure 12] FIG. 1(c) is a diagram showing the formation and regions of the reaction section and buffer section in the steady state in the device structure shown in FIG. [Figure 13] FIG. 1(d) is a diagram showing the formation and regions of the reaction section and buffer section in the steady state in the device structure shown in FIG. [Figure 14] FIG. 1(e) is a diagram showing the formation and regions of the reaction section and buffer section in the steady state in the device structure shown in FIG. [Figure 15] FIG. 2(b) is a diagram showing the formation and regions of the reaction section and buffer section in the steady state in the device structure shown in FIG. 2(a). [Figure 16] FIG. 2(b) is a diagram showing the formation and regions of the reaction section and buffer section in the steady state in the device structure shown in FIG. 2(b). [Figure 17] FIG. 4 is a diagram showing the formation and regions of the reaction section and buffer section in the steady state in the device structure shown in FIG. 3(a). [Figure 18] FIG. 4 is a diagram showing the formation and regions of the reaction section and buffer section in the steady state in the device structure shown in FIG. 3(b). [Figure 19]FIG. 4(b) is a diagram showing the formation and regions of the reaction section and buffer section in the steady state in the device structure shown in FIG. 4(a). [Figure 20] FIG. 4(b) is a diagram showing the formation and regions of the reaction section and buffer section in a steady state in the device structure shown in FIG. [Figure 21] FIG. 5(b) is a diagram showing the formation and regions of a reaction section and a buffer section in a steady state in the device structure shown in FIG. 5(a). [Figure 22] FIG. 5(b) is a diagram showing the formation and regions of the reaction section and buffer section in a steady state in the device structure shown in FIG. 5(b). [Figure 23] FIG. 7 is a diagram showing the formation and regions of the reaction section and buffer section in the steady state in the device structure shown in FIG. 6(a). [Figure 24] FIG. 7 is a diagram showing the formation and regions of the reaction section and buffer section in the steady state in the device structure shown in FIG. 6(b). [Figure 25(a)] FIG. 7(b) is a diagram showing the formation and regions of a reaction section and a buffer section in a steady state in the device structure shown in FIG. 7(a). [Figure 25(b)] FIG. 7(b) is a diagram showing the formation and regions of the reaction section and buffer section in a steady state in the device structure shown in FIG. [Figure 26(a)] FIG. 7(c) is a diagram showing the formation and regions of the reaction section and buffer section in a steady state in the device structure shown in FIG. [Figure 26(b)] FIG. 7(d) is a diagram showing the formation and regions of the reaction section and buffer section in a steady state in the device structure shown in FIG. [Figure 27] 8(a) is a diagram showing the formation of a reaction section and a buffer section in a steady state and their regions. FIG. [Figure 28] FIG. 8(b) is a diagram showing the formation and regions of the reaction section and buffer section in a steady state in the device structure shown in FIG. 8(b). [Figure 29(a)] FIG. 9(b) is a diagram showing the formation and regions of a reaction section and a buffer section in a steady state in the device structure shown in FIG. 9(a). [Figure 29(b)] FIG. 9(b) is a diagram showing the formation and regions of the reaction section and buffer section in a steady state in the device structure shown in FIG. 9(b). [Figure 30(a)]FIG. 9(c) is a diagram showing the formation and regions of the reaction section and buffer section in a steady state in the device structure shown in FIG. 9(c). [Figure 30(b)] FIG. 9(d) is a diagram showing the formation and regions of the reaction section and buffer section in a steady state in the device structure shown in FIG. 9(d). [Figure 31] This is a diagram showing the configuration of a mechanically stirred multi-stage liquid-liquid distributor without zigzag flow paths, used for comparison with the device structure shown in Figure 5(a). [Figure 32] This 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 Figure 5(b). DETAILED DESCRIPTION OF THE INVENTION

[0014] The present invention relates to a multi-stage or single-stage liquid-liquid distributor characterized in that the vessel for liquid-liquid distribution 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] Figures 1(a) to 9(d) show examples of zigzag flow paths 15, 16 in multi-stage and single-stage liquid-liquid distribution devices 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 the variations are not limited to those shown in these figures.

