Method for forming striped fluid, method for producing chemical substances, and apparatus for forming striped fluid

By introducing and reducing flow rates of incompatible fluids alternately, the method and apparatus facilitate the formation of slug flows with high throughput and simplified control, addressing the complexity of existing slug flow technologies.

JP2025150526APending Publication Date: 2025-10-09TOKUYAMA CORP
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Patent Information

Application Number
JP2024051435
Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
Filing Date
2024-03-27
Publication Date
2025-10-09

AI Technical Summary

Technical Problem

Existing technologies for forming slug flows require complex device structures due to the need for high flow rates, which complicates the control of fluid dynamics at the confluence.

Method used

A method and apparatus that form striped fluids by introducing two or more incompatible fluids into a flow channel, then simultaneously reducing the flow rates of all fluids to less than their introduction rates but greater than 0 mL/min, alternating between introduction and formation steps to create a slug flow.

Benefits of technology

This approach allows for the easy formation of slug flows at high rates without the need for complex valve control, maintaining the striped fluid pattern even when flow rates increase, thus simplifying the device structure and enhancing throughput.

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Abstract

To provide a technology capable of more easily forming a slug flow.SOLUTION: Provided is a method for forming a striped fluid in which two or more mutually immiscible fluids respectively constitute two or more phases arranged alternately along the longitudinal direction of a flow channel. The method comprises: an introduction step, in which the two or more fluids are together introduced into the flow channel to form a flow of the two or more fluids; and a formation step, in which the flow rates of all the two or more fluids in the flow channel are simultaneously set to less than each of the flow rates of the two or more fluids in the introduction step, or more than 0 mL / min, so that the striped fluid is formed. These steps are alternately repeated to generate the striped fluid.SELECTED DRAWING: Figure 1
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Description

[Technical Field]

[0001] The present invention relates to a method for forming a striped fluid, a method for producing a chemical substance, and an apparatus for forming a striped fluid. [Background technology]

[0002] In chemical manufacturing processes, a slug flow, in which two or more phases alternately flow side by side along the length of a flow channel, is sometimes used for the purposes of heterogeneous reactions, extraction, and separation. Patent Document 1, for example, describes a technology for generating a slug flow. The device includes fluid holding units that hold multiple fluids, pumps that constantly pump each of the multiple fluids, flow channels connecting the multiple fluid holding units to the pumps and the pumps to a fluid confluence, and a slug flow generating channel located downstream of the fluid confluence. Valves are installed in each channel between the fluid confluence and the pumps, and the valves control the system so that only one type of fluid is constantly pumped to the fluid confluence and the other fluids are discharged to a discharge channel. [Prior art documents] [Patent documents]

[0003] [Patent Document 1] Japanese Patent Publication No. 2023-13422 Summary of the Invention [Problem to be solved by the invention]

[0004] The technology described in Patent Document 1 is capable of forming a slug flow at a large flow rate, but has the problem of requiring a complex device structure.

[0005] An object of one aspect of the present invention is to provide a technique that can more easily form a slug flow. [Means for solving the problem]

[0006] In order to solve the above-mentioned problems, one embodiment of the present invention provides a method for forming a striped fluid, which is a method for forming a striped fluid in which two or more phases, each composed of two or more mutually incompatible fluids, are arranged alternately along the length of a flow channel, and which alternately includes an introduction step in which the two or more fluids are introduced together into the flow channel to form flows of the two or more fluids, and a formation step in which the flow rates of all of the two or more fluids in the flow channel are simultaneously reduced to less than the flow rates of each of the two or more fluids in the introduction step and greater than 0 mL / min, so as to form the striped fluid.

