Continuous separation device and method for slug flow

Abstract

To provide a continuous separation device enabling separation and discharge by fluid type, by detecting the liquid type by a sensor provided to a channel of a slag flow to switch an outlet of a destination of a flow by a valve bound to the sensor, and a method of improving a separation rate by a simple and a versatile method without necessitating a particular device such as time correction of a valve operation in the continuous separation method.SOLUTION: In a continuous separation method, a contraction portion is provided to extend a slug length of a slug flow passing through a branch point from a sensor location and / or a slag expanding portion aimed to generate a slag flow having a larger slag volume by confluence of slag flows is provided on an upstream side than the sensor location, thereby the slag length of the slag flow passing the sensor location is extended to improve a separation rate.SELECTED DRAWING: Figure 4

Description

[Technical Field]

[0001] The present invention relates to a continuous separation device and method for slug flow, and more particularly to a continuous separation device and method that detects fluid types using sensors provided in the flow path of the slug flow, and separates and discharges each fluid type. [Background technology]

[0002] In the synthesis of chemical products, production has traditionally been carried out using a batch method in which reactions and separation / purification are repeated in multiple stages, but this production method generates a large amount of waste and has 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 (flow process) in which multi-stage reactions and separation / purification of the synthesized products are carried out continuously, achieving both reduced waste and high yield and selectivity (Non-Patent Document 1).

[0003] In flow processes, operations such as temperature control, pressure control, mixing, reaction, extraction, separation and purification are performed while a fluid flows through a pipe or equipment connected to the pipe. Particularly important in flow processes are processes involving the flow of multiphase fluids that are partially or completely soluble in each other (for example, liquid-liquid reactions, gas-liquid reactions, liquid-liquid extraction, gas-liquid extraction, gas-liquid separation, and liquid-liquid separation).

[0004] In a flow process, after producing a chemical substance, a known method for separating and purifying the resulting product is to contact a liquid to be extracted containing the product with an extracting agent that is immiscible with the liquid to be extracted, and then separate the two-phase liquid consisting of the liquid to be extracted and the extracting agent containing the product into liquid-liquid phases according to their respective specific gravities.

[0005] 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, and that monitors the position of the interface in the chamber using an interface detection means and controls a flow rate adjustment means provided on at least one of the outlet paths so as to maintain the position of this interface at a predetermined position. In such so-called settler-type separation devices, if the two phases have similar specific gravities, it takes time for the upper and lower phases to separate.

[0006] Liquid-liquid separation using a porous membrane has also been proposed. For example, Non-Patent Document 2 describes a continuous liquid-liquid separator in which minute 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, and the 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 the 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.

[0007] Patent Document 2 also 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, and the heavy liquid permeable porous membrane has a material and pore size that generates a heavy liquid retention force that prevents the light liquid from passing through even when there is 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 that has a pore size and membrane area that prevent the pressure upstream of the heavy liquid permeable porous membrane from exceeding the heavy liquid retention force. However, these porous membranes require adjustment of the membrane's affinity for the solution, and when two phases with similar specific gravities are involved, separation of the upper and lower phases takes time.

[0008] On the other hand, in flow processes involving multiphase fluids, reducing interphase mass transfer resistance is important when aiming for process compactness and high-speed processing. In multiphase fluid processes, compacting equipment is also an important factor, actively utilizing flow conditions favorable for the target unit operation. Flow processes typically aimed at small-scale production are smaller in scale and have lower flow rates than batch processes, resulting in low Reynolds numbers and predominantly laminar flow. Even in this laminar flow regime, slug flow (also known as segmented flow or Taylor flow, shown in Figures 1(a) and 1(b)), in which separate fluids of different phases alternate, reduces mass transfer resistance by promoting interface renewal through internal circulation within the slug due to shear from the wall. Furthermore, the ability to form large fluid masses offers the advantage of relatively short phase separation times. Therefore, the use of slug flow has been investigated for continuous processes involving a wide variety of chemicals, including functional chemicals, from reaction and extraction to separation and purification (Patent Document 3).

[0009] In such flow processes using slug flows, methods have been proposed that do not use settlers or porous membranes as a means of separating and purifying products. For example, the two-liquid separation device described in Non-Patent Document 3 (Figures 3 and 4) is a separation device that has a three-way flow path (Y-shaped flow path) connected to the downstream of the flow path through which the slug flows, with a steel tube connected to one of the two outlets and a PTFE tube connected to the other. This device utilizes the fact that the aqueous phase, which is easily wetted (has affinity) with steel, easily flows through the steel tube, and the organic phase, which is easily wetted (has affinity) with PTFE, easily flows through the PTFE tube. However, when using this device, the difference in wettability between the two phases must be large to some extent, and the material of the flow path must be adjusted depending on the type of fluid.