[0016] First, Figure 1(a) shows an example of a mechanically agitated 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 agitation system, the two liquid phases are mixed using the rotation of the agitator 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 installed, and these 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 at the bottom of the vessel, and where the emulsion reaches the bottom of the zigzag flow path 15 on the light liquid phase side at the top of the vessel. However, if the emulsion does not develop well, the heavy liquid phase, the light liquid phase, or both may pass through. 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] Figure 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 each stage of the multi-stage liquid-liquid distributor 1, and each zigzag flow path 15, 16 is equipped with a vertical plate 18 to prevent liquid from passing through. The flows of the heavy liquid phase and the light liquid phase inside the vessel of the apparatus are indicated by dotted arrows.

[0021] Figure 1(c) shows an example of a droplet-jetting type multistage liquid-liquid distributor with a left-right separated double-zigzag flow path on the light liquid phase side and a left-right separated double-zigzag flow path 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. Nozzles 21 and 22 are installed on each stage, and pumps 20 deliver the liquid phases to the nozzles 21 and 22, respectively. The vessel structure is similar to that of the multistage liquid-liquid distributor 1 shown in Figure 1(a). Separate left-right separated double-zigzag flow paths are installed on both the light and heavy liquid phase sides, and stage dividers 19, vertical plates 18, and overflow plates 17 are also installed. The dotted arrows indicate the flow of the heavy and light liquid phases from the inlet side within the vessel.

[0022] Figure 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, as 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 container 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 flow of the heavy and light liquid phases inside the device vessel is 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 way as in Figure 1(a). The dotted arrows indicate the flow of the heavy liquid phase and light liquid phase from the inlet side inside the device vessel.

[0025] Figure 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 each stage of a 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 with a four-times zigzag flow path 15 (a flow path that alternates between left and right and changes direction four times) on the light liquid phase side and a two-times zigzag flow path 16 on the heavy liquid phase side. The stage divider 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 of the heavy and light liquid phases from the inlet side within the device vessel. Increasing the number of flow changes can more reliably suppress entrainment, but this can also increase pressure loss.

[0027] Figure 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 a multi-stage liquid-liquid distributor, and vertical plates 18 are installed in each of the zigzag flow paths 15 and 16 to prevent liquid from passing through. The flows of the heavy liquid phase and the light liquid phase inside the vessel of the apparatus are indicated by dotted arrows.

[0028] Figure 4(a) shows an example of a mechanically stirred multistage liquid-liquid distributor with a left-right integrated double zigzag channel 15 on the light liquid phase side and a left-right integrated double zigzag channel 16 on the heavy liquid phase side. The stage divider 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 and light liquid phases from the inlet side within the device vessel. The left-right integrated zigzag channel has the advantage of allowing for a longer channel length, which is expected to provide a greater entrainment suppression effect than the left-right separated type. However, because each liquid phase is more likely to pass through without a break than the left-right separated type, the installation of the vertical plate 18 becomes even more important.

[0029] Figure 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 a multi-stage liquid-liquid distributor, and vertical plates 18 are installed in each of the zigzag flow paths 15 and 16 to prevent liquid from passing through. The flows of the heavy liquid phase and the light liquid phase inside the vessel of the apparatus are indicated by dotted arrows.

[0030] Figure 5(a) shows an example of a mechanically stirred multistage liquid-liquid distributor in which a double zigzag flow path 15 is installed only in the light liquid phase outlet direction (light liquid phase outlet side) and a double zigzag flow path 16 is installed only in the heavy liquid phase outlet direction (heavy liquid phase outlet side). The stage divider 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 and light liquid phases from the inlet side within the vessel. The absence of a zigzag flow path toward the inlet allows for a longer flow path length than a system with separate zigzag flow paths 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 the liquid phases are sufficiently separated at the outlet side (entrainment is sufficiently suppressed) and backflow from the inlet to the outlet is controlled.

