Slug flow generating device, chemical substance treatment apparatus equipped with said generating device, slug flow generating method, and chemical substance treatment method using slug flow

The slug flow generating device with a single reciprocating pump and multiple heads addresses the complexity and precision issues of conventional systems, achieving stable and efficient slug flow for high-speed chemical processing.

JP7720558B2Active Publication Date: 2025-08-08NATIONAL INSTITUTE OF ADVANCED INDUSTRIAL SCIENCE & TECHNOLOGY +1
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Patent Information

Application Number
JP2021090993
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Filing Date
2021-05-31
Publication Date
2025-08-08
Estimated Expiration
2041-05-31

AI Technical Summary

Technical Problem

Conventional slug flow generation devices require multiple pumps and complex mechanisms for fluid control, leading to large and intricate equipment, and struggle with precise liquid transfer and versatility in handling different fluid combinations.

Method used

A slug flow generating device using a single reciprocating pump with multiple heads, driven by a mechanical camshaft, alternately pumps incompatible fluids to generate slug flow, enabling precise liquid delivery and reducing interphase mass transfer resistance.

Benefits of technology

The device stabilizes slug flow over a wide range of flow rates, facilitating high-speed processing and compact design, with improved liquid transfer accuracy and versatility in handling various fluid combinations.

✦ Generated by Eureka AI based on patent content.

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Abstract

To provide a generation device for slug flow that can reduce the number of pumps that are required in reproducing slug flow so as to be downsized and simplified, and can accurately feed liquid in a wide flow rate range, and a generation method for slug flow.SOLUTION: A generation device for slug flow comprises: a plurality of fluid supply parts; a reciprocating pump which has a plurality of enclosures defining a space sandwiched between a suction-side valve and an ejection-side valve which operate in a non-return manner, through which fluid in the enclosures is alternately and intermittently fed by pressure; a plurality of suction piping parts connecting the plurality of fluid holding parts to the plurality of enclosures respectively; a plurality of ejection piping parts connecting the plurality of enclosures to fluid merging parts respectively; and fluid accumulation parts connected to downstream sides of the fluid merging parts, and a chemical substance treatment device comprising the generation device.SELECTED DRAWING: Figure 3
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Description

[Technical Field]

[0001] The present invention relates to a slug flow generating device, a chemical substance processing apparatus including the slug flow generating device, a slug flow generating method, and a chemical substance processing method using a slug flow, in which the term "processing" refers to a reaction or separation (extraction, absorption, crystallization, etc.) of chemical substances or a reactive separation. [Background technology]

[0002] In conventional chemical reaction processes, there has been a demand for efficiency through scaling up. In recent years, there has also been an increased demand for reducing environmental impact and saving resources and energy. Batch production, which is suitable for small-scale production, is the mainstream method for producing high-value-added products such as pharmaceuticals, functional chemicals, and fine chemicals, which are expected to grow in the future. However, because it involves large energy losses and produces a large amount of co-products, there has been a recent trend toward using flow production methods (hereinafter referred to as "flow processes"), which perform operations from reaction to separation and purification in a continuous manner to reduce losses between each batch processing step. There is also a movement in research and development to modularize each unit operation incorporated into a flow process so that it can be used to manufacture a wide variety of functional chemicals by rearranging reaction modules and separation and purification modules as needed (Non-Patent Document 1).

[0003] In a flow process, operations such as temperature adjustment, pressure adjustment, mixing, reaction, extraction, separation and purification are performed while a fluid flows through a pipe or through equipment connected to the pipe. Compactness and high-speed processing are required for each unit operation module. In particular, important targets in flow processes are processes involving the flow of multiphase fluids that are partially or completely soluble in each other (e.g., liquid-liquid reaction, gas-liquid reaction, liquid-liquid extraction, gas-liquid extraction, gas-liquid separation, and liquid-liquid separation). In processes involving multiphase fluids, reducing interphase mass transfer resistance is typically important when aiming for compactness and high-speed processing (Non-Patent Documents 2, 3, 4).

