Slag flow generation device, chemical substance treatment device equipped with the slag flow generation device, slag flow generation method, and chemical substance treatment method using the slag flow

Abstract

To provide a slag flow generator suitable for reactions between various phases, and a separation operation, by controlling a slag length without inviting instability of a process due to variation of a flow rate or stoppage of liquid delivery, and by stably controlling a flow rate and a slag length respectively, independently in a wide range.SOLUTION: A device for generating a slug flow of a plurality of fluids, comprises: a fluid holding portion for holding each of the plurality of fluids; a pump for constantly pumping each of the plurality of fluids; the plurality of fluid holding portions and the pump; and a channel respectively connecting the pump and a fluid confluence portion, a slug flow generation channel is provided downstream of the fluid confluence portion, a valve is installed in each of the channels between the fluid confluence portion and the pump. and the valve is controlled such that one kind of fluid is always pressure-fed to the fluid confluence portion and other fluids are discharged to the discharge channel.SELECTED DRAWING: Figure 3

Description

Technical Field

[0001] The present invention relates to a slag flow generation device, a chemical substance treatment device including the slag flow generation device, a slag flow generation method, and a chemical substance treatment method using a slag flow. Here, the treatment refers to a reaction or separation (extraction, absorption, crystallization, etc.) or reaction separation related to a chemical substance.

Background Art

[0002] In conventional chemical reaction processes, improvement in efficiency by scale-up has been demanded. Furthermore, in recent years, demands for reduction of environmental load, resource saving, and energy saving have also been added. In the production of high-value-added products such as pharmaceuticals, functional chemicals, or fine chemicals, for which future growth is expected, a batch production method suitable for small-scale production is the mainstream. However, since it has a large energy loss and discharges a large amount of co-products, in recent years, there has been a movement to attempt to reduce the loss between each batch treatment step by a flow production method (hereinafter referred to as "flow process") that performs continuous operations from reaction to separation and purification. In addition, there is a research and development movement to modularize each unit operation incorporated in the flow process so that it can cope with the production of various functional chemicals by recombining reaction modules and separation and purification modules as necessary (Non-Patent Document 1).

[0003] In the flow process, operations such as temperature adjustment, pressure adjustment, mixing, reaction, extraction, separation and purification are performed while the fluid flows through a pipe or a device connected in the middle of the pipe. As requirements for each unit operation module, it is required to be compact and have high-speed processing. Particularly in the flow process, an important object is a process involving the flow of a multiphase fluid in which some parts are mutually soluble or completely insoluble (examples include liquid-liquid reaction, gas-liquid reaction, liquid-liquid extraction, gas-liquid extraction, gas-liquid separation, liquid-liquid separation). Usually, in a process involving a multiphase fluid, when aiming for compactification and high-speed processing of the process, it is important to reduce the interfacial mass transfer resistance.

[0004] In a multiphase fluid process, compacting the apparatus can also be mentioned in order to actively utilize the flow state advantageous for the target unit operation. In a flow process typically aimed at small-scale production, compared to the space handled in a batch process, the scale is small and the flow rate is low, so the Reynolds number is low and laminar flow is dominant. Even in such a laminar flow region, slug flow (also called segmented flow or Taylor flow, the flow states shown in Figs. 1(a) and (b)), in which fluids of different phases in a separated state flow alternately, promotes interfacial renewal due to the internal circulation flow in the slug derived from the shear from the wall surface, thereby reducing the mass transfer resistance. Also, since large fluid masses can be formed, there is an advantage that the time required for phase separation is relatively short (Patent Document 1). Fig. 1 shows typical flow states of multiphase flow. For example, in the flow states shown in Figs. 1(c) to (f), the effect of reducing the mass transfer resistance cannot be obtained, whereas in the slug flow shown in (a) and (b), the effect of reducing the mass transfer resistance by the internal circulation flow is exhibited.

