Continuous liquid-liquid separator and continuous liquid-liquid separation method

Abstract

To provide a continuous liquid-liquid separator and continuous liquid-liquid separation method, having high versatility in various solution systems without needing any auxiliary device for monitoring of a boundary face or flow rate adjustment.SOLUTION: A continuous liquid-liquid separator comprises a mechanism, introducing a biphase liquid comprising at least two components separating into two phases of light and heavy liquids without completely mutually mixing from an inflow port provided at a side of a chamber and discharging the light and heavy liquids from respective discharge ports provided in the chamber. Both light and heavy liquids are discharged from a higher position than the inflow port of the biphase liquid and besides, a liquid level-adjusting mesh plate making the light liquid only floating from the biphase liquid pass through is provided at the vicinity of the light liquid discharge port.SELECTED DRAWING: Figure 8

Description

[Technical field]

[0001] The present invention relates to a continuous liquid-liquid separator and a continuous liquid-liquid separation method for continuously separating a two-phase liquid into a light liquid and a heavy liquid according to the specific gravity of each liquid. [Background technology]

[0002] In the past, chemical synthesis processes were carried out using a batch method in which reactions and separation / purification were repeated in multiple stages, but this manufacturing method produced a large amount of waste and had a low yield of the product. Therefore, in recent years, in order to reduce the environmental burden and improve cost competitiveness, efforts have been made to switch to a flow method in which multiple reactions and separation / purification of the synthesized products are carried out continuously, achieving both reduced waste and high yield and selectivity. As a means of separating and purifying a product in a flow method, a prior art technique is known in which a liquid to be extracted containing the product is contacted with an extracting liquid agent that is immiscible with the liquid to be extracted, and a two-phase liquid consisting of the liquid to be extracted and the extracting liquid containing the product is separated into liquid-liquid separation according to the specific gravities of each.

[0003] For example, Patent Document 1 describes a continuous liquid separation device that separates a mixed liquid of liquids with different specific gravities that flows into a chamber from a liquid inlet port into layers, and then discharges the upper layer liquid and the lower layer liquid from an upper outlet port and a lower outlet port, respectively, in which the position of the interface in the chamber is monitored by an interface detection means, and a flow rate adjustment means provided on at least one of the outlet paths is controlled to maintain the position of this interface at a predetermined position.

[0004] On the other hand, Non-Patent Document 1 describes a continuous liquid-liquid separator in which small flow paths are provided above and below a hydrophobic porous membrane made of polytetrafluoroethylene, parallel to the membrane surface, with an inlet at one end of the upper flow path, an outlet at the other, and an outlet at one end of the lower flow path. In this separator, a slug flow of water / hexane is passed through the flow path above the hydrophobic porous membrane, whereby hexane permeates the hydrophobic porous membrane and is discharged from the outlet at the end of the flow path below the hydrophobic porous membrane, while water does not permeate the hydrophobic porous membrane and is discharged from the outlet of the flow path above the hydrophobic porous membrane, thereby performing liquid-liquid separation.

[0005] Patent Document 2 describes a continuous liquid-liquid separator that separates a two-phase liquid into a light liquid and a heavy liquid, discharging the light liquid from a light liquid outlet and the heavy liquid from a heavy liquid outlet, in which a heavy liquid permeable porous membrane is installed at the heavy liquid outlet, the heavy liquid permeable porous membrane having a material and pore size that generates a heavy liquid retention force that prevents the light liquid from passing through even due to a pressure difference between the upstream and downstream of the heavy liquid permeable porous membrane, and the light liquid outlet is equipped with a light liquid permeable porous membrane having a pore size and membrane area such that the pressure upstream of the heavy liquid permeable porous membrane does not exceed the heavy liquid retention force. [Prior art documents] [Patent documents]

[0006] [Patent Document 1] JP 2008-6387 A [Patent Document 2] JP 2019-130484 A [Non-patent literature]

[0007] [Non-Patent Document 1] Ind. Eng. Chem. Res. 2013, 52, 10802-10808 Summary of the Invention [Problem to be solved by the invention]

[0008] As described in Patent Document 1, conventional continuous liquid-liquid separators required auxiliary devices, such as an interface monitor and a flow rate control means, for adjusting the liquid feed amount and liquid feed speed conditions in order to keep the interface position between the separated upper and lower layers constant. On the other hand, in the continuous liquid-liquid separators described in Non-Patent Document 1 and Patent Document 2, a porous membrane that allows only one of the heavy liquid or the light liquid to pass through and does not allow the other to pass through is used to separate the heavy liquid and the light liquid, so no additional devices are required to monitor the interface or adjust the flow rate. However, since the selectivity of permeation and non-permeation of the porous membrane is utilized, the material and pore size of the porous membrane must be adjusted according to the wettability of the heavy liquid and the light liquid, and this has poor versatility.