[0004] The larger the contact interface between the phases, the lower the interphase mass transfer resistance, and the higher the reactivity. As a means for reducing the interphase mass transfer resistance, it is known to incorporate a stirring mechanism into the reactor to increase the contact interface between the phases. Non-Patent Document 5 describes the active use of a fluid state called turbulence by means of a stirring mechanism within a batch reactor. Patent Document 1 describes a method in which an ultrasonic vibrator is placed downstream of an introduction portion for a plurality of sample fluids, and the sample fluids are stirred and mixed. Furthermore, Patent Document 2 describes that a minute stirrer made of carbon nanotubes is rotated in a recess in a flow channel to stir the liquid, thereby changing the flow from laminar to turbulent, thereby shortening the reaction time. However, adopting the above method requires complex flow channel configurations and the installation of vibrators or stirrers for mixing, making it difficult to design the device. Also, if incompatible liquids are dispersed too finely, an emulsion state (the fluid state shown in Figure 1(f)) results, resulting in a large contact interface between the phases. While this is advantageous for reactions or extraction, it makes it difficult to improve the efficiency of phase separation.

[0005] In multiphase fluid processes, one approach is to compact the equipment to actively utilize 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 a low Reynolds number and predominantly laminar flow. Even in this laminar region, slug flow (also known as segmented flow or Taylor flow; see Figures 1(a) and 1(b)), in which separate fluids of different phases alternate, reduces mass transfer resistance by promoting interface renewal due to internal circulating flow within the slug caused by shear from the wall. Another advantage is the ability to form large fluid masses, resulting in a relatively short phase separation time (Patent Document 3). Figure 1 shows a typical flow state of multiphase flow. For example, in the flow states shown in Figure 1(c) to (f), the effect of reducing mass transfer resistance cannot be obtained, whereas in the slug flow shown in (a) and (b), the effect of reducing mass transfer resistance due to internal circulation flow is achieved.

[0006] Conventionally, slug flow has been generated by pumping a plurality of fluids of different phases using a plurality of fluid transport means, namely, pumps, corresponding to the respective fluids. Figures 2(a) and (b) show conceptual diagrams of a conventional slug flow generating device. Specifically, in the case of two-phase fluids, as shown in Patent Document 3 (claim 9) and Non-Patent Document 4 (Fig. 2), two immiscible liquids are pumped together and merged in a T-shaped channel or the like to generate a slug flow. In the case of three-phase fluids, a slug flow can also be generated by combining the fluids pumped using three or more pumps (Fig. 1 in Non-Patent Document 6, Fig. 1 in Non-Patent Document 7).

[0007] Furthermore, as a means for generating a slug flow more stably, Patent Document 8 describes a method in which two incompatible liquids are alternately flowed by switching a valve installed in a flow path to generate a slug flow and extract and separate the extractant. This method makes it possible to send the liquids alternately with good reproducibility in a laminar flow-dominated environment. Non-Patent Document 9 describes that the slug length can be controlled by controlling the operation of two piezoelectric micropumps in conjunction with each other by changing the voltage and frequency. [Prior art documents] [Patent documents]

[0008] [Patent Document 1] Japanese Patent Application Publication No. 11-347392 [Patent Document 2] Japanese Patent Application Laid-Open No. 2004-321063 [Patent Document 3] Japanese Patent Publication No. 2020-32346 [Non-patent literature]

[0009] [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] J.R. Burns and C. Ramshaw, The intensification of rapid reactions in multiphase systems using slug flow in capillaries, Lab Chip, 2001, 1, 10-15 [Non-patent document 3] Matthew W. Losey, Martin A. Schmidt, and Klavs F. Jensen, Microfabricated MultiphasePacked-Bed Reactors: Characterization of Mass Transfer and Reactions, Ind. Eng. Chem. Res.2001, 40, 12, 2555-2562 [Non-patent document 4] Madhvanand N. Kashid, Albert Renken, Lioubov Kiwi-Minske, Gas-liquid and liquid-liquid mass transfer in microstructure reactors, Chemical Engineering Science 66 (2011) 3876-3897 [Non-Patent Document 5] Fanfu Guan, Nikil Kapur, J. Taylor, Jialin Wen, Xumu Zhang and A.John Blacker, A universal reactor platform for batch and flow: application tohomogeneous and heterogeneous hydrogenation, React. Chem. Eng., 2020, 5, 1903-1908 [Non-patent document 6] 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 7] Nobuaki Aoki, Ryuichi Ando, and Kazuhiro, Mae,Gas-Liquid-Liquid Slug Flow for Improving Liquid-Liquid Extraction inMiniaturized Channels, Ind. Eng. Chem. Res. 2011, 50, 8, 4672-4677 [Non-patent document 8] Nobutaka Kadowaki, Development and Application of Three-Way Solenoid Valves for Micro Chemical Processes, Okayama University Graduate School Doctoral Dissertation, Chapter 3, March 2014 [Non-Patent Document 9] K301 SCEJ 86th Annual Meeting Generation of liquid-liquid slug flow by two pumps operating in tandem Summary of the Invention [Problem to be solved by the invention]