[0005] Conventionally, as shown in Figs. 2(a) and (b), slug flow has been generated by continuously pumping a plurality of fluids of different phases to a fluid confluence part using a plurality of pumps corresponding to each fluid (for example, Non-Patent Document 2: Figure 2, 2.1. Experimental Setup). This method can be realized by an apparatus with a simple configuration that only connects pumps for pumping each of the plurality of fluids and a fluid confluence part. Also, since slug flow is generated spontaneously, the slug length cannot be controlled, but the liquid-liquid ratio can be changed during operation by changing the flow rate ratio of each pump.

[0006] Also, Non-Patent Document 3 describes that by periodically driving a three-way electromagnetic valve provided at the fluid confluence part of two liquids while keeping two pumps in a constant pumping state, alternating liquid feeding is performed at the fluid confluence part to generate slug flow. By using such an apparatus, it is possible to perform alternating flow feeding in a situation dominated by laminar flow. Also, the slug length can be controlled by the switching frequency of the valve.

[0007] Non-Patent Document 4 describes generating a slug flow by continuously flowing a continuous phase (carrier oil) at all times and controlling the intermittent introduction of the dispersed phase 1 and the dispersed phase 2 by switching a valve and starting and stopping a pump. By using this device, the flow rate and the length of each slug can be controlled during the pump operation by controlling the valve and the pump.

[0008] Non-Patent Document 5 describes a device for generating a slug flow by operating two piezoelectric micropumps in antiphase by electronic control of voltage and frequency. By using this device, the flow rate and the slug length can be controlled by controlling the voltage and the frequency during the pump operation. Also, since there is no state in which the fluid is blocked in principle, no pressurized state occurs in the pump or the flow path.

Prior Art Documents

Patent Documents

[0009]

Patent Document 1

Non-Patent Documents

[0010]

Non-Patent Document 1

Non-Patent Document 2

Non-Patent Document 3

Non-Patent Document 4

Non-Patent Document 5

Summary of the Invention

Problems to be Solved by the Invention

[0011] In the slug flow, the promoting effect of mass transfer has an optimum point for the flow velocity and slug length according to various fluid physical properties, and a technology is required that can independently and easily control the flow velocity and slug length within a range that can cover the optimum points different depending on the fluid physical properties. Also, it is preferable that the slug length can be controlled by a pump in a constant pumping state without using a pump that stops and starts, which causes flow rate fluctuations that are a concern for process instability. However, a slug flow generation device having both of these two characteristics has not been developed yet. In the device of Non-Patent Document 2, since the generation of the slag flow is random, the slag length is defined by the flow rate of each pump, the shape and size of the fluid confluence part, and the fluid physical properties, and there is almost no degree of freedom. In the device described in Non-Patent Document 3, although the slag length can be controlled, since the pump is constantly in the pressure-feeding state, a state occurs where the fluid is blocked, and there is a concern that the pump and the flow path may be in an overpressure state, causing a load and resulting in damage or a fluctuation in the flow rate. In the device described in Non-Patent Document 4, since the pump is stopped when the valve is closed, there is no concern about damage to the device due to pressurization. By synchronizing a plurality of syringe pumps, control of the slag length and flow velocity of each phase in the three-phase slag flow was achieved. However, since it is a liquid feeding control by appropriately starting and stopping the liquid-feeding pump, there is a concern about the instability of the process due to the flow rate fluctuation. In Non-Patent Document 5, there is no state where the fluid is blocked, and no pressurized state occurs in the pump or the flow path. Also, due to the structure of the piezo micropump (hereinafter referred to as "PMP"), by changing the amplitude width of the diaphragm by voltage and changing the frequency of the voltage change, it is possible to independently control the amount of fluid fed by one reciprocation of the diaphragm and the average flow rate, and as a result, the slag length and the flow velocity can be independently controlled. However, since the discharge pressure of the PMP is small, it is difficult to accurately control the liquid-feeding characteristics. Also, when changing the ratio of the slag lengths of the two fluids, it is necessary to replace that part or the PMP itself in order to change the amount of fluid fed by one reciprocation of the diaphragm, which cannot be said to be easy control.