[0009] The present invention has been made in consideration of the above-mentioned current situation, and an object of the present invention is to provide a continuous liquid-liquid separator and a continuous liquid-liquid separation method that do not require any additional devices for monitoring the interface or adjusting the flow rate, and that are highly versatile for use in various solution systems. [Means for solving the problem]

[0010] The present inventors have conducted intensive research to solve the above-mentioned problems and have found that by discharging both the heavy liquid and the light liquid from a position higher than the inlet of the two-phase liquid and providing a liquid level adjustment mesh plate near the outlet of the light liquid which allows only the light liquid floating in the two-phase liquid to pass through, it is possible to continuously separate the two-phase liquid without using a porous membrane which has poor versatility as described in Non-Patent Document 1 and Patent Document 2.

[0011] In order to solve the above problems, the present invention employs the following means based on the above findings. [1] A continuous liquid-liquid separator having a structure in which a two-phase liquid consisting of at least two or more components that are not completely miscible with each other and separate into two phases, a light liquid and a heavy liquid, is introduced through an inlet provided on the side of a chamber, and the light liquid and the heavy liquid are discharged from a light liquid outlet and a heavy liquid outlet provided at a position higher than the inlet, The chamber is provided with, in the order of the inflow direction of the two-phase liquid, a first chamber having the light liquid outlet on one of its side walls, and a second chamber having the heavy liquid outlet on one of its side walls, a partition wall separating the first chamber from the second chamber, a flow path provided below the partition wall and connecting the first chamber to the second chamber, and a liquid level adjusting mesh plate that allows only the light liquid floating in the two-phase liquid placed at the light liquid outlet to pass through, A continuous liquid-liquid separator in which the light liquid outlet and the heavy liquid outlet are at the same height, the upper end of the light liquid outlet exceeds the height of the upper surface of the liquid level adjustment mesh plate, and the lower end of the light liquid outlet is within the height range from the lower surface to the upper surface of the liquid level adjustment mesh plate. [2] A continuous liquid-liquid separator having a structure in which a two-phase liquid consisting of at least two or more components that are not completely miscible with each other and separate into two phases, a light liquid and a heavy liquid, is introduced through an inlet provided on the side of a chamber, and the light liquid and the heavy liquid are discharged from a light liquid outlet and a heavy liquid outlet provided at a position higher than the inlet, The chamber is provided with, in the order of the inflow direction of the two-phase liquid, a first chamber having the light liquid outlet on one of its side walls, and a second chamber having the heavy liquid outlet on one of its side walls, a partition wall separating the first chamber from the second chamber, a flow path provided below the partition wall and connecting the first chamber to the second chamber, and a liquid level adjusting mesh plate that allows only the light liquid floating in the two-phase liquid placed at the light liquid outlet to pass through, The liquid level adjusting mesh plate is located above the inlet and below the light liquid discharge port, and the height h from the upper surface of the liquid level adjusting mesh plate to the lower end of the light liquid discharge port o and the height h from the upper surface of the liquid level adjusting mesh plate to the lower end of the heavy liquid discharge port. w A continuous liquid-liquid separator that satisfies the following formula:

[0012]

number

[0013]

number

[0014] According to the present invention, it is possible to provide a continuous liquid-liquid separator and a continuous liquid-liquid separation method which do not require any additional device for monitoring or adjusting the interface and are highly versatile for use in various solution systems. [Brief description of the drawings]