[0010] Although generating a slug flow is effective in reducing interphase mass transfer resistance, conventional generation devices require more than one pump to pump one type of fluid, and also require mechanisms for flow control and switching valves for alternate liquid transfer, making the equipment large and complex. Furthermore, because each pump has its own individual differences, it is necessary to adjust the liquid transfer volume and liquid transfer speed conditions each time the combination of multiple pumps is changed. Furthermore, the piezoelectric micropump (PMP) described in Non-Patent Document 9 is a diaphragm pump using a piezoelectric element, and controls the discharge pressure by changing the amplitude of the diaphragm using voltage. Because the discharge pressure is low, it is difficult to prevent backflow, making it difficult to deliver liquid precisely. Furthermore, the three-phase slug flow generated by existing technology is limited in the combinations of liquid species that can be extracted and separated, making it less versatile. Therefore, an object of the present invention is to provide a slug flow generating device that reduces the number of pumps required to generate a slug flow, thereby making it smaller and simpler, and that can perform precise liquid transfer while maintaining conditions that are effective in reducing interphase mass transfer resistance, and to provide a chemical substance treatment apparatus equipped with this slug flow generating device. [Means for solving the problem]

[0011] The inventors focused on the mechanism in which each plunger of a double plunger pump alternately pumps fluids, and discovered that a slug flow can be generated by using a pumping method in which one fluid does not flow while the other fluids do not flow when two or more completely incompatible fluids are pumped.

[0012] That is, in order to solve the above problems, the present invention employs the following means. [1] A device for generating a slug stream of multiple fluids, comprising: a plurality of fluid holding portions each holding the plurality of fluids; The valve has a plurality of housings that define a space between a suction-side valve and a discharge-side valve, and the fluid in each housing is By using a mechanical drive system with a camshaft to perform suction and discharge, Alternately intermittently pumped reciprocating pumps; a plurality of suction pipes respectively connecting the plurality of fluid holding units to the plurality of housings; a plurality of discharge pipes respectively connecting the plurality of housings to a fluid confluence portion; and A slug flow generating device having a fluid retention section connected downstream of the fluid confluence section. [ 2 ] the fluid retention section in which reaction or separation occurs [1 ]of A device for generating slug flow. [ 3 ] At least one of the plurality of housings has a temperature control function to maintain the liquid state of the fluid flowing through the housing [1] or [2] A device for generating slug flow. [ 4 ] one phase of the slug stream is liquefied carbon dioxide and the other phase is liquid 3 ] A device for generating slug flow. [ 5 ]The above [1]~[ 4 ] A chemical treatment apparatus equipped with a slug flow generating device according to any one of the preceding claims. [ 6 ] The device for generating a slug flow has a liquid-liquid separation mechanism downstream thereof. 5 ] Chemical substance processing equipment. [ 7 ] the device for generating a slug flow and the liquid-liquid separation mechanism, 6 ] Chemical substance processing equipment. [ 8 ] A gas discharge pipe equipped 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 of the gas-liquid separation mechanism. 7 ] Chemical substance processing equipment. [ 9 ] A valve having a plurality of housings that define a space between a suction side valve and a discharge side valve that operate in a non-return manner. The pump is a single unit that performs suction and discharge using a mechanical drive system with a camshaft. Using a reciprocating pump, alternately and intermittently sending the plurality of fluids through a plurality of suction piping means connecting the plurality of fluid supply units to the plurality of housings, respectively, and a plurality of discharge piping means connecting the plurality of housings to a confluence of the plurality of fluids; A method for generating slug flows of the plurality of fluids in a fluid retention section provided downstream of the confluence section. [ 10 ]The above[ 9 ] A method for treating a chemical substance, comprising: a method for producing a slug flow of the [ 11 ] The generated slug flow is subjected to liquid-liquid separation. 10 ] Methods for treating chemical substances. [ 12 ] The generated slug flow is separated into gas and liquid, and then separated into liquid and liquid. 11 ] Methods for treating chemical substances. [ 13 ] by applying back pressure to the gas separated from the gas-liquid to control the pressure of the entire fluid 12 ] Methods for treating chemical substances. [Effects of the Invention]