[0012] In view of the above problems, an object of the present invention is to provide a slag flow generation device and a slag flow generation method suitable for reaction and separation operations in various phases by controlling the slag length without causing process instability due to fluctuations in the flow rate or stoppage of liquid feeding, and by independently and stably controlling the flow velocity and the slag length within a wide range.

Means for Solving the Problems

[0013] In order to solve the above problems, the present invention employs the following means. [1] An apparatus for generating slug flows of a plurality of fluids, comprising a fluid holding section for holding each of the plurality of fluids, a pump for constantly pumping each of the plurality of fluids, flow paths connecting the plurality of fluid holding sections, the pump, and the pump and the fluid confluence section respectively, and a slug flow generating flow path provided downstream of the fluid confluence section. Valves are installed in the flow paths between the fluid confluence section and the pump respectively, and by the valves, one type of fluid is constantly pumped to the fluid confluence section, and the other fluids are controlled to be discharged to the discharge flow path. A slug flow generating apparatus. [2] The slug flow generating apparatus according to [1], wherein the discharge flow path is connected to the original fluid holding section, and the discharged fluid is recovered by the original fluid holding section. [3] The slug flow generating apparatus according to [1], wherein the discharge flow path is connected to a fluid confluence section different from the fluid confluence section, and the discharged fluid is pumped to the different fluid confluence section, whereby another slug flow generating flow path is provided in parallel. [4] The slug flow generating apparatus according to any one of [1] to [3], wherein reaction or separation is performed in the slug flow generating flow path. [5] The slug flow generating apparatus according to any one of [1] to [4], wherein at least one of the pumps has a temperature regulating mechanism for maintaining the liquid state of the fluid flowing through the head. [6] The slug flow generating apparatus according to [5], wherein one phase of the slug flow is liquefied carbon dioxide and the other phase is a liquid. [7] A chemical substance treatment apparatus provided with the slug flow generating apparatus according to any one of [1] to [6]. [8] The chemical substance treatment apparatus according to [7], having a liquid-liquid separation mechanism downstream of the slug flow generating apparatus. [9] The chemical substance treatment apparatus according to [8], having a gas-liquid separation mechanism between the slug flow generating apparatus and the liquid-liquid separation mechanism.

[10] The chemical substance treatment apparatus according to [9], wherein a gas discharge pipe provided with a pressure control mechanism is connected to the upper part of the gas-liquid separation mechanism, and a liquid discharge pipe connected to the liquid-liquid separation mechanism is connected to the lower part.

[11] A method of constantly pumping a plurality of fluids through respective flow paths from respective fluid holding portions to a fluid confluence portion by pumps, and generating a slug flow in a flow path downstream of the fluid confluence portion, comprising: said Controlling a valve installed between the fluid confluence portion and the pump to constantly pump one type of fluid to the fluid confluence portion and A slug flow generation method for discharging other fluids to a discharge flow path.

[12] The slug flow generation method according to

[11] , wherein the fluid discharged to the discharge flow path is recovered to the original fluid holding portion.

[13] The slug flow generation method according to

[11] , wherein the fluid discharged to the discharge flow path is pumped to a fluid confluence portion different from the fluid confluence portion, and slug flow is generated in parallel in another slug flow generation flow path.

[14] The slug flow generation method according to any one of

[11] to

[13] , wherein reaction or separation is performed in the flow path for generating the slug flow.

[15] The slug flow generation method according to any one of

[11] to

[14] , wherein at least one of the pumps performs temperature control to maintain the liquid state of the fluid flowing through the head.

[16] The slug flow generation method according to

[15] , wherein one phase of the slug flow is liquefied carbon dioxide and the other phase is a liquid.

[17] A method for treating a chemical substance including the slug flow generation method according to any one of

[11] to

[16] .

[18] The method for treating a chemical substance according to any one of

[11] to

[17] , including liquid-liquid separation of the generated slug flow.

[19] The method for treating a chemical substance according to

[18] , including liquid-liquid separation after gas-liquid separation of the generated slug flow.