[0015] [Figure 1] Diagram explaining separation using the difference in specific gravity between heavy and light liquids [Diagram 2] A plot of the height of the interface between the heavy liquid and the light liquid (how) against the density of the light liquid (oil) (ρo). [Diagram 3] FIG. 1 is a diagram illustrating interface fixing by openings in a liquid level adjusting mesh plate according to the present invention. [Figure 4] A diagram explaining an experiment that demonstrated that the pressure (Fm / S) that prevents water from passing through a mesh plate is capillary pressure. [Diagram 5] A plot of the height of the water phase (hw) against the height of the oil phase (cyclohexane) (ho) in the demonstration experiment. [Figure 6] A graph showing the relationship between the inverse of the mesh plate opening radius r (r-1) and the experimentally determined capillary pressure Pc (=Fm / S). [Figure 7] FIG. 1 is a diagram for explaining a first embodiment of the present invention; [Figure 8] FIG. 1 is a rear cross-sectional view showing an example of an apparatus according to a first embodiment of the present invention; [Figure 9] FIG. 1 is a top cross-sectional view illustrating an example of an apparatus according to a first embodiment of the present invention. [Figure 10] FIG. 1 is a diagram illustrating a second embodiment of the present invention. [Figure 11] A photograph of the continuous liquid-liquid separator used in the examples taken from the front. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0016] The present invention provides a separator and separation method that continuously separates a two-phase liquid consisting of at least two or more components that separate into two phases, a light liquid and a heavy liquid, which are completely immiscible with each other, by using the difference in specific gravity between the heavy liquid and the light liquid, and is characterized in that both the heavy liquid and the light liquid are discharged from a position higher than the inlet of the two-phase liquid, and a liquid level adjustment mesh plate that allows only the light liquid floating in the two-phase liquid to pass through is provided at the same height as each of the outlets of the light liquid and the heavy liquid, or at a specified height position between the outlet and inlet of the light liquid, thereby fixing the interface between the light liquid and the heavy liquid, and continuously separating and discharging each of the heavy liquid and the light liquid.

[0017] In the present invention, since only light liquids pass through the openings in the liquid level adjustment mesh plate due to buoyancy, it is only necessary to control the wettability of the liquid level adjustment mesh plate for heavy liquids, and there is no need to control the wettability for both light and heavy liquids as with the porous membranes in Non-Patent Document 1 and Patent Document 2, making it possible to perform versatile continuous liquid-liquid separation.

[0018] Hereinafter, an embodiment of the present invention (hereinafter, sometimes referred to as "the present embodiment") will be described, but this is intended to explain the present invention and is not intended to limit the scope of the present invention. In this specification, the use of "to" indicating a range of values ​​means that the values ​​before and after it are included as the lower limit and upper limit.

[0019] <Continuous liquid-liquid separation using the difference in specific gravity between heavy and light liquids> First, a continuous liquid-liquid separation will be described in which both the heavy liquid and the light liquid are discharged from a position higher than the inlet of the two-phase liquid by utilizing the difference in specific gravity between them. FIG. 1 is a diagram for explaining, as an example, separation using the difference in specific gravity when water and oil are used as the heavy liquid and the light liquid, respectively. In a separator having an oil phase outlet and an aqueous phase outlet at a position higher than the inlet of the two-phase liquid, the height of the oil phase outlet, the height of the aqueous phase outlet, and the height of the interface of the two-phase liquid are respectively defined as H o , H w , and h ow The densities of the oil phase and the water phase are ρ o and ρ w Then, (H o -h ow )ρ o =(H w -h ow )ρ w (However, all variables are positive.) At this time, the aqueous phase and the oil phase are discharged from the oil phase outlet and the aqueous phase outlet, respectively.

[0020] For example, ρ w =1, H w If we set =10, (H o -h ow )ρ o =(10-h ow ) h ow =(10-H o ρ o ) / (1-ρ o ) It becomes. Figure 2 shows the o For h ow This is a plot of In the figure, ◯: H0=12, □: H o =11, ◆:H o =10, ×:H o =9

[0021] h ow > 0, so the oil phase outlet height (H o ) is the height of the aqueous phase outlet (H w ), the applicable density range of oil (light liquid) becomes narrower, as shown in Figure 2. On the other hand, as shown in FIG. 2, the oil phase outlet height (H o ) = Water phase outlet height (H w ) = interface height (h ow ) it is applicable to all oils (light liquids). In this case, however, it is necessary to fix the interface so that the aqueous phase does not discharge from the oil phase outlet. In addition, the oil phase outlet height (H o ) is the height of the aqueous phase outlet (H w ) is applicable to all oils (light liquids). However, even in this case, it is necessary to suppress the interface rise and fix the interface so that the aqueous phase is not discharged from the oil phase outlet. In the present invention, a liquid level adjusting mesh plate is used as a means for fixing the interface.