[0007] In order to solve the above problems, one embodiment of the present invention provides an apparatus for forming a striped fluid, which forms a striped fluid in which two or more phases composed of two or more mutually incompatible fluids are arranged alternately along the length of a flow path, and which comprises two or more tanks for holding each of the two or more fluids, flow paths connected to the two or more tanks, a pump for pressurizing each of the two or more fluids into the flow paths, and a control unit. The control unit causes the apparatus for forming a striped fluid to perform an introduction process in which the two or more fluids are introduced together into the flow paths to form a flow of the two or more fluids, a formation process in which the flow rates of all of the two or more fluids in the flow paths are simultaneously reduced to less than the flow rates of each of the two or more fluids in the introduction process and greater than 0 mL / min so as to form the striped fluid, and a process in which the apparatus for forming a striped fluid alternately performs the introduction process and the formation process. [Effects of the Invention]

[0008] According to one aspect of the present invention, a slug flow can be more easily formed. [Brief explanation of the drawings]

[0009] [Figure 1] 1 is a flow diagram showing a method for forming a striped fluid according to an embodiment of the present invention. [Figure 2]1A and 1B are schematic diagrams showing the relationship between the change in flow rate over time and the state of the fluid in the flow channel in a striped fluid formation method according to one embodiment of the present invention. (a) is a graph showing the change in flow rate over time. (b) shows the state of the fluid in the flow channel during the first introduction step shown in (a). (c) shows the state of the fluid in the flow channel during the first formation step shown in (a). (d) shows the state of the fluid in the flow channel during the next introduction step shown in (a). (e) shows the state of the fluid in the flow channel during the next formation step shown in (a). [Figure 3] 1 is a block diagram showing the configuration of a striped fluid forming device according to an embodiment of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0010] [Concept of the present invention] When using slug flows in industrial applications, a high flow rate is often desired to increase the throughput of chemicals. To achieve this, it is usually necessary to increase the flow rates of each of the two or more fluids that make up the slug flow. However, increasing the flow rates of two or more fluids makes it difficult to control the dynamics of the two or more fluids at the confluence. Specifically, when two or more fluids are simultaneously introduced into a confluence, the fluids discharged from the confluence form a slug flow in the flow path downstream of the confluence immediately after introduction. However, once the fluids form parallel flows within the confluence due to unstable dynamics, the subsequent discharge from the confluence remains a stable parallel flow. To avoid this, the technology described in Patent Document 1 introduces only one fluid into the confluence by rapidly switching a valve installed upstream of the confluence, but this requires a complex device structure for high-speed valve control.

[0011] The inventors have found that even if the fluids form parallel flows, reducing the flow rates of all fluids while continuing to introduce them changes the fluid pattern from parallel flows to striped flows within the channel. Furthermore, they have found that striped flows, once formed in the channel, do not easily return to parallel flows but instead flow as slug flows, even when the flow rates of all fluids are increased to their original levels. These phenomena are presumed to be due to the following principle: Once parallel flows are formed at the confluence, friction occurs between the inner wall and the flow rate. This friction is particularly large at the phase boundary between the two fluids. Therefore, the flow rate of all fluids decreases, and the flow rate of the two fluids stabilizes as parallel flows, preventing the formation of a phase boundary between the two fluids. On the other hand, reducing the flow rates of all fluids reduces friction, and the surface tension, which acts to minimize the contact area between the two fluids, becomes dominant over the friction, resulting in the parallel flow pattern changing to striped flows. Once the striped fluid is formed in the channel, the friction it experiences increases again when the flow rate returns to its original level. However, unlike the confluence, which is unstable, the pressure acting unilaterally in the flow direction in the channel dominates over the friction, and the striped fluid continues to flow as a slug without changing its form.

[0012] As mentioned above, in order to achieve a large flow rate of a slug flow, it is usually necessary to consider how to increase the flow rate of each of the two or more fluids that form the slug flow. However, the inventors have changed their approach and discovered that by continuing to introduce all the fluids while reducing their flow rates, a striped fluid that includes a slug flow as one aspect of the flow can be formed, thereby completing the present invention.