[20] The method for treating a chemical substance according to

[19] , including discharging the gas-liquid separated gas from the upper part while controlling the pressure and discharging the liquid-liquid separated liquid from the lower part.

Advantages of the Invention

[0014] According to the present invention, the flow velocity and the slug length can be independently and easily controlled. Therefore, a slug flow controlled to an optimal flow velocity and slug length enables high-speed processing while compactifying a chemical substance manufacturing apparatus. In addition, since the pump can always be in a pressure - feeding state, it is difficult to inhibit the stability of the process.

Brief Description of the Drawings

[0015]

Figure 1

Figure 2

Figure 3

Figure 4

Figure 5

Figure 6

Figure 7

Figure 8

Figure 9

Modes for Carrying Out the Invention

[0016] The present invention relates to an apparatus and a method for generating a slag flow in which each phase is sequentially introduced, and an apparatus and a method for treating a chemical substance provided with the above-described slag generation apparatus. While continuously pumping each fluid forming each phase by continuously operating pumps for pumping each fluid, the switching valve incorporated upstream of the fluid confluence portion of each flow path is operated so that only one fluid is always pumped to the fluid confluence portion, and the other than the one fluid is discharged to the discharge flow path. By having a piping configuration, it is characterized in that the flow velocity and the slag length of each phase are controlled. Hereinafter, the present invention will be described based on embodiments of the present invention (hereinafter referred to as "the present embodiment"), but the present invention is not limited to the present embodiment.

[0017] [Pumping method] The simplest configuration of the slag flow generation device is, as shown in FIGS. 2(a) and 2(b), to prepare pumps for pumping one fluid in the number corresponding to the number of fluids to be pumped, and connect the discharge ports of each pump to the same fluid confluence portion. In this way, in the method of introducing all fluids into the fluid confluence portion simultaneously (hereinafter referred to as "simultaneous pumping method"), a slag flow is generated in a specific flow rate range, and the slag length is inevitably determined according to the physical properties and the flow path (Non-Patent Document 2 Fig. 2). On the other hand, the alternate pumping method in which only one fluid is always controlled to flow through the fluid confluence portion (hereinafter referred to as "alternate pumping method") is a pumping method in which a slag flow is more likely to occur, and the slag length can be controlled by controlling the pumping time to the fluid confluence portion. The alternate pumping method includes a method of realizing alternate pumping to the fluid confluence portion by intermittently operating the pump to intermittently pump the fluid (Patent Document 1: Claim 9, Non-Patent Document 4: Fig. 1), and continuously operating the pump to continuously pump the fluid while operating the switching valve installed in the fluid confluence portion. There is a method of realizing alternate pumping to the fluid confluence portion (Non-Patent Document 3).

[0018] The pressure feeding method related to the slag generation mechanism of this embodiment is an alternating pressure feeding method in which each pump is continuously operated to continuously feed fluid, a valve is provided on the upstream side of the fluid confluence section, and a fluid always flows through the fluid confluence section. It is greatly different from the conventional alternating pressure feeding method in that the fluid is switched by the valve provided in the fluid confluence section. FIGS. 3(a) to (e) are configuration examples of the apparatus. FIGS. 3(a) and (b) are configuration examples in which a slug flow of a two-phase or three-phase fluid is generated using a three-way valve, and the fluid discharged into the discharge flow path is recovered to the original fluid holding section. FIG. 3(c) is a configuration example in which each three-way valve in FIG. 3(a) is replaced with two two-way valves. FIG. 3(d) is a configuration example when the two-phase fluid is liquid and gas. The flow of the liquid is the same as that in FIG. 3(c), but for the gas, a part of it flows from the pressurized gas holding section to the fluid confluence section using a flow controller, and the other part is discharged from the discharge flow path. FIG. 3(e) is a configuration example in which the slug flow generation flow path can be paralleled by connecting the discharge flow path to another fluid confluence section. In any of the configuration examples, as described in FIG. 6 to be described later, it is preferable to provide a back pressure valve in the discharge flow path because the switching accuracy of the valve can be adjusted.