[0022] The liquid level adjusting mesh plate has openings that allow light liquids to pass through but have a pressure (capillary pressure) that suppresses the passage of heavy liquids. Because light liquids pass through the openings in the mesh plate due to buoyancy, it is only necessary to control the capillary pressure (wettability) in the mesh plate for heavy liquids. The shape of the opening may be either rectangular or round, but if it is rectangular, it shall have an opening diameter converted into a circle of radius r.

[0023] Fig. 3(A) shows the capillary pressure when the heavy liquid is an aqueous phase and the material of the mesh plate is hydrophobic, while Fig. 3(B) is a diagram explaining the capillary pressure when the heavy liquid is an aqueous phase and the material of the mesh plate is hydrophilic. Whether the mesh plate is hydrophobic or hydrophilic, the capillary pressure of the openings in the mesh plate prevents the heavy liquid (aqueous phase) from passing through. When the heavy liquid is an oil phase, a hydrophilic mesh plate is preferable because it provides a large capillary pressure, regardless of whether the light liquid is an oil phase or an aqueous phase.

[0024] <Demonstration experiment> An experiment demonstrating that the pressure that prevents water from passing through the liquid level adjusting mesh plate is capillary pressure will be described below. FIG. 4 is an explanatory diagram of a demonstration experiment using a hydrophobic mesh plate (made of PTFE, width 20 mm × depth 10 mm × thickness 0.5 mm). The pressure that prevents water from passing through is F m / S, oil load pressure F o / S, water load pressure F w / S´, the bottom area of ​​the first chamber in the chamber is S, the bottom area of ​​the second chamber is S´, and the density of the oil is ρ o , density of water ρ w , height of oil phase (cyclohexane) h o , height of the aqueous phase h w , then, F w / S´=F o / S+F m / S ρ w· g · h w =ρ o· g · h o +F m / S Therefore, the height of the water phase (h w ) is expressed by the following relational expression:

[0025]

number

[0026] Four types of hydrophobic mesh plates were used, each with round openings (pitch: distance between holes) having a hole diameter of 0.75 mm (pitch: 1 mm), a hole diameter of 1.0 mm (pitch: 1.5 mm), a hole diameter of 1.5 mm (pitch: 2.5 mm), and a hole diameter of 2 mm (pitch: 1.5 mm). Both the first and second chambers in the chamber were filled with aqueous phase up to the height of the bottom surface of the hydrophobic mesh plate, and then an oil phase (cyclohexane) was dropped from above the first chamber in the chamber to a certain height. From that state, an aqueous phase (heavy liquid) was dropped from above the second chamber in the chamber to raise the water level, and the height of the aqueous phase from the bottom surface of the mesh plate when the water had passed through the mesh was measured. Figure 5 shows the height (h o ) with respect to the height of the water phase (h w ) is plotted. As is clear from the above formula, the slope of the graph is the specific gravity of the oil (ρ o ) and the Y-intercept represents the pressure that prevents water from passing through. Table 1 shows a summary of the hole (opening) diameter, inclination, and Y-intercept of the hydrophobic mesh plate in FIG.

[0027] [Table 1]

[0028] The capillary pressure Pc of a heavy liquid at an opening of radius r is expressed by the following equation. Pc=2γcosθ / r (In the formula, γ represents the interfacial tension between the heavy liquid and the light liquid, and θ represents the contact angle of the heavy liquid.) The pressure that prevents the passage of the heavy liquid through the liquid level adjustment mesh plate (F m Assuming that the pressure (Pc) is the capillary pressure (Pc), it can be expressed by the following equation. F m / S=Pc=2γcosθ / r (γ: interfacial tension between heavy liquid and light liquid, θ: contact angle of heavy liquid, r: mesh opening radius) The following table shows the reciprocal of the radius r of the mesh hole (r -1 ) and the capillary pressure calculated from the Y-intercept.

[0029] [Table 2]

[0030] Figure 6 shows the reciprocal of the radius r of the mesh hole (r -1 ) and the capillary pressure obtained by experiment. The slopes in Figure 6 are all based on the literature value for interfacial tension, cyclohexane-water γ cw =50.49mN, water-PTFEγ wt =40.25mN, Cyclohexane-PTFEγ ct This roughly coincides with the slope of 0.078 when using =1.22mN. This means that the above assumption is correct, and the pressure that prevents water from passing through the mesh plate is the capillary pressure.