[0010] The separation device described in Non-Patent Document 4 (Figure 1) and Non-Patent Document 5 (Chapter 4) is a device that detects the type of liquid in the slug flow using a sensor installed in the flow path and enables separation of two liquids by switching the outlet to which the liquid flows using a valve linked to the sensor depending on the type of liquid. These devices have advantages over the devices described in Patent Documents 1 and 2 and Non-Patent Document 2, such as being capable of separating two-phase fluids even when there is no difference in specific gravity, and being a separation method that is independent of the membrane or flow path material. [Prior art documents] [Patent documents]

[0011] [Patent Document 1] Japanese Patent Application Laid-Open No. 2008-6387 [Patent Document 2] Japanese Patent Application Publication No. 2019-130484 [Patent Document 3] Japanese Patent Publication No. 2020-32346 [Non-patent literature]

[0012] [Non-Patent Document 1] NEDO, "Development of Continuous Precision Production Process Technology for Functional Chemicals," 2020 / 06 / 25, https: / / www.nedo.go.jp / activities / ZZJP_100152.html, "Development of Continuous Precision Production Process Technology for Functional Chemicals" Basic Plan, https: / / www.nedo.go.jp / content / 100893512.pdf (Last updated March 3, 2021) [Non-patent document 2] Andrea Adamo, Patrick L. Heider, Nopphon Weeranoppanant, and KlavsF. JensenInd. Membrane-Based, Liquid-Liquid Separator with Integrated PressureControl, Ind. Eng. Chem. Res. 2013, 52, 10802-10808 [Non-patent document 3] MN Kashid, YM Harshe, and DW Agar, Liquid-LiquidSlug Flow in a Capillary: An Alternative to Suspended Drop or Film Contactors, Ind. Eng. Chem. Res. 2007, 46, 8420-8430 [Non-patent document 4] Shusaku Asano, Yu Takahashi, Taisuke Maki, Yosuke Muranaka, Nikolay Cherkasov & Kazuhiro Mae, Contactless mass transfer for intra-droplet extraction, Scientific Reports, 10 (2020), pp.7685-7693 [Non-patent document 5] Nobutaka Kadowaki, Development and Application of Three-Way Solenoid Valves for Micro Chemical Processes, Okayama University Graduate School Doctoral Dissertation, Chapter 4, March 2014 Summary of the Invention [Problem to be solved by the invention]

[0013] However, in a continuous separation device using a sensor, the distance from the sensor to the branch point is a factor in reducing the separation rate. Figure 2 shows an overview of a continuous separation device described in Non-Patent Document 4 (Figure 1), which detects the fluid type using a sensor installed in the flow path and enables separation of a two-phase slug flow by switching the flow destination between outlet A and outlet B. In this device, as shown in Figure 3, there is a certain distance (L ) between the position of the sensor that detects the fluid type and the branch point of the flow path that connects the A-side outlet and the B-side outlet. gap ), the moment the sensor detects the interface of the two-phase slug flow, the two-way valves switch simultaneously. gap The other fluid is discharged to the outlet by the volume of the flow path, and the separation rate of the two-phase slug flow deteriorates.

[0014] Non-Patent Document 5 addresses this issue by providing a mechanism for correcting the two-liquid separation rate by delaying the valve operation by the time it takes for the fluid to travel from the sensor position to the branch point, based on the distance from the sensor position to the branch point and the flow velocity. However, the configuration described in this document requires that the correction time for the delay operation be reset each time the flow velocity is changed, which makes it less versatile.

[0015] The present invention has been made in consideration of the current situation, and an object of the present invention is to provide an apparatus and method for improving the separation rate using a simple and versatile technique, without requiring any special mechanism such as time correction of the valve operation. [Means for solving the problem]

[0016] The present inventors have conducted extensive research to solve the above problems, and have found that the sensor Installation location From the branch point length (Lgap) vs. the net passing Slug length of slug flow If we could increase (Lslug), that is, if we could make Lslug >> Lgap, we could expect an improvement in the separation rate according to the formula for the theoretical separation rate: (theoretical separation rate [%]) ≒ (1 - Lgap / Lslug) × 100. The slug length of the slug flow ( Lslug ) We have found that by using the following (1) and (2) as a method for extending the slug flow, it is possible to continuously separate the slug flow without using a mechanism with poor versatility such as that described in Non-Patent Document 5. (1) Providing a contraction section to extend the length of the slug flow passing from the sensor position through the branch point, and (2) Providing a divergence section upstream of the sensor position in the flow path intended to generate a slug flow with a larger slug volume by combining the slug flows.