[0019] FIGS. 4(a) and (b) show patterns in which a plurality of fluids merge at the fluid confluence section. However, the collision order, collision angles θ and θ' are not defined in FIG. 4.

[0020] [Pump] The pump referred to here is a fluid pressure feeding device in a broad sense. For example, it includes a plunger pump, a diaphragm pump, and a syringe pump. A positive pressure fluid stock tank for the purpose of feeding fluid regardless of gas or liquid and a flow controller connected thereto (mainly assumed for gas feeding. See FIG. 3(d)) are also defined as pumps in the same way. The driving method of the pump is preferably mechanical to obtain a high pumping force so that precise liquid delivery can be performed, and it is preferably by a camshaft that eccentrically rotates in conjunction with the rotation of the motor. Typically, a plunger pump and a diaphragm pump can be mentioned. In particular, a multi-plunger pump having a plurality of heads (a housing that defines a space sandwiched between a suction-side valve and a discharge-side valve that operate in a check manner) is preferable to prevent pulsatile flow.

[0021] Figure 5 shows a comparison of the liquid delivery accuracy between the plunger pump (NP-KX-220P, Nippon Precision Science Co., Ltd., maximum discharge pressure 10 MPa) used in the present embodiment described later and the piezo micropump (PMP) (APP-20KG, Takasago Electric Industry Co., Ltd., standard discharge pressure 20 kPa) in which reciprocating motion is electrically performed by a piezoelectric element used in Comparative Example 2. An example of the former result is shown in Figure 5(a), and an example of the latter result is shown in Figure 5(b). Using the R 2 value as an index, the former is R 2 = 1.0 (>0.999), and the latter's R 2 = 0.968. From this, it can be seen that the plunger pump has higher liquid delivery accuracy than the PMP.

[0022] Generally, the liquid delivery capacity of a syringe pump is limited by the syringe volume. However, for example, if a syringe pump is provided with a mechanism having a pipe with a valve in the flow path so that the syringe reciprocates and becomes a liquid delivery mode in one direction and a suction mode in the reverse direction, this limitation is eliminated, and it can be applied to a constant pressure pumping method at all times.

[0023] [Fluid] As the plurality of fluids, since non-slurry flow is not generated between mutually compatible fluids, fluids that are not completely compatible are combined. It may be a liquid-liquid of an aqueous phase and an oil phase, or a gas-liquid of a liquid phase and a gas phase. The liquid phase may be a liquefied gas, for example, liquefied carbon dioxide. The supercritical fluid, subcritical fluid, or ionic liquid may be any one of the incompatible fluids.

[0024] When one or more of the fluids are gases at normal temperature and pressure, it is preferable that the head through which the fluid passes has a temperature control function and a pressure control function to keep the fluid in a liquid state in order for the fluid to liquefy when passing through the pump head. Preferable gases that can generate a slug flow include carbon dioxide that is at 31°C or lower and is kept below the equilibrium temperature so as to maintain a liquid phase at the extraction site.

[0025] As an example of the combination of the aqueous phase and carbon dioxide, it is assumed that the liquefied carbon dioxide is present at the pump discharge. In that case, the process is preferably at or above the critical pressure of carbon dioxide (7.4 MPa), and a backpressure valve is provided downstream of the slug flow region to control the pressure from the pump to the backpressure valve. Since carbon dioxide can replace the organic solvent only under high-pressure conditions, it is expected that the hydrophobic valuable substances in the aqueous phase will be extracted by high-pressure carbon dioxide.

[0026] [Slug Flow Generation Flow Path] In the slug flow generation flow path, reactions or separations are carried out by utilizing the promoting effect of mass transfer in the slug flow. Specifically, it includes reactions such as liquid-liquid reactions, gas-liquid reactions, solid-catalyst reactions, separations such as extraction, absorption, crystallization, etc., or reaction-separations. Although there are optimal points for the flow rate and slug length according to various fluid physical properties in the promoting effect of mass transfer, in the slug flow generation flow path of the present embodiment, the flow rate and slug length can be independently realized within a range that can cover the optimal points different according to the fluid physical properties.