[0031] <Liquid level adjustment mesh plate> In an embodiment of the present invention, the opening diameter of the liquid level adjusting mesh plate is preferably about 0.2 to 5.0 mm, and more preferably about 0.75 to 2.0 mm, allowing separation of two-phase solutions with various combinations of two liquids. Furthermore, the pressure preventing water from passing through the liquid level adjustment mesh plate does not change depending on the number of openings in the liquid level adjustment mesh plate or their arrangement (pitch or whether they are evenly arranged), so the number of openings and their arrangement are not particularly limited.

[0032] In the embodiment of the present invention, the thickness of the mesh plate is not particularly limited as long as it does not warp, and is preferably 0.5 mm or more, more preferably 0.5 to 2 mm, and further preferably 0.5 mm.

[0033] In addition, in the embodiments of the present invention, the material of the mesh plate may be either hydrophobic or hydrophilic, and is not particularly limited. For example, hydrophobic materials include polytetrafluoroethylene (PTFE), polyolefin, polystyrene, polyphenylene vinylene, polyvinyl chloride, etc., and when the heavy liquid is water, PTFE is preferred. Examples of hydrophilic materials include hydrophilized polytetrafluoroethylene, acrylic resins such as polymethacrylate, polyamide, polyimide, polyester, polycarbonate, polyether, polyurethane, ceramics, and metals. When the heavy liquid is an organic solvent, polymethacrylate is preferred.

[0034] <Two-phase liquid> The two-phase liquid usable in the embodiment of the present invention is a two-phase liquid consisting of at least two components that are completely immiscible with each other and separate into two phases, a light liquid and a heavy liquid, and examples of such two-phase liquids include water / pentane, water / hexane, water / heptane, water / octane, water / nonane, water / decane, water / cyclohexane, water / decane, water / benzene, water / toluene, water / xylene, water / nitrobenzene, water / aniline, water / phenol, water / methyl acetate, water / ethyl acetate, water / propyl acetate, water / butyl acetate, water / diene, and the like. Examples of suitable solvents include ethyl ether, water / dipropyl ether, water / dibutyl ether, water / diphenyl ether, water / butanol, water / hexanol, water / heptanol, water / octanol, water / nonanol, water / decanol, water / butoxyethanol, water / triethylamine, water / chloroform, water / carbon tetrachloride, Fluorinert / water, methanol / hexane, methanol / cyclohexane, N,N-dimethylformamide / hexane, and N-methyl-2-pyrrolidone / hexane.

[0035] Other examples include three- or more-component two-phase liquids obtained by dissolving an inorganic salt or an organic compound in the two-component two-phase liquid described above, and liquids obtained by dissolving an inorganic salt or an organic compound in a mixture such as water / acetone, water / formaldehyde, water / tetrahydrofuran, water / N,N-dimethylformamide, water / dimethyl sulfoxide, water / methanol, water / ethylene carbonate, or water / acetic acid, and then separating the mixture into two phases, a light liquid and a heavy liquid.

[0036] [First embodiment] FIG. 7 is a diagram showing a first embodiment of the present invention. The first embodiment of the present invention is an embodiment in which the height of the light liquid outlet and the height of the heavy liquid outlet are the same (see

[0021] ).In this embodiment, as shown in Figure 7, a liquid level adjustment mesh plate is provided at the light liquid outlet to allow only the oil phase (light liquid) floating in the two-phase liquid to pass through, thereby fixing the interface between the light liquid (upper layer) and the heavy liquid (lower layer).Even if the height of the light liquid outlet and the height of the heavy liquid outlet are the same, the heavy liquid (lower layer) is not discharged from the light liquid outlet (upper layer outlet).

[0037] In order for the light liquid to float in the two-phase liquid and pass through the mesh plate to be discharged from the outlet, it goes without saying that the thickness of the liquid level adjusting mesh plate installed at the light liquid outlet does not exceed the diameter of the light liquid outlet, but the upper end of the light liquid outlet must exceed the height of the upper surface of the liquid surface mesh plate, and the lower end of the light liquid outlet must be within the range of height from the lower surface to the upper surface of the liquid surface mesh plate.

[0038] 8 and 9 are a rear cross-sectional view and a top cross-sectional view that typically show one example of the device according to the first embodiment of the present invention. The side of the chamber is provided with an inlet for introducing the two-phase liquid. Located within the chamber are a first chamber and a second chamber, a partition wall separating the first chamber and the second chamber, and a flow path connecting the first chamber and the second chamber located below the partition, and the first chamber and the second chamber each have a light liquid outlet and the heavy liquid outlet. The light liquid discharge port and the heavy liquid discharge port are provided at a position higher than the inlet on the other side wall of the chamber, so that the light liquid discharge port and the heavy liquid discharge port are at the same height, and the light liquid and heavy liquid of the two-phase liquid are discharged from both discharge ports, respectively. In addition, a liquid level adjustment mesh plate is provided at the light liquid outlet of the first chamber, which allows only the light liquid floating in the two-phase liquid to pass through, and the interface between the light liquid and the heavy liquid is fixed by the liquid level adjustment mesh plate.