[0017] In order to solve the above problems, the present invention employs the following means based on the above findings. [1] Complex a flow channel into which a slug flow consisting of several fluid species enters; branching means for branching the flow path into a plurality of flow paths provided for each of the fluid types; a sensor provided in the flow path upstream of the branching means for detecting a plurality of fluid types in the slug flow; a means for switching the plurality of flow paths in response to the fluid type detected by the sensor, thereby separating and discharging the slug flow into the plurality of branched flow paths according to the fluid type; of A continuous separation device for separating and discharging a slug flow consisting of a plurality of fluid types, , a narrowed flow section in which the flow path width of the slug flow is narrowed, From the upstream side of the installation position of the sensor in the flow path to the branch point of the flow path, or The sensor is provided in the flow path from the installation position of the sensor to the branch point of the flow path. 、 For all of the plurality of fluid types, the length (Lgap) from the installation position of the sensor to the branch point / the amount of fluid detected by the sensor , passing through the contracted flow section Slug length of slug flow (Lslug)≦0.5 、 A continuous separation device. [2] The continuous separation device according to [1], wherein the flow contraction section is provided from the upstream side of the installation position of the sensor in the flow path to the branch point of the flow path. [3] Complex a flow channel into which a slug flow consisting of several fluid species enters; branching means for branching the flow path into a plurality of flow paths provided for each fluid type; a sensor provided in the flow path upstream of the branching means for detecting a plurality of fluid types in the slug flow; a means for switching the plurality of flow paths in response to the fluid type detected by the sensor, thereby separating and discharging the slug flow into the plurality of branched flow paths according to the fluid type; of A continuous separation device for separating and discharging a slug flow consisting of a plurality of fluid types, , A flow expansion section in which the flow path width of the slug flow is expanded is provided upstream of the installation position of the sensor in the flow path. 、 For all of the plurality of fluid types, the length (Lgap) from the installation position of the sensor to the branch point / the amount of fluid detected by the sensor , after passing through the diverging section Slug length of slug flow (Lslug)≦0.5 、 A continuous separation device. [4] A continuous separation device as described in [3], in which a constriction section is provided from the end position of the expansion section to the branching point of the flow path, in which the flow path width of the slug flow is narrower than the flow path width before the expansion section. [5] Complex a flow channel into which a slug flow consisting of several fluid species enters; branching means for branching the flow path into a plurality of flow paths provided for each of the fluid types; a sensor provided in the flow path upstream of the branching means for detecting a plurality of fluid types in the slug flow; a means for switching the plurality of flow paths in response to the fluid type detected by the sensor, thereby separating and discharging the slug flow into the plurality of branched flow paths according to the fluid type; Using A continuous separation method for separating and discharging a slug flow consisting of a plurality of fluid types, , a narrowed flow section in which the flow path width of the slug flow is narrowed, From the upstream side of the installation position of the sensor in the flow path to the branch point of the flow path, or The sensor is provided in the flow path from the installation position of the sensor to the branch point of the flow path. 、 For all of the plurality of fluid types, the length (Lgap) from the installation position of the sensor to the branch point / the amount of fluid detected by the sensor , passing through the contracted flow section Slug length of slug flow (Lslug)≦0.5 、 A continuous separation method. [6] The continuous separation method according to [5], wherein the flow contraction section is provided from the upstream side of the installation position of the sensor in the flow channel to a branch point of the flow channel. [7] Complex a flow channel into which a slug flow consisting of several fluid species enters; branching means for branching the flow path into a plurality of flow paths provided for each of the fluid types; a sensor provided in the flow path upstream of the branching means for detecting a plurality of fluid types in the slug flow; a means for switching the plurality of flow paths in response to the fluid type detected by the sensor, thereby separating and discharging the slug flow into the plurality of branched flow paths according to the fluid type; Using A continuous separation method for separating and discharging a slug flow consisting of a plurality of fluid types, , A flow expansion section in which the flow path width of the slug flow is expanded is provided upstream of the installation position of the sensor in the flow path. 、 For all of the plurality of fluid types, the length (Lgap) from the installation position of the sensor to the branch point / the amount of fluid detected by the sensor , after passing through the diverging section Slug length of slug flow (Lslug)≦0.5 、 A continuous separation method. [8] A continuous separation method according to [7], in which a narrowing section is provided from the end position of the widening section to the branching point of the flow path, in which the width of the flow path for the slug flow is narrower than the width of the flow path before the widening section. [Effects of the Invention]