[0027] [Chemical Substance Treatment Apparatus and Treatment Method] In the present embodiment, as illustrated in FIG. 6, after reactions, separations, or reaction-separations are carried out in the slug flow generation flow path, a liquid-liquid separator is arranged downstream of the slug flow generation flow path, and, if necessary, a gas-liquid separator is arranged between the slug flow generation flow path and the liquid-liquid separator, so that the phases containing chemical substances can be continuously separated and purified. When arranging the gas-liquid separator, a gas discharge pipe is connected to the upper part of the gas-liquid separator, and a liquid discharge pipe connected to the liquid-liquid separator is connected to the lower part. A backpressure valve for controlling the pressure of the slag flow generation flow path is provided in the gas discharge pipe.

Example

[0028] Hereinafter, the present invention will be specifically described based on examples and comparative examples. However, the examples show preferred examples of the present invention, and the present invention is not limited by the examples. The set value range of the equipment in the examples has nothing to do with the performance limit of the present invention.

[0029] <Example 1> In the configuration shown in Fig. 3(a), as the main component devices, two double plunger pumps (Nippon Precision Science NP-KX-220P), two three-way valves (SMC Corporation, LVM105R), and one valve control timer (Omron Corporation, H5CX) were used. A tank storing toluene as liquid A (organic phase) was connected to one pump via a suction pipe, and a tank storing water as liquid B (aqueous phase) was connected to the suction side of the other pump via another suction pipe. A three-way valve was installed in the middle of each discharge pipe on the discharge side of each pump, and the wirings of the two three-way valves were connected in reverse phase. The discharge pipe on the downstream side of the three-way valve was connected to the fluid confluence part of liquid A and liquid B composed of SUS tube with an inner diameter of 2 mm, and the two three-way valves were alternately opened to the fluid confluence part. A slag flow generation flow path composed of a glass tube with an inner diameter of 2 mm and a length of 30 cm was connected downstream of the confluence part. The flow rate set values of the two pumps were set to 1 - 20 mL / min so that the total flow rate of liquid A and liquid B corresponded to 1 - 20 mL / min. The time when the flow path of the valve is connected to the fluid confluence part is defined as the opening time, and the opening time of liquid A (organic phase) is t or , and the opening time t aq of liquid B (aqueous phase) is defined. (t or , t aq ) = (1 sec, 1 sec), (0.25 sec, 0.25 sec), (0.13 sec, 0.13 sec) in three patterns, and the three-way valve was operated. Note that t or + taq When taking one cycle, the number of cycles per second (frequency) is 0.5 Hz, 2 Hz, and 4 Hz, respectively. The length (l or +l aq )(organic phase: l or , aqueous phase: l aq ) of the slug flow obtained by combining the organic phase and the aqueous phase in the slug flow generation channel was measured. At this time, the ratio of the organic phase to the aqueous phase calculated from these set values is approximately 1:1 (the slug length ratio l or / (l or +l aq ) × 100 [%] is about 50%).

[0030] <Comparative Example 1> Comparative Example 1 was carried out with the configuration shown in Fig. 2(a). Using two of the same double plunger pumps as in Example 1, and performing the same operations as in Example 1 except that the A liquid and the B liquid were simultaneously pressure-fed at the same flow rate setting value by each pump, Comparative Example 1 was set up, and the length of the slug flow in the slug flow generation channel was measured.

[0031] <Comparative Example 2> Comparative Example 2 was carried out with the configuration described in Non-Patent Document 5. That is, by wiring two PMPs (APP-20KG, Takasago Electric Industry Co., Ltd.) to a micropump controller (MPC-200B, Takasago Electric Industry Co., Ltd.) so as to perform reverse-phase operation, a configuration enabling alternate liquid feeding to the fluid confluence section was achieved. The vibration frequency of the diaphragm built into the pump was set to 40 Hz, and the applied voltage was controlled so that the total flow rate was approximately 40 to 60 mL / min for operation, and the length of the slug flow in the slug flow generation channel was measured.