[0013] According to the present invention, a slug flow can be stably generated over a wide range of flow rates, thereby enabling high-speed processing while making a chemical manufacturing device that utilizes a slug flow more compact. Furthermore, the reciprocating pump is driven by an eccentric camshaft that moves in conjunction with the rotation of the motor, which allows for high discharge pressure, prevents backflow, and achieves highly accurate liquid delivery. [Brief explanation of the drawings]

[0014] [Figure 1] Representative flow diagrams for multiphase flows: (a) Two-phase slug flow, (b) Three-phase slug flow, (c) Parallel flow, (d) Annular flow, (e) Droplet flow, (f) Dispersed flow [Figure 2] Diagram of a conventional slug flow generating device: (a) Two-phase system, (b) Three-phase system [Figure 3] Diagram of the slug flow generating device of the present invention. (a) Two-phase system, (b) Three-phase system [Figure 4] Graph showing the liquid delivery accuracy of plunger pumps and piezoelectric micropumps (PMPs) [Figure 5] Confluence pattern of fluid confluence: (a) Two-phase system, (b) Three-phase system [Figure 6]1 is a diagram showing the configuration of a chemical substance treatment apparatus using a slug flow generating device according to the present invention. [Figure 7] Visual flow state of toluene / water (Example 1 and Comparative Example 1) at each liquid flow rate [Figure 8] Visual flow state at each liquid flow rate for toluene / ethanol:water = 1:1 (Example 2 and Comparative Example 2) [Figure 9] Visual flow state at each liquid flow rate for toluene / ethanol:water=2:1 (Example 3 and Comparative Example 3) [Figure 10] Visual flow state at each liquid flow rate of toluene / ethanol:water=3:1 (Example 4 and Comparative Example 4) [Figure 11] Visual flow state of the toluene-rich phase / ethanol-rich phase (Example 5 and Comparative Example 5) at each liquid flow rate [Figure 12] Changes in flow state over time for toluene / water (Example 1 and Comparative Example 1) at a liquid flow rate of 4 mL / min [Figure 13] Changes in flow state over time at a liquid flow rate of 4 mL / min for toluene / ethanol:water = 2:1 (Example 3 and Comparative Example 3) DETAILED DESCRIPTION OF THE INVENTION

[0015] The terms used in this specification will be explained below. The pump's "multiple housings that define the space between the suction-side valve and the discharge-side valve that operate in a non-return manner" are called the "head." A pumping method in which a type of liquid corresponding to the number of pump heads is supplied at each head, and while one fluid is flowing, the other fluids do not flow is called "alternate pumping." One fluid, more than one head One pump with A common pumping method characterized by pumping liquids at a single pressure is called "single liquid pumping."

[0016] While a typical slug flow is generated by a combination of multiple pumps, in which a single pump with one or more heads pumps a single fluid, the present invention is characterized in that a slug flow is generated by alternating pumping, in which a single pump with multiple heads is used to pump multiple fluids alternately and intermittently so that while one fluid is flowing, the other fluids are not flowing. The present invention is also characterized in that it enables the treatment of chemical substances by reacting or separating (extracting, absorbing, crystallizing, etc.) the chemical substances that have been reacted or separated while the slug flow is retained, or by subjecting the chemical substances to liquid-liquid separation, and, if necessary, gas-liquid separation. Hereinafter, the present invention will be described based on an embodiment (hereinafter referred to as "the present embodiment"), but the present invention is not limited to the present embodiment.