[0018] According to the present invention, by extending the length of the slug flow passing through the sensor, the separation rate of the slug flow can be improved without incorporating time correction for valve operation due to the distance from the sensor to the branch point, and it is possible to provide a continuous separation device and a continuous separation method that improves the separation rate using a simple and versatile technique. [Brief explanation of the drawings]

[0019] [Figure 1] Diagram showing the flow state of slug flow [Figure 2] A diagram showing the outline of a continuous separation device that detects the fluid type using a sensor installed in the flow path and switches the flow destination between outlet A and outlet B, enabling the separation of two-phase slug flows. [Figure 3] This figure explains how the separation rate of the two-phase slug flow deteriorates in the device shown in Figure 2 because a separate fluid is discharged to the outlet in the amount corresponding to the flow path volume Lgap between the sensor position and the branch point of the flow path. [Figure 4] FIG. 1 is a schematic diagram illustrating an example of a first embodiment of the present invention. [Figure 5] FIG. 1 is a schematic diagram illustrating an example of a second embodiment of the present invention. [Figure 6] FIG. 10 is a schematic diagram showing an example of a second embodiment of the present invention in which the configuration of the first embodiment is used in combination. [Figure 7] Graph showing the results of Examples and Comparative Examples DETAILED DESCRIPTION OF THE INVENTION

[0020] The present invention will be described below based on an embodiment thereof, but the present invention is not limited to this embodiment. In this specification, the use of "to" to indicate a range of values ​​means that the values ​​before and after it are included as the lower and upper limits.

[0021] First, a conventional continuous separation device and method will be described with reference to the above-mentioned FIGS. 2 and 3 when the slug flow is composed of two phases, fluid A and fluid B. As shown in the figure, the flow path through which the two-phase slug flow flows is connected to one of the three openings of the three-way flow path, and one of the remaining two openings is connected to a flow path with a two-way valve (side A) for discharging fluid A, and the other is connected to a flow path with a two-way valve (side B) for discharging fluid B. Here, the two-way valve (side A) and the two-way valve (side B) are assumed to be electromagnetic valves, but they can also be other types of valves such as air-operated valves as long as they have the function of opening and closing. When de-energized, one of the two-way valves (side A) and two-way valve (side B) is in an open state (normally open), and the other is in a closed state (normally closed). Naturally, when energized, the open valve becomes closed, and the closed valve becomes open.

[0022] A sensor for detecting the fluid type is placed inside or outside the flow path through which the two-phase slug flow passes. Here, a light-transmitting photoelectric sensor is assumed, but sensors based on other principles, such as electrical conductivity detection, can also be used as long as they can detect differences in signal strength depending on the fluid type. Fluids A and B are distinguished by binarizing the signal strength output from the photoelectric sensor using a threshold value. The wiring of the device is configured so that when fluid A is identified based on the binary external output from the photoelectric sensor, the two-way valve (side A) is opened and the two-way valve (side B) is closed. Conversely, when fluid B is identified, the two-way valve (side A) is closed and the two-way valve (side B) is opened.

[0023] As mentioned above, the moment the sensor detects the interface of the two-phase slug flow, all of the two-way valves switch simultaneously. However, this causes another fluid to enter the outlet and be discharged in an amount equal to the volume of the flow path from the sensor installation position to the branching point of the three-way flow path, resulting in a deterioration in the separation rate of the two-phase slug flow. Here, the slug length of the slug flow detected by the sensor is defined as "L slug " and the length from the installation position of the sensor to the branch point is "L gap ", the theoretical separation rate (%) is expressed by the following formula:

[0024]

number

[0025] A first embodiment of the present invention comprises: Slug length of slug flow ( Lslug ) As a means for increasing the flow rate, a contraction section is provided in which the width of the flow path for the slug flow is reduced. That is, in the first embodiment of the present invention, the installation position of the sensor From the upstream side At the branch point of the three-way flow path or at the installation position of the sensor Place The length of the slug flow is increased by providing a narrowed flow constriction section in which the width of the slug flow passage is narrowed from the installation position of the sensor to the branch point of the three-way flow passage, and the length (Lgap) from the installation position of the sensor to the branch point / the length detected by the sensor is The flow passes through the contracted portion. The slug length (Lslug) of the slug flow is set to 0.5 or less.