[0032] <Example 2> Using the configuration shown in Fig. 3(a), the total flow rate of the A liquid and the B liquid was fixed at 10 mL / min, (t or , t aq) As the conditions, except for changing to (0.2 sec, 1.8 sec), (0.4 sec, 1.6 sec), (1.6 sec, 0.4 sec), (1.8 sec, 0.2 sec) at valve operation 0.5 Hz, (0.1 sec, 0.4 sec), (0.4 sec, 0.1 sec) at 2 Hz, and (0.05 sec, 0.2 sec), (0.2 sec, 0.05 sec) at 4 Hz, it was carried out in the same manner as in Example 1. The slug length ratio calculated from the set value was in the range of 10, 20, 80, 90%, and this was designated as Example 2. The slug length ratio l or / (l or +l aq )×100% was measured together with Example 1.

[0033] <Example 3> The configuration shown in Fig. 3(c), that is, the function of opening and closing the flow path of each three-way valve was replaced by two two-way valves (normally closed type, normally open type). Otherwise, the same configuration as in Examples 1 and 2 was used. Two pumps were set for the flow rate so that the total flow rate of liquid A and liquid B would be approximately 3.4 mL / min. Except for setting the valve switching conditions to (t or , t aq ) = (0.12 sec, 0.12 sec), (0.36 sec, 0.12 sec), (0.60 sec, 0.12 sec), it was carried out in the same manner as in Example 1, and this was designated as Example 3. The lengths l or and l aq of the respective slug flows in the slug flow generation flow path were measured.

[0034] Fig. 7 shows the slug lengths (l or +l aq ) in the total flow rates of Example 1 and Comparative Examples 1 to 2. Fig. 8 shows the slug length ratio (l or / (l or +l aq )×100 [%]) in Example 2. Fig. 9 shows the respective slug lengths of the organic phase and the aqueous phase in Example 3.

[0035] According to FIG. 7, in Comparative Example 1, in the range of a total flow rate of 2 to 15 mL / min, the slag length (l or +l aq ) was 7.8 mm to 20.6 mm, and since it was a natural slag generation, the total flow rate and the slag length were related in a correlated manner. In Example 1, in the range of a total flow rate of 4 to 15 mL / min, the slag length (l or +l aq ) could be made in the range of 6.6 mm to 200 mm. Therefore, it can be seen that a slag length in a wider range than that in Comparative Example 1 could be controlled independently of the flow rate. In Comparative Example 2, in the range of a total flow rate of 39.6 to 61.8 mL / min, the slag length (l or +l aq ) was 2.6 mm to 4.5 mm. It can be inferred that the present invention is good at generating a slag flow having a longer slag length than Comparative Example 2. Also, in the present invention, it can be seen that the plots for each Hz approximately show a linear shape.

[0036] According to FIG. 8, it can be seen that a slag length ratio (vertical axis of the graph) approximately corresponding to the slag length ratio calculated from the set value of the equipment was obtained. Particularly at 0.5 Hz, it was closest to the calculated value. In the slag generation methods of Comparative Example 1 and Comparative Example 2, it was impossible to easily perform such control of the slag length ratio or the slag length by electronic control.

[0037] According to FIG. 9, while maintaining the total flow rate at about 3.4 mL / min and the aqueous phase slag length at about 2 mm, the organic phase slag length can be changed to 2.4 mm, 6.7 mm, and 10.7 mm by the opening and closing time of the valve. Also in Example 3 using two two-way valves instead of one three-way valve, it can be seen that the slag length ratio or the slag length can be controlled in the same manner as in Examples 1 and 2.

Industrial Applicability

[0038] The slag flow generation device according to the present invention can stably generate a highly precise slag flow within a flow rate range and a slag length range having a width, thereby promoting mass transfer between different fluids and enabling a synthesis reaction of high-quality chemical substances. Further, by connecting a liquid-liquid separation mechanism, a gas-liquid separation mechanism, etc. downstream of this generation device, it is expected to perform extraction separation, etc. at high speed and low cost. According to the present invention, it becomes possible to continuously perform a process from a reaction to separation and purification of chemical substances including various functional chemicals. Further, not limited to application to a continuous process, it is expected to perform the same at high speed and low cost by applying it to a reaction or extraction separation, etc. carried out in a batch process.