[0017] [Slug flow generating device and slug flow generating method] Known reciprocating pumps with multiple heads include double plunger pumps and triple plunger pumps, which have two or more plungers in one pump. These pumps have multiple heads, and the reciprocating motion of each plunger alternately pumps fluid from each head, offsetting fluctuations in flow rate from each head and suppressing pulsation. However, because the fluid pumped from each head is usually the same, these pumps pump a single liquid at a constant flow rate.

[0018] In this embodiment, a different fluid is supplied to each head by utilizing the known pump pulsation suppression mechanism. Figures 3(a) and (b) show a configuration using a plunger pump. The reciprocating pump is preferably driven mechanically to obtain high pumping force for precise liquid delivery, preferably by an eccentric camshaft that rotates in conjunction with the rotation of the motor. In addition to the plunger pump, a diaphragm pump is also a typical example. Figure 4 shows a comparison of the liquid delivery accuracy between the plunger pump used in this example (described later) and a piezoelectric micropump (PMP) in which reciprocation is performed electrically by a piezoelectric element. An example of the results for the former is shown in Figure 4(a), and an example of the results for the latter is shown in Figure 4(b). R of the approximated line 2 If the value is used as an index, the former is R 2 = 1.0 (> 0.999), and the latter R 2 = 0.968, it can be seen that the plunger pump has higher liquid delivery accuracy than the PMP.

[0019] The different fluids are those that are not completely miscible, since miscible fluids do not form a slug flow. The fluids may be liquid-liquid, consisting of an aqueous phase and an oil phase, or gas-liquid, consisting of a liquid phase and a gas phase. The liquid phase may be a liquefied gas, such as liquefied carbon dioxide. The fluid may be any one of supercritical fluids, subcritical fluids, and fluids that are immiscible with ionic liquids.

[0020] If one or more of the fluids is a gas at room temperature and pressure, the fluid is liquefied as it passes through the pump head, so it is preferable that the head through which the fluid passes has a temperature control function to maintain the fluid in a liquid state. A preferred gas capable of forming a slug flow is carbon dioxide, which has a gas-liquid equilibrium temperature of 31°C or less.

[0021] As an example of a combination of aqueous phase and carbon dioxide, consider a case where the pump discharges liquefied carbon dioxide. In this case, the process should preferably be performed at or above the critical pressure of carbon dioxide (7.4 MPa), and a back-pressure valve can be installed downstream of the slug flow region to control the pressure from the pump to the back-pressure valve. Since carbon dioxide can only replace organic solvents under high pressure, it is expected that hydrophobic valuables in the aqueous phase will be extracted by the high-pressure carbon dioxide.

[0022] The multiple fluids are alternately and intermittently pumped to the fluid junction via multiple fluid holding sections (liquid tanks or gas cylinders, etc.) that hold each fluid and multiple suction piping sections that connect the multiple heads, and multiple discharge piping sections that connect each head and the fluid junction, and a slug flow can be generated in a fluid stagnation section that is connected downstream of the fluid junction.

[0023] Figures 5(a) and (b) show the confluence pattern of the fluid confluence area. However, the collision order and collision angle θ are not specified in Figure 5. In the fluid retention section, reactions including liquid-liquid reactions, gas-liquid reactions, and solid catalyst reactions, separation by extraction, absorption, crystallization, etc., or reaction separation can be carried out.

[0024] [Chemical substance treatment device and treatment method] In this embodiment, as shown in FIG. 6, after reaction, separation, or reaction separation is carried out in the fluid retention section where the slug flow is generated, a liquid-liquid separator is disposed downstream of the fluid retention section, and if necessary, a gas-liquid separator is disposed between the fluid retention section and the liquid-liquid separator, to continuously separate and purify the phase containing the chemical substance. When a gas-liquid separator is provided, a gas discharge pipe equipped with a back pressure valve is connected to the top of the gas-liquid separator, and a liquid discharge pipe connected to the liquid-liquid separator is connected to the bottom. The back pressure valve can control the pressure between the pump outlet and the back pressure valve. [Example]

[0025] 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.