[0026] FIG. 4 is a schematic diagram showing an example of the first embodiment of the present invention, in which the flow contraction section is provided from the upstream side of the installation position of the sensor to the branch point of the three-way flow path. The flow channel width (flow channel inner diameter) of the flow contraction section is narrowed to, for example, 1 / 2, 1 / 4, or 1 / 8 of the width of the flow channel through which the slug flow is sent, Passing through the contraction section By increasing the slug length (Lslug) of the slug flow by 4 times, 16 times, or 64 times, etc., it is possible to make Lgap / Lslug≦0.5, preferably Lgap / Lslug≦0.1, and more preferably Lgap / Lslug≦0.01. The position of the contraction portion is not limited to that shown in FIG. 4, but may be incorporated from the installation position of the sensor to the branch point.

[0027] In a second embodiment of the present invention, a diverging section is provided in which the width of the flow path for the slug flow is enlarged, with the intention of generating a slug flow with a larger slug volume by combining the slug flows. That is, in the second embodiment of the present invention, a flow expansion section in which the flow path width of the slug flow is expanded is provided upstream of the installation position of the sensor, and the length (Lgap) from the installation position of the sensor to the branch point / the length detected by the sensor is calculated for all of the plurality of fluid types. After passing through the diverging section The slug length (Lslug) of the slug flow is ≦0.5.

[0028] FIG. 5 is a schematic diagram showing an example of the second embodiment of the present invention. The flow expansion section is incorporated upstream of the sensor installation position, and the flow path width of the flow expansion section is adjusted to gap / L slug Preferably, L is set to ≦0.5. gap / L slug More preferably, L gap / L slug Make sure that it is ≦0.01.

[0029] In the present invention, the contracting structure of the first embodiment may be combined with the diverging structure of the second embodiment. Even if a sufficient separation rate cannot be obtained with the contracting structure alone, a sufficient separation rate can be achieved by combining it with the diverging structure. FIG. 6 is a schematic diagram showing an example of this. In the second embodiment, a constriction section is provided from the end position of the expansion section to the branch point of the slug flow, in which the flow path width of the slug flow is narrower than the flow path width before the expansion.

[0030] In any embodiment, when a light-transmitting photoelectric sensor is used to detect the fluid type as in the above example, the material of the flow path in which the sensor is placed must be transparent to the light used.

[0031] The continuous liquid-liquid separation device and continuous liquid-liquid separation method of this embodiment are used as a means for separating and purifying products after chemical substances are produced by mixing, synthesis, reaction, extraction, etc. in a flow process using a slug flow. The slug flow and flow paths in the embodiment of the present invention will be described in detail below.

[0032] [Slag flow] In an embodiment of the present invention, a slug of multiple fluid species is a liquid that consists of at least two components that are completely immiscible with each other and separate into two or more phases. In an embodiment of the present invention, when the slug flow is a two-phase liquid consisting of two liquid species, it may be a liquid-liquid mixture of an aqueous phase and an oil phase, or a gas-liquid mixture of a liquid phase and a gas phase. The liquid phase may be a liquefied gas, such as liquefied carbon dioxide. It may also be any one of a supercritical fluid, a subcritical fluid, and a fluid in which ionic liquids are immiscible. If one or more of the fluid species is a gas at room temperature and pressure, it is preferable to have temperature and pressure control functions to maintain the fluid in a liquid state in the flow path through which the fluid passes. A preferred gas capable of generating a slug flow is carbon dioxide, maintained at a temperature of 31°C or less and below its equilibrium temperature so as to maintain the liquid phase in the extraction field.

[0033] In an embodiment of the present invention, when the slug stream is a two-phase liquid, examples thereof include water / pentane, water / hexane, water / heptane, water / octane, water / nonane, water / decane, water / cyclohexane, water / decane, water / decalin, 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 / diethyl 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.

[0034] Other examples include two-phase liquids of three or more components obtained by dissolving an inorganic salt or an organic compound in a two-phase liquid consisting of the above two components, and also examples of liquid mixtures such as water / acetone, water / formaldehyde, water / tetrahydrofuran, water / N,N'-dimethylformamide, water / dimethyl sulfoxide, water / ethyl alcohol, water / methanol, water / ethylene carbonate, and water / acetic acid, in which an inorganic salt or an organic compound is dissolved and the mixture is separated into two phases.