[0031] Figure 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 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 vessel structure is the same as 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 flows of the heavy liquid phase and light liquid phase inside the vessel of the apparatus are indicated by dotted arrows.

[0032] Figure 6(a) shows an example of a mechanically stirred multistage 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 tiered 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 dotted arrows indicate the flow of the heavy and light liquid phases from the inlet side within the apparatus vessel. The only difference from Figure 5(a) is that the plates forming the zigzag flow paths 15 and 16 are sloped from the horizontal (gradient plates). The gradient from the horizontal here is preferably an angle of about 2 to 20 degrees, but is not limited to this (the appropriate gradient 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 (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 (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, naturally returning to the emulsion state and 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 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 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 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 flows of the heavy liquid phase and light liquid phase inside the vessel are respectively indicated by dotted arrows.

[0035] Figures 7(a) and 7(b) show examples of a mechanically stirred multi-stage liquid-liquid distributor that combines the structure of Figure 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 installing 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 installing 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 upstream of the heavy liquid phase. On the other hand, it is easy to install an overflow plate 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 in separate diagrams, Figures 7(a) and 7(b), respectively. Figure 7(a) shows the configuration of the heavy liquid phase side, and Figure 7(b) shows the configuration 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 diagrams 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 shown in 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 the configuration of the heavy liquid phase side, and Figure 7(d) shows the configuration of the light liquid phase side. The vessel structure is similar to 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 heavy liquid phase side and the light liquid phase side are depicted separately, and are indicated by dotted arrows.

[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, it has a similar mechanism to those 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 two zigzag flow paths 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 effects of suctioning the light liquid phase, the heavy liquid phase, or both, and the effects of mixing the two phases. Specifically, this mechanism has a structure in which agitation blades are installed inside a cylindrical structure, or on the outside of a cylindrical structure near the top or bottom end, or both. This cylindrical structure is equipped with an Ω (ohm)-shaped partition 10 (Ω-shaped with its head facing left when viewed from above) to guide the light liquid phase into the cylindrical structure. The vertical dashed lines in Figure 8(a) indicate the positions where the Ω-shaped partition 10 is fixed to the front and rear walls of the container. At this position, the light liquid phase can pass through the center of the container (the center when viewed from above) but cannot move beyond the head of the Ω-shaped partition 10 located beyond. The cylindrical structure is fitted snugly into the head of the Ω-shaped partition 10.

[0041] Figure 8(b) shows an example of a mechanically stirred single-stage liquid-liquid distributor that combines a suction / stirring amplifier 2 with two zigzag channels 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 channel 15, 16 to prevent liquid from passing through. The flows of the heavy liquid phase and light liquid phase inside the vessel of the apparatus are shown by dotted arrows, respectively.

[0042] By combining the suction / mixing amplifier 2 with the zigzag flow path, a fine phase mixing state can be obtained without increasing the rotation speed of the mixing blades. 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 an example of a mechanically agitated multistage liquid-liquid distributor that combines an interface position adjuster 3 and a suction / agitation amplifier 2 with two zigzag flow paths installed on the light and heavy liquid phase sides. Similar to Figures 7(a) and 7(b), the heavy and light liquid phases are shown in separate diagrams. In these separate diagrams, the flow of the heavy and light liquid phases within the device vessel is indicated by dotted arrows. The tiered 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), 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 channels 15, 16 installed on the light and heavy liquid phase sides. As with Figures 9(a) and 9(b), the heavy and light liquid phase sides are depicted separately. The vessel structure is similar to that of each stage shown in Figures 9(a) and 9(b), with vertical plates 18 installed in each zigzag channel 15, 16 to prevent flow-through. The dotted arrows indicate the flow of the heavy and light liquid phases within the vessels on the heavy and light liquid phase sides, respectively.