[0026] Example 1 A double plunger pump (Nihon Seimitsu Kagaku NP-KX-220P, plunger diameter 4.6 mm, stroke length: 5 mm (liquid volume per stroke: 0.0831 mL)) driven by a camshaft and equipped with a pulsating flow suppression mechanism was used. A tank containing toluene (liquid A) was connected to the suction side of one head via a suction pipe, and a tank containing water (liquid B) was connected to the suction side of the other head via another suction pipe. The discharge side of each head was connected via its respective discharge pipe to a confluence of liquids A and B, consisting of a 2 mm inner diameter stainless steel tee. A fluid retention section consisting of a 2 mm inner diameter, 30 cm long glass tube was connected downstream of the confluence. The plungers were reciprocated to alternately pump the A and B solutions so that their flow rates were equivalent to 0.5, 1, 2, 4, 6, 8, and 10 mL / min, respectively, and the flow state in the fluid retention area was visually checked.

[0027] <Examples 2 to 4> Alternate pumping was carried out in the same manner as in Example 1, except that solution B was changed to a solution in which the volume ratio of ethanol / water was 1:1 (Example 2), 2:1 (Example 3), or 3:1 (Example 4).

[0028] <Comparative Examples 1 to 4> Comparative Example 1 was prepared in the same manner as in Examples 1 to 4, except that two double plunger pumps identical to those in Example 1 were used, liquid A was supplied to the two heads of one pump, and liquid B was supplied to the two heads of the other pump, and liquid A and liquid B were pumped one by one by each pump so that the respective flow rates were the same as in Example 1. Furthermore, the liquid was transferred in the same manner as in Comparative Example 1, except that the liquid B was changed to an ethanol / water solution with the same volume ratio as in Examples 2 to 4, and these were designated Comparative Examples 2 to 4, respectively.

[0029] <Example 5> Equal amounts of toluene and a liquid with a volume ratio of ethanol / water of 1:1 were mixed, and then the liquids were separated, with the toluene-rich liquid being designated Liquid A and the ethanol-rich liquid being designated Liquid B. In other words, Liquid A and Liquid B are two completely immiscible liquids. Liquid A and Liquid B were alternately pumped using a single double plunger pump, as in Example 1.

[0030] <Comparative Example 5> The same liquids A and B as in Example 5 were pumped together using two double plunger pumps in the same manner as in Comparative Example 1.

[0031] 7 to 11 show the flow state in the fluid stagnation portion at each liquid flow rate in Examples 1 to 5 and Comparative Examples 1 to 5. In the figure, circles indicate slug flow, black circles indicate slug flow occurring downstream, squares indicate stratified flow, and triangles indicate annular flow. Flows containing droplets of any size are marked with a prime. 12 and 13 show the time-dependent changes in the flow state in the fluid retention area when the flow rate of each liquid was 4 mL / min, visualized by the potential digitized by a photoelectric sensor, in Example 1 and Comparative Example 1, and in Example 3 and Comparative Example 3. If the slug flow is stable, it will show regular rectangular changes in potential that reflect the alternating flow of two phases.

[0032] 7 shows that slug flows occurred in Example 1 and Comparative Example 1 regardless of the flow rate of each liquid, from 0.5 to 10 mL / min. However, according to Fig. 12, in Comparative Example 1, the alternating period of the slug flows was short, averaging 0.20 seconds, suggesting that separation and purification of chemical substances following the fluid stagnation area would be difficult, whereas in Example 1, alternating flows with a long period, averaging 1.24 seconds, were observed, indicating that separation and purification would be easy after reactions, extractions, etc., occurred in the slug flows.

[0033] 8, it can be seen that in Comparative Example 2, the flow rate range for generating a slug flow was narrow and limited, but in Example 2, a slug flow was generated at a flow rate of 1 to 10 mL / min. The relationship between Comparative Example 3 and Example 3 in Figure 9 is similar; in Comparative Example 3, a slug flow was not generated unless the flow rate was 4 mL / min or less, but in Example 3, a slug flow was generated at flow rates up to 8 mL / min. Furthermore, according to FIG. 10, in Comparative Example 4 (where the difference in polarity and specific gravity with respect to Liquid A is smaller), in which the organic content of Liquid B is higher than in Comparative Examples 2 and 3, no slug flow was obtained, whereas in Example 4, the generation of a slug flow was observed over a wide range of flow rates.