[0035] [Slug flow generation method] In embodiments of the present invention, the method for generating a slug flow is not particularly limited. Conventionally, a slug flow is generated by pumping multiple fluids of different phases using multiple pumps, which are corresponding fluid transfer means. Specifically, in the case of a two-phase fluid, immiscible liquids are pumped from their respective liquid holders by separate pumps and then merged in a T-shaped channel or the like to generate a slug flow. In the case of a three-phase fluid, a slug flow can also be generated by merging fluids sent by three or more pumps. The pump is preferably a double-plunger pump or a triple-plunger pump, which has two or more plungers in a single pump. These pumps have multiple heads, and the reciprocating motion of each plunger alternately pumps the fluids in each head, canceling out flow rate fluctuations from each head and suppressing pulsation. Another method for generating a slug flow more stably is to alternately flow two incompatible liquids by switching a valve installed in the flow path to generate a slug flow, which extracts and separates the extractant. This method makes it possible to alternately send the liquids with good reproducibility under conditions dominated by laminar flow. Furthermore, a method for controlling the slug length by controlling the operation of two piezoelectric micropumps in conjunction with each other by changing the voltage and frequency is also known. In addition, there are cases where a change in temperature or other factors triggers phase separation within the flow channel, resulting in the generation of a slug flow.

[0036] [Flow path] In an embodiment of the present invention, the material of the flow path through which the slug flow is transported 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. Examples of hydrophilic materials include hydrophilized polytetrafluoroethylene, acrylic resins such as polymethacrylate, polyamide, polyimide, polyester, polycarbonate, polyether, polyurethane, ceramics, and metal. Generally, in two-phase flow, the fluid species with a higher affinity for the flow channel becomes the continuous phase. In this case, when the other fluid species that has become the dispersed phase is recovered, there is a high possibility that the continuous phase fluid species that form a liquid film on the flow channel surface will be entrained. Therefore, it is preferable to select a material for the flow channel at the branching point of the two-phase fluid that has a high affinity for the fluid species that is desired to be separated at a high efficiency. [Example]

[0037] The present invention will be specifically described below based on examples and comparative examples. However, the examples are intended to illustrate preferred examples of the present invention, and the present invention is not limited to the examples in any way.

[0038] (Comparative Example 1) The two-phase fluid introduced into the two-phase separation device was pumped at 1 mL / min using two double plunger pumps (Nihon Seimitsu Kagaku, NP-KX-220P): cyclohexane as liquid A and ethanol / water (1:1 (v / v)) as liquid B. The two fluids collided face-to-face using a 2 mm inner diameter stainless steel T-joint, and circulated as slugs in a 2 mm inner diameter, 30 cm long quartz tube. The slug length was approximately 4 mm for both liquid A and B. The quartz tube was connected to a 2 mm inner diameter stainless steel Tee joint, which served as the branching point for the two-phase fluid. One end of the Tee joint was connected to a PFA tube incorporating a two-way valve (SMC, LVM10R3, normally closed type), and the other end was connected to a PFA tube incorporating a two-way valve (SMC, LVM10R4, normally open type). The photoelectric sensor was a combination of a fiber amplifier (Keyence, FS-N11N) and a through-beam fiber unit (Keyence, FU58), and was fixed to the outside of the flow path piping using a jig. The aforementioned Sensor Installation From the position to the branch point where the two-phase liquid separates length The fiber unit was positioned so that the gap (Lgap) was 20 mm (see FIG. 2). The liquid discharged from the outlet of the flow channel was sampled, and the volumes of liquids A and B were measured using measuring flasks. From the measured values ​​obtained, Separation rate of the outlet of the flow path for discharging fluid A into which a two-way valve (side A) is incorporated (hereinafter referred to as "liquid A separation rate") [%] = (liquid A volume) / [(liquid A volume) + (liquid B volume)] × 100 [%], Separation rate of the outlet of the flow path for discharging fluid B incorporating a two-way valve (side B) (hereinafter referred to as "liquid B separation rate") [%] = (volume of liquid B) / [(volume of liquid A) + (volume of liquid B)] × 100 [%], The separation rate of liquid A was 17.2% and that of liquid B was 17.6%.

[0039] Example 1 A contraction section consisting of a PTFE tube with an inner diameter of 0.25 mm and a length of 5 cm was installed downstream of the quartz tube with an inner diameter of 2 mm and a length of 30 cm via a SUS joint, and connected to a PEEK Tee joint with an inner diameter of 0.5 mm instead of the SUS Tee joint with an inner diameter of 2 mm, which served as a branch point for the two-phase fluid. Other than these, the same procedures were followed as in Comparative Example 1, and this was designated Example 1 (see Figure 4). In Example 1, the separation rate of liquid A was 94.32%, and the separation rate of liquid B was 95.1%.