[0039] (Discharge of light and heavy liquids) The two-phase liquid introduced from the inlet separates into a light liquid phase and a heavy liquid phase in the first chamber due to the difference in specific gravity, and only the light liquid passes through the liquid level adjustment mesh plate and is discharged from the light liquid outlet provided on the side wall of the first chamber. On the other hand, of the introduced two-phase liquid, the heavy liquid flows into the second chamber through a flow path provided under the partition and is discharged from a heavy liquid discharge port provided in the side wall of the second chamber.

[0040] (Inlet) An inlet provided on one side wall of the chamber is used to continuously introduce a two-phase liquid using a pump (not shown) or the like, and the pump and the inlet are connected by a pipe (not shown). The material, inner diameter, outer diameter, length, etc. of the pipe are not limited. The position of the inlet is not particularly limited as long as it is a position where the introduced two-phase liquid can flow into the flow path connecting the first and second chambers in the chamber, but it is desirable for it to be located as low as possible below the separator.

[0041] (Light liquid outlet and heavy liquid outlet) In this embodiment, by making the heights of the light liquid outlet and the heavy liquid outlet provided on the side wall of the chamber the same, the heavy liquid and the light liquid can be continuously separated and discharged even if there is a density difference between them. Therefore, the side wall of the chamber in which the light liquid outlet and heavy liquid outlet are located is not particularly limited, except that both outlets must be located at a higher position than the inlet, but the inlet and the light liquid outlet must have a distance sufficient to allow the light liquid in the two-phase liquid to separate and float in the first chamber due to the difference in specific gravity so that the light liquid is discharged from the light liquid outlet provided in the first chamber. To facilitate collection of the discharged liquid, a light liquid collection tube and a heavy liquid collection tube can be connected to the light liquid discharge outlet and the heavy liquid discharge outlet, respectively, but the material, inner diameter, outer diameter, length, etc. of these tubes are not limited.

[0042] [Second embodiment] The second embodiment of the present invention is a height (h o ) is the height of the heavy liquid outlet (h w ) (see

[0021] ), in which the liquid level adjusting mesh plate is provided above the inlet for the two-phase liquid and below the light liquid outlet to fix the interface between the light liquid and the heavy liquid, and the height h of the lower end of the light liquid outlet from the upper surface of the liquid level mesh plate is o and the height h of the lower end of the heavy liquid discharge port w is set to satisfy the following formula:

[0043]

number

[0044] Hereinafter, in the second embodiment, the height h of the lower end of the light liquid outlet o and the height of the lower end of the heavy liquid outlet h w The relationship between these two will be explained. As mentioned above, the pressure that prevents the heavy liquid from passing through the mesh plate is the capillary pressure F m / S, in this embodiment, we considered how far the liquid level adjusting mesh plate can be lowered, or how far the heavy liquid discharge outlet can be raised, when there is a certain amount of pressure from the heavy liquid pressing against the mesh plate.

[0045] As shown in Fig. 10, the height of the light liquid outlet (h o ) is the height of the heavy liquid outlet (h w ), F m / S≧F w / SCIENCE FICTION o / S=P w-o (1) (Wherein, S is the base area of ​​the first chamber, S' is the base area of ​​the second chamber, F m / S is the pressure that prevents water from passing through, F w / S' is the load pressure of water (heavy liquid), F o / S is the load pressure of oil (menstrual fluid), P w-o represents the load pressure difference.) If the above formula is true, it functions as a continuous liquid-liquid separator.

[0046] P w-o =ρ w h w g-ρ o h o ·g =(ρ w h w -ρ o h o )·g···(2) (In the formula, ρ is density, h is the height from the top of the mesh plate to the lower end of the outlet, S is the cross-sectional area of ​​the pipe, and g is the acceleration due to gravity.) Therefore, substituting equation (2) into equation (1) gives F m / S≧(ρ w h w -ρ o h o )·g It becomes. The formula is expressed as h o This can be summarized as follows:

[0047]

number

[0048] On the other hand, the capillary pressure Pc can be expressed by the following equation (4). Pc=2γcosθ / r=F m / S····(4) From the above formulas (3) and (4), the height h of the lower end of the light liquid outlet from the top surface of the mesh plate o and the height of the lower end of the heavy liquid outlet h w is expressed by the following equation (5).