[0034] The change in the flow state over time for the droplet-containing slug flow of Example 3 was confirmed in Figure 13. A periodic waveform with an average of 1.27 seconds was observed, which is thought to be due to the alternate flow of liquids A and B. On the other hand, only an irregular, random waveform was obtained from Comparative Example 3.

[0035] According to Figure 11, even in the case of toluene-rich and ethanol-rich two-phase flows, the generation of slug flow was hardly observed in Comparative Example 5, whereas in Example 5, the generation of slug flow was observed, although it contained droplets, in the flow rate range of 1 to 10 mL / min. [Industrial Applicability]

[0036] The slug flow generating device of the present invention can stably generate highly precise slug flows over a wide flow rate range, facilitating mass transfer between different fluids and enabling high-quality chemical synthesis reactions. Furthermore, by connecting a liquid-liquid separation mechanism or a gas-liquid separation mechanism downstream of this generating device, extraction and separation processes can be performed quickly and at low cost. The present invention enables continuous processes from reaction to separation and purification for chemical substances, including a wide variety of functional chemicals. Furthermore, the present invention is not limited to application to continuous processes; it can also be applied to reactions or extraction and separation performed in batch processes, enabling similar high-speed and low-cost performance.

Claims

1. 1. A device for producing a slug stream of multiple fluids, comprising: a plurality of fluid holding portions each holding the plurality of fluids; A reciprocating pump having a plurality of housings defining a space between a suction-side valve and a discharge-side valve that operate in a check manner, in which the fluid in each housing is alternately and intermittently pumped by suction and discharge using a mechanical drive system using a camshaft; a plurality of suction pipes respectively connecting the plurality of fluid holding units to the plurality of housings; a plurality of discharge pipes respectively connecting the plurality of housings to a fluid confluence portion; and A slug flow generating device having a fluid retention section connected downstream of the fluid confluence section.

2. The device for generating a slug flow according to claim 1 , wherein a reaction or separation takes place in the fluid retention section.

3. 3. The slug flow generating device according to claim 1, wherein at least one of the plurality of housings has a temperature control function for maintaining the fluid flowing within the housing in a liquid state.

4. 4. The device for generating a slug stream according to claim 3, wherein one phase of the slug stream is liquefied carbon dioxide and the other phase is a liquid.

5. A chemical substance treatment device comprising the slug flow generating device according to any one of claims 1 to 4.

6. 6. The chemical substance treatment apparatus according to claim 5, further comprising a liquid-liquid separation mechanism downstream of the slug flow generating device.

7. 7. The chemical substance treatment apparatus according to claim 6, further comprising a gas-liquid separation mechanism between the slug flow generating device and the liquid-liquid separation mechanism.

8. 8. The chemical substance treatment device according to claim 7, wherein a gas discharge pipe equipped 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.

9. The pump has a plurality of housings that define a space between a suction-side valve and a discharge-side valve that operate in a check manner, and uses one reciprocating pump that performs suction and discharge using a mechanical drive system using a camshaft. alternately and intermittently sending the plurality of fluids through a plurality of suction piping means connecting the plurality of fluid supply units to the plurality of housings, respectively, and a plurality of discharge piping means connecting the plurality of housings to a confluence of the plurality of fluids; A method for generating slug flows of the plurality of fluids in a fluid retention section provided downstream of the confluence section.

10. A method for treating chemicals comprising the method for generating a slug stream according to claim 9.

11. 11. The method for treating chemical substances according to claim 10, wherein the resulting slug stream is subjected to liquid-liquid separation.

12. 12. The method for treating a chemical substance according to claim 11, wherein the generated slug stream is subjected to gas-liquid separation and then liquid-liquid separation.

13. The method for treating a chemical substance according to claim 12, wherein a back pressure is applied to the gas separated from the liquid to control the pressure of the entire fluid.

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