[0040] (Comparative Example 2) This was designated Comparative Example 2, and was conducted in the same manner as in Example 1, except that the contracted flow section was replaced with a glass tube having an inner diameter of 1 mm and a length of 5 cm. In Comparative Example 2, the separation rate of liquid A was 19.4%, and the separation rate of liquid B was 29.6%.

[0041] Example 2 Example 2 was the same as Comparative Example 1, except that a glass tube with an inner diameter of 4 mm and a length of 10 cm was incorporated into the quartz tube with an inner diameter of 2 mm and a length of 30 cm upstream of the sensor position via a stainless steel joint. This was designated Example 2 (see Figure 5). In Example 2, the separation rate of liquid A was 54.2%, and the separation rate of liquid B was 54.0%.

[0042] Example 3 Example 3 was the same as Comparative Example 2, except that a glass tube with an inner diameter of 4 mm and a length of 10 cm, which was the flow-expanding section of Example 2, was inserted between the quartz tube with an inner diameter of 2 mm and a length of 30 cm in Comparative Example 2 and the glass tube with an inner diameter of 1 mm and a length of 5 cm (flow-constricting section) via a stainless steel joint. This was designated Example 3 (see Figure 6). In Example 3, the separation rate of liquid A was 88.1%, and the separation rate of liquid B was 91.9%.

[0043] Example 4 Example 4 was the same as Example 2, except that the glass tube with an inner diameter of 1 mm and a length of 5 cm in the contraction section in Example 3 was replaced with a PTFE tube with an inner diameter of 0.25 mm and a length of 5 cm in the contraction section in Example 1. In Example 4, the separation rate of liquid A was 98.5%, and the separation rate of liquid B was approximately 100%.

[0044] The results are shown in the table below and in FIG.

[0045] [Table 1]

[0046] As shown in Table 1 and FIG. 7, Comparative Example 1 Solution A and Solution B The slug length (Lslug) was approximately 4 mm, which did not satisfy the condition of Lslug > Lgap (= 20 mm). The separation rates of liquid A and liquid B were 17.2% and 17.8%, respectively. In contrast, Example 1, which is a flow contraction section added to Comparative Example 1, had a liquid A separation rate of 94.3% and a liquid B separation rate of 95.1%, which were significantly improved compared to Comparative Example 1. The slug length ( Lslug ) is 256 mm, so Lgap / Lslug = 0.078, which fully satisfies the condition Lslug >> Lgap.

[0047] In Example 2, a diverging section was added to Comparative Example 1. The slag volume increased by approximately 10 times due to the coalescence of the slags in the diverging section. The slug length ( Lslug ) As a result, the separation rate of liquid A was 54.2% and the separation rate of liquid B was 54.0%, which was an improvement over Comparative Example 1.

[0048] In Comparative Example 2, the effect of the contraction flow caused by the glass tube with an inner diameter of 1 mm , the slug length ( Lslug ) Although the length of the liquid increased, it was only about 16 mm, which did not satisfy the condition of Lslug>Lgap (=20 mm). As a result, the separation rate of liquid A was 19.4% and that of liquid B was 29.6%, which were low. In contrast, Example 3 is a combination of Comparative Example 2 and the effect of the diverging section of Example 2. At this time, the slags coalesce in the diverging section, increasing the slag volume by approximately 10 times. The slug length ( Lslug ) The gap was approximately 165 mm, resulting in an Lgap / Lslug ratio of 0.12. As a result, the separation rate of liquid A was 88.1%, and the separation rate of liquid B was 91.9%, which was a significant improvement over Comparative Example 2. This can also be attributed to the fact that the condition Lslug >> Lgap (20 mm) was met.

[0049] The fourth embodiment is a configuration in which the contraction effect of the third embodiment is strengthened.3 So , the slug length ( Lslug ) The gap length was increased from approximately 165 mm to approximately 2634 mm, resulting in Lgap / Lslug = 0.0078, further satisfying the condition Lslug >> Lgap (20 mm). As a result, the separation rate was further improved compared to Example 3, with the separation rate of liquid A reaching 98.5% and the separation rate of liquid B reaching approximately 100%. In addition, Table 4.2 of the above-mentioned Non-Patent Document 5 describes that the maximum separation rate of two liquids for different organic phases was 98.4% for the liquid A side separation rate and 94.2% for the liquid B side separation rate. Although the types of liquids used were different from those described in Non-Patent Document 5, fruit It can be said that Example 4 showed a separation rate equal to or higher than that of non-literature Reference 5. [Industrial Applicability]

[0050] According to the present invention, it is possible to increase the separation rate of a slug flow using a continuous separation device with a simple configuration. Therefore, by connecting the continuous separation device of the present invention downstream of a flow process using a slug flow, it is possible to continuously carry out processes from reaction to separation and purification for chemical substances including a wide variety of functional chemicals.