[0049]

number

[0050] The present invention will be specifically described below based on examples. However, the examples are intended to illustrate preferred examples of the present invention, and the present invention is not limited to these examples in any way.

[0051] A device according to a first embodiment of the invention, illustrated in Figures 8 and 9, was used to carry out continuous separation of a two-phase liquid. FIG. 11 is a photograph taken from the front of the continuous liquid-liquid separator used in the examples. The separator is made by a stereolithography 3D printer (formlabs, Form3) using an acrylic monomer. The chamber (external dimensions: width 46 mm x depth 15 mm x height 22 mm), light liquid discharge section and heavy liquid discharge section (external dimensions: diameter 6 mm x length 30 mm, hole diameter 3 mm), inlet (external dimensions: width 15 mm x depth 9 mm x height 14 mm), partition (width 2 mm x depth 10 mm x height 15 mm), first chamber and second chamber (size: width 20 mm x depth 10 mm x height 20 mm), flow path connecting the first chamber and the second chamber (size: width 2 mm x depth 10 mm x height 5 mm), and liquid level adjustment mesh plate (width 20 mm x depth 10 mm x thickness 0.5 mm) are integrally molded at a height (14 mm from the bottom of the first chamber) such that the upper surface of the plate coincides with the lower end of the light liquid discharge port (hole). The opening shape of the liquid level adjusting mesh plate was a square with a wire diameter of 1 mm and a mesh size of 1 mm.

[0052] A liquid inlet tube (PTFE, 1 / 16 inch, inner diameter 1 mm) was connected to the inlet, and a two-phase liquid (slug flow) consisting of cyclohexane and water was introduced at 1 mL / min each. As is clear from the photograph in Figure 11, the water (colored with food coloring) did not pass through the mesh plate, and only cyclohexane (a colorless, transparent liquid) was discharged from the light liquid outlet, allowing for a clean separation. In addition, when a two-phase liquid consisting of cyclohexane and water was introduced at a rate of 5 mL / min each, the water (colored with food coloring) was also able to be separated cleanly without passing through the mesh plate.

[0053] Furthermore, separation of a two-phase liquid was performed in the same manner, except that the material and opening size of the two-phase liquid and the liquid level adjusting mesh plate were changed as shown in Table 3. The liquid level adjusting mesh plate made of polytetrafluoroethylene (PTFE) had the same round openings as those used in the above-mentioned demonstration experiment. The results are shown in Table 3. In the table, "x" indicates that the lower layer (heavy liquid) passed through the mesh plate, and "-" indicates that no experiment was performed.

[0054] [Table 3]

[0055] As a result, it was found that it was possible to separate various two liquids, such as water (heavy liquid) / low polarity solvent (light liquid), water (heavy liquid) / high polarity solvent (light liquid), high specific gravity organic solvent (heavy liquid) / water (light liquid), and organic solvent (heavy liquid) / organic solvent (light liquid). [Industrial Applicability]

[0056] According to the present invention, a product can be obtained in high yield and selectivity using a continuous liquid-liquid separator having a simple configuration, and therefore the present invention can be used in a continuous precision production process for functional chemicals.

Claims

1. A continuous liquid-liquid separator having a structure in which a two-phase liquid consisting of at least two or more kinds of components which are not completely miscible with each other and separate into two phases, a light liquid and a heavy liquid, is introduced through an inlet provided on a side surface of a chamber, and the light liquid and the heavy liquid are respectively discharged through a light liquid outlet and a heavy liquid outlet provided at a position higher than the inlet, The chamber is provided with, in the order of the inflow direction of the two-phase liquid, a first chamber having the light liquid outlet on one of its side walls, and a second chamber having the heavy liquid outlet on one of its side walls, a partition wall separating the first chamber from the second chamber, a flow path provided below the partition wall and connecting the first chamber to the second chamber, and a liquid level adjusting mesh plate that allows only the light liquid floating in the two-phase liquid placed at the light liquid outlet to pass through, A continuous liquid-liquid separator in which the heights of the light liquid outlet and the heavy liquid outlet are the same, the upper end of the light liquid outlet exceeds the height of the upper surface of the liquid surface mesh plate, and the lower end of the light liquid outlet is within the height range from the lower surface to the upper surface of the liquid surface mesh plate.