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

[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 the regions thereof are shown in Figures 10 to 14. In addition, 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 the regions thereof 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 device 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 device 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 device 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 Figure 29(a) (heavy liquid phase side) and Figure 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 Figure 30(a) (heavy liquid phase side) and Figure 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. [Example]

[0048] Liquid-liquid distribution experiments were conducted using a multistage liquid-liquid distribution device with a zigzag flow path structure, as shown in Figures 9(a) and 9(b), that combines an interface position adjuster 3 and a suction / stirring amplifier 2. Specifically, a sulfuric acid solution containing approximately 3,000 ppm cobalt and approximately 8,000 ppm nickel was neutralized with sodium hydroxide and then purified using a phosphoric acid extractant, PC88A. The PC88A was diluted with an 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) were both set to 20 min, and the extraction yields of cobalt and nickel were measured while varying the pH from 1 to 5. All values ​​were nearly identical to those at chemical equilibrium.

[0049] Furthermore, in the liquid-liquid partitioning experiment, the phase mixture was maintained in a fine and stable emulsion state without entrainment. <Comparative Example 1>

[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 compared with the zigzag flow path of the present invention in terms of the ability to suppress entrainment while maintaining a fine, stable emulsion state. 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 devices shown in Figures 31 and 32 were compared with the zigzag flow path shown in Figures 5(a) and 5(b), which have a similar structure (one more horizontal plate on each side), and the devices shown in Figures 31 and 32 were found to be significantly less able to suppress entrainment while maintaining a fine, stable emulsion state than the devices shown in Figures 5(a) and 5(b). [Industrial Applicability]

[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. [Explanation of symbols]

[0053] 1...Liquid-liquid distribution device 2. Suction and stirring amplifier 3…Interface position adjuster 10...Ω type screen board 11...tube 12...Agitating 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 board 18...Vertical plate 19...Divider board 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 performing forward extraction, washing or stripping, or a combination of these, 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 delivering each of the liquid phases; a zigzag flow path having a structure in which two or more plates are stacked horizontally or at an incline from the horizontal at intervals in the vertical direction, the zigzag flow path being installed at an inlet portion of each stage for a light liquid phase and a heavy liquid phase to each stage or at an outlet portion from each stage, or both, for transferring each liquid phase while alternating between left and right, and further comprising: A tier partition plate is provided between adjacent tiers in the container, and the tier partition plate is connected vertically, A liquid-liquid distribution device characterized in that each stage separated by the stage partition plate has a reaction section in which the distribution reaction of the substance proceeds by phase mixing of the light liquid phase and the heavy liquid phase, and a buffer section in which the phase-separated light liquid phase and heavy liquid phase exist across adjacent stages above and below the container via the reaction section.

2. 2. The liquid-liquid distributor according to claim 1, wherein 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. 3. The liquid-liquid distributor according to claim 1, 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. 4. The liquid-liquid distributor according to claim 1, 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 performing forward extraction, washing or back-extraction 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 delivering each liquid phase; A flow path is provided at an inlet portion or an outlet portion, or both, of the container, for transferring each liquid phase into the container while alternating left and right directions, the flow path having a zigzag flow path structure in which two or more plates are stacked horizontally or at an angle from the horizontal at intervals in the vertical direction, A liquid-liquid distribution device characterized in that a reaction section in which the distribution reaction proceeds by phase mixing of a light liquid phase and a heavy liquid phase, and buffer sections in which the phase-separated light liquid phase and heavy liquid phase exist above and below the container via the reaction section are formed inside the container, the phase-separated light liquid phase is discharged through a zigzag flow path located at the top of the container, and the phase-separated heavy liquid phase is discharged from the reaction section to the outside through a zigzag flow path located at the bottom of the container.

6. 6. The liquid-liquid distributor according to claim 5, wherein 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 by both.

7. 7. The liquid-liquid distributor according to 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. 8. The liquid-liquid distributor according to claim 5, 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.

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