Claims

1. An apparatus for generating slug flows of a plurality of fluids, comprising: a fluid holding section for holding each of the plurality of fluids; a pump for constantly pumping each of the plurality of fluids; flow paths connecting the plurality of fluid holding sections, the pump, and the fluid confluence section and the pump respectively; and a slug flow generating flow path provided downstream of the fluid confluence section; valves are respectively installed in the flow paths between the fluid confluence section and the pump; a slug flow generating apparatus, wherein by means of the valves, one type of fluid is constantly pumped to the fluid confluence section, and the other fluids are controlled to be discharged to a discharge flow path.

2. The slug flow generating apparatus according to claim 1, wherein the discharge flow path is connected to the original fluid holding section, and the discharged fluid is recovered by the original fluid holding section.

3. The slug flow generating apparatus according to claim 1, wherein the discharge flow path is connected to a fluid confluence section different from the fluid confluence section, and the discharged fluid is pumped to the different fluid confluence section, whereby another slug flow generating flow path is provided in parallel.

4. The slug flow generating apparatus according to any one of claims 1 to 3, wherein reaction or separation is performed in the slug flow generating flow path.

5. The slug flow generating apparatus according to any one of claims 1 to 4, wherein at least one of the pumps has a temperature regulating mechanism for maintaining the liquid state of the fluid flowing through the head.

6. The slug flow generating apparatus according to claim 5, wherein one phase of the slug flow is liquefied carbon dioxide and the other phase is a liquid.

7. A chemical substance treatment apparatus comprising the slug flow generating apparatus according to any one of claims 1 to 6.

8. The chemical substance treatment apparatus according to claim 7, having a liquid-liquid separation mechanism downstream of the slug flow generating apparatus.

9. The chemical substance treatment apparatus according to claim 8, having a gas-liquid separation mechanism between the slug flow generating apparatus and the liquid-liquid separation mechanism.

10. The chemical substance treatment apparatus according to claim 9, wherein a gas discharge pipe provided with a pressure control mechanism is connected to the upper part of the gas-liquid separation mechanism, and a liquid discharge pipe connected to the liquid-liquid separation mechanism is connected to the lower part.

11. A method for generating slug flows by constantly pumping a plurality of fluids from their respective fluid holding sections to the fluid confluence section through respective flow paths by pumps, and generating a slug flow in a flow path downstream of the fluid confluence section, the method comprising: controlling a valve installed between the fluid confluence section and the pump to constantly pump one type of fluid to the fluid confluence section and discharge the other fluids to a discharge flow path.

12. The slag flow generation method according to claim 11, wherein the fluid discharged into the discharge flow path is recovered to the original fluid holding part.

13. The slag flow generation method according to claim 11, wherein the fluid discharged into the discharge flow path is pumped to a fluid confluence part different from the fluid confluence part, and slag flow is generated in parallel in another slag flow generation flow path.

14. The slag flow generation method according to any one of claims 11 to 13, wherein reaction or separation is performed in the flow path for generating the slag flow.

15. The slag flow generation method according to any one of claims 11 to 14, wherein at least one of the pumps performs temperature control to maintain the liquid state of the fluid flowing through the head.

16. The slag flow generation method according to claim 15, wherein one phase of the slag flow is liquefied carbon dioxide and the other phase is a liquid.

17. A method for treating a chemical substance including the slag flow generation method according to any one of claims 11 to 16.

18. The method for treating a chemical substance according to any one of claims 11 to 17, including liquid-liquid separation of the generated slag flow.

19. The method for treating a chemical substance according to claim 18, including liquid-liquid separation after gas-liquid separation of the generated slag flow.

20. The method for treating a chemical substance according to claim 19, including discharging the gas separated by gas-liquid separation from the upper part while controlling the pressure, and discharging the liquid separated by liquid-liquid separation from the lower part.

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