[0013] [Striped fluid] As used herein, a striped fluid refers to a fluid in which two or more phases, each composed of two or more mutually immiscible fluids, alternate along the length of the flow channel. For example, a fluid in which a phase PA composed of a first fluid A and a phase PB composed of a second fluid B are arranged in the order PA, PB, PA, PB, ... is a striped fluid. The number of fluids constituting a striped fluid may be three or more. For example, a fluid in which a phase PA composed of a first fluid A, a phase PB composed of a second fluid B, and a phase PC composed of a third fluid C are arranged in the order PA, PB, PC, PA, PB, PC, ... is a striped fluid. In a striped fluid, the order of the phases is not limited as long as adjacent phases are composed of the same fluid. For example, a fluid in which the phases are arranged in an irregular order, such as PA, PB, PA, PC, PB, PA, ..., is also a striped fluid.

[0014] Furthermore, each of the two or more fluids may be immiscible with at least one of the other fluids. For example, the fluids may be an aqueous solution A, an aqueous solution B that is miscible with the aqueous solution A, and an organic solvent C that is immiscible with the aqueous solutions A and B. In this case, a striped fluid may be formed that includes a phase PAB formed by the mixture of the aqueous solutions A and B, and a phase PC formed by the organic solvent C.

[0015] The "striped fluid" may be in a state of flowing through a flow channel, or in a state of being stationary and not flowing through a flow channel. In this specification, the striped fluid in a state of flowing through a flow channel may be referred to as a "slug flow."

[0016] [Method for forming striped fluid] A method for forming a striped fluid according to one embodiment of the present invention is a method for forming a striped fluid in which two or more phases, each composed of two or more mutually incompatible fluids, are arranged alternately along the length of a flow channel, and the method alternately comprises an introduction step in which two or more fluids are introduced together into a flow channel to form a flow of the two or more fluids, and a formation step in which the flow rates of all of the two or more fluids in the flow channel are simultaneously reduced to less than the respective flow rates of the two or more fluids in the introduction step and greater than 0 mL / min, so as to form a striped fluid.

[0017] A striped fluid forming method M1 according to one embodiment of the present invention will be described below with reference to FIGS. 1 and 2. FIG. 1 is a flow diagram illustrating the process of the striped fluid forming method M1 according to one embodiment of the present invention. FIG. 2 is a schematic diagram illustrating the relationship between the change in flow rate over time and the state of the fluid in the flow channel 11 in the striped fluid forming method M1 according to one embodiment of the present invention. FIG. 2(a) is a graph illustrating the change in flow rate over time. FIG. 2(b) shows the state of the fluid in the flow channel 11 during the first introduction step S11 shown in FIG. 2(a). FIG. 2(c) shows the state of the fluid in the flow channel 11 during the first formation step S12 shown in FIG. 2(a). FIG. 2(d) shows the state of the fluid in the flow channel 11 during the next introduction step S11 shown in FIG. 2(a). FIG. 2(e) shows the state of the fluid in the flow channel 11 during the next formation step S12 shown in FIG. 2(a).

[0018] 1, the formation method M1 alternately repeats an introduction step S11 and a formation step S12. As will be described later, in the formation method M1, a striped fluid F is formed in the formation step S12, and then in the subsequent introduction step S11, the striped fluid F is made to flow faster through the flow path than in the formation step S12, thereby forming a slug flow.

[0019] [Introduction process] The introducing step S11 is a step of introducing two or more fluids that are incompatible with each other into the flow channel 11 together to form flows of the two or more fluids.

[0020] (fluid) In one embodiment of the present invention, the two or more fluids are not particularly limited as long as they are incompatible with each other. Furthermore, two fluids or three or more fluids may be used as the fluids. The two or more fluids are each independently a liquid or a gas.

[0021] As shown in FIG. 2(b), in this embodiment, the striped fluid F is composed of two fluids, a first fluid A and a second fluid B. While not limited thereto, the first fluid A may be water or an aqueous solution, and the second fluid may be a hydrophobic organic liquid. In this case, a liquid-liquid striped fluid F is formed in which the aqueous phase composed of the first fluid A and the organic phase composed of the second fluid B are arranged side by side.