2. A continuous liquid-liquid separator having a structure in which a two-phase liquid consisting of at least two or more kinds of components which are not completely miscible with each other and separate into two phases, a light liquid and a heavy liquid, is introduced through an inlet provided on a side surface of a chamber, and the light liquid and the heavy liquid are respectively discharged through a light liquid outlet and a heavy liquid outlet provided at a position higher than the inlet, The chamber is provided with, in the order of the inflow direction of the two-phase liquid, a first chamber having the light liquid outlet on one of its side walls, and a second chamber having the heavy liquid outlet on one of its side walls, a partition wall separating the first chamber from the second chamber, a flow path provided below the partition wall and connecting the first chamber to the second chamber, and a liquid level adjusting mesh plate that allows only the light liquid floating in the two-phase liquid placed at the light liquid outlet to pass through, The liquid level adjusting mesh plate is located above the inlet and below the light liquid discharge port, and the height h from the upper surface of the liquid level adjusting mesh plate to the lower end of the light liquid discharge port ｏ and the height h from the upper surface of the liquid level adjusting mesh plate to the lower end of the heavy liquid discharge port. ｗ A continuous liquid-liquid separator that satisfies the following formula: [0010] (In the formula, h ｏ and h ｗ is a positive value, ρ ｏ is the density of the light liquid, ρ ｗ is the density of the heavy liquid, r is the radius of the mesh opening, γ is the interfacial tension between the heavy liquid and the light liquid, and θ is the contact angle.)

3. A continuous liquid-liquid separation method comprising: introducing a two-phase liquid consisting of at least two or more components that are not completely miscible with each other and separate into two phases, a light liquid and a heavy liquid, through an inlet provided on a side surface of a chamber; and discharging the light liquid and the heavy liquid from a light liquid outlet and a heavy liquid outlet provided at a position higher than the inlet, respectively; a first chamber having the light liquid outlet on one of its side walls and a second chamber having the heavy liquid outlet on one of its side walls, the first chamber being disposed inside the chamber in that order in the inflow direction of the two-phase liquid, a partition wall separating the first chamber from the second chamber, a flow path connecting the first chamber to the second chamber, the flow path being disposed below the partition wall, and a liquid level adjusting mesh plate allowing only the light liquid suspended in the two-phase liquid disposed at the light liquid outlet to pass therethrough; A continuous liquid-liquid separation method, in which the light liquid outlet and the heavy liquid outlet are at the same height, and the liquid level adjustment mesh plate is positioned so that the upper end of the light liquid outlet exceeds the height of the upper surface of the liquid level adjustment mesh plate, and the lower end of the light liquid outlet is within the height range from the lower surface to the upper surface of the liquid level adjustment mesh plate.

4. A continuous liquid-liquid separation method comprising: introducing a two-phase liquid consisting of at least two or more components that are not completely miscible with each other and separate into two phases, a light liquid and a heavy liquid, through an inlet provided on a side surface of a chamber; and discharging the light liquid and the heavy liquid from a light liquid outlet and a heavy liquid outlet provided at a position higher than the inlet, respectively; a first chamber having the light liquid outlet on one of its side walls and a second chamber having the heavy liquid outlet on one of its side walls, the first chamber being disposed inside the chamber in that order in the inflow direction of the two-phase liquid, a partition wall separating the first chamber from the second chamber, a flow path connecting the first chamber to the second chamber, the flow path being disposed below the partition wall, and a liquid level adjusting mesh plate allowing only the light liquid suspended in the two-phase liquid disposed at the light liquid outlet to pass therethrough; The liquid level adjusting mesh plate is disposed above the inlet and below the light liquid discharge port, and a height h from the upper surface of the liquid level adjusting mesh plate to the lower end of the light liquid discharge port is set. ｏ and a height h from the upper surface of the liquid level adjusting mesh plate to the lower end of the heavy liquid discharge port. ｗ A continuous liquid-liquid separation method, wherein the following formula is satisfied: [0010] (In the formula, h ｏ and h ｗ is a positive value, ρ ｏ is the density of the light liquid, ρ ｗ is the density of the heavy liquid, r is the radius of the mesh opening, γ is the interfacial tension between the heavy liquid and the light liquid, and θ is the contact angle.)

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