Claims

1. A flow path into which a slug flow consisting of multiple fluid types flows; branching means for branching the flow path into a plurality of flow paths provided for each of the fluid types; a sensor provided in the flow path upstream of the branching means for detecting a plurality of fluid types in the slug flow; a means for switching the plurality of flow paths in response to the fluid type detected by the sensor, thereby separating and discharging the slug flow into the plurality of branched flow paths according to the fluid type; A continuous separation apparatus for separating and discharging a slug flow consisting of a plurality of fluid types into individual fluid types, comprising: a flow contraction section in which the flow path width of the slug flow is reduced is provided from the upstream side of the installation position of the sensor in the flow path to a branch point of the flow path, or from the installation position of the sensor in the flow path to a branch point of the flow path, For all of the plurality of fluid types, the length (L gap) from the installation position of the sensor to the branch point / the slug length (L slug ) of the slug flow passing through the contraction section detected by the sensor is ≦0.5; A continuous separation device.

2. 2. The continuous separation device according to claim 1, wherein the flow contraction section is provided from a side upstream of the position where the sensor is installed in the flow path to a branch point of the flow path.

3. A flow path into which a slug flow consisting of a plurality of fluid types flows; branching means for branching the flow path into a plurality of flow paths provided for each fluid type; a sensor provided in the flow path upstream of the branching means for detecting a plurality of fluid types in the slug flow; a means for switching the plurality of flow paths in response to the fluid type detected by the sensor, thereby separating and discharging the slug flow into the plurality of branched flow paths according to the fluid type; A continuous separation apparatus for separating and discharging a slug flow consisting of a plurality of fluid types into individual fluid types, comprising: a widening section in which the flow path width of the slug flow is widened is provided upstream of the installation position of the sensor in the flow path, For all of the plurality of fluid types, the length (L gap) from the installation position of the sensor to the branch point / the slug length (L slug ) of the slug flow detected by the sensor after passing through the diverging section is ≦0.5; A continuous separation device.

4. 4. The continuous separation apparatus according to claim 3, further comprising a flow contraction section provided between the terminal end of the flow expansion section and the branch point of the flow channel, the flow channel width of the slug flow being narrower than the flow channel width before the flow expansion.

5. A flow path into which a slug flow consisting of a plurality of fluid types flows; branching means for branching the flow path into a plurality of flow paths provided for each of the fluid types; a sensor provided in the flow path upstream of the branching means for detecting a plurality of fluid types in the slug flow; a means for switching the plurality of flow paths in response to the fluid type detected by the sensor, thereby separating and discharging the slug flow into the plurality of branched flow paths according to the fluid type; A continuous separation method for separating and discharging a slug flow consisting of a plurality of fluid types, comprising: a flow contraction section in which the flow path width of the slug flow is reduced is provided from the upstream side of the installation position of the sensor in the flow path to a branch point of the flow path, or from the installation position of the sensor in the flow path to a branch point of the flow path, For all of the plurality of fluid types, the length (L gap) from the installation position of the sensor to the branch point / the slug length (L slug ) of the slug flow passing through the contraction section detected by the sensor is ≦0.5; A continuous separation method.

6. 6. The continuous separation method according to claim 5, wherein the flow contraction section is provided from a side upstream of the position where the sensor is installed in the flow channel to a branch point of the flow channel.

7. A flow path into which a slug flow consisting of a plurality of fluid types flows; branching means for branching the flow path into a plurality of flow paths provided for each of the fluid types; a sensor provided in the flow path upstream of the branching means for detecting a plurality of fluid types in the slug flow; a means for switching the plurality of flow paths in response to the fluid type detected by the sensor, thereby separating and discharging the slug flow into the plurality of branched flow paths according to the fluid type; A continuous separation method for separating and discharging a slug flow consisting of a plurality of fluid types, comprising: a widening section in which the flow path width of the slug flow is widened is provided upstream of the installation position of the sensor in the flow path, For all of the plurality of fluid types, the length (L gap) from the installation position of the sensor to the branch point / the slug length (L slug ) of the slug flow detected by the sensor after passing through the diverging section is ≦0.5; A continuous separation method.

8. 8. The continuous separation method according to claim 7, further comprising a flow contraction section provided between the terminal position of the flow expansion section and the branch point of the flow channel, the flow channel width of the slug flow being narrower than the flow channel width before the flow expansion.

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