[0022] Examples of aqueous solutions include aqueous hydrochloric acid, aqueous ammonium chloride, aqueous potassium hydrogen sulfate, aqueous citric acid, aqueous sodium thiosulfate, aqueous sodium hydrogen carbonate, aqueous sodium carbonate, aqueous potassium carbonate, aqueous sodium hydroxide, and aqueous sodium chloride. Examples of hydrophobic organic liquids include 4-methyltetrahydropyran (MTHP), cyclopentyl methyl ether (CPME), chloroform, dimethylformamide, dimethyl sulfoxide, diethyl ether, diisopropyl ether, tetrahydrofuran, 2-methyltetrahydrofuran, 1,4-dioxane, methyl t-butyl ether, ethyl acetate, isopropyl acetate, dichloromethane, toluene, xylene, hexane, heptane, and cyclohexane.

[0023] Alternatively, the two or more fluids may be a combination of a first fluid that is water or an aqueous solution, a second fluid that is a hydrophobic organic liquid, and a third fluid that is a gas, where examples of aqueous solutions and hydrophobic organic liquids are as described above, and examples of gases include nitrogen and carbon dioxide.

[0024] Furthermore, each of the two or more fluids may independently contain a solute, examples of which include peptides and surfactants.

[0025] (flow path) As shown in FIG. 2(b), in this embodiment, the flow path 11 is a cylindrical tubular flow path having an inner diameter D and a length L. However, in one aspect of the present invention, the flow path 11 is not limited to this, and may have any structure that prevents fluid from leaking from the flow path 11. The flow path 11 may be, for example, a tubular flow path whose peripheral side surface is completely covered, or a U-shaped flow path having an opening on the top surface. The cross section of the flow path 11 taken perpendicular to the length L direction may have any shape, such as a circle or a rectangle.

[0026] The inner diameter D of the flow path 11 can be selected appropriately depending on the purpose. The inner diameter D of the flow path 11 is preferably 0.8 mm or more, more preferably 1.0 mm or more. A larger inner diameter D within this range has the effect of improving the separation of two or more fluids in the recovery tank. Furthermore, the inner diameter D is preferably 8.0 mm or less, more preferably 4.5 mm or less. A smaller inner diameter D within this range has the effect of increasing the circulation speed of the fluid within the phases constituting the striped fluid F and increasing the material exchange between the phases. Note that when the cross section of the flow path 11 is non-circular, such as rectangular, it is preferable that the cross section of the flow path 11 has a cross-sectional area corresponding to a circle having an inner diameter D within the above-mentioned preferred range.

[0027] The inner diameter D of the flow path 11 may be adjusted as appropriate depending on the type of fluid, the material of the flow path 11, the performance of the pump that pumps the fluid, etc. For example, when a fluid that is prone to emulsion is used, it tends to take a long time to separate two or more fluids in the recovery tank, so it is preferable to set the inner diameter D larger.

[0028] The length L of the flow path 11 can be appropriately selected depending on the purpose. The length L of the flow path 11 is preferably 0.01 m or more, and more preferably 0.5 m or more. The longer the length L within this range, the greater the effect of increasing the mass transfer between two phases of the fluid. Furthermore, the length L is preferably 50 m or less, and more preferably 10 m or less. The shorter the length L within this range, the greater the effect of enabling accurate liquid transfer according to the set flow rate value without being affected by back pressure.

[0029] The length L of the flow path 11 may be adjusted as appropriate depending on the type of fluid, the material of the flow path 11, the performance of the pump that pumps the fluid, and the like.

[0030] In the present invention, the material of the flow channel 11 is not particularly limited. The material of the flow channel 11 can be appropriately selected from substances known in the art as materials for flow channels, and may be, for example, resin, glass, or metal. Examples of resins include perfluoroalkoxyalkane (PFA) resin and polytetrafluoroethylene (PTFE) resin.

[0031] (flow rate) As shown in FIG. 2(a), in the introduction step S11, a first fluid A is introduced into the flow path 11 at a flow rate VA, and a second fluid B is introduced into the flow path 11 at a flow rate VB. In this embodiment, the flow rates VA and VB are constant during the introduction step S11. However, one aspect of the present invention is not limited to this, and the flow rates VA and VB may be independently constant or variable during the introduction step S11. Also, in this embodiment, the flow rates VA and VB are equal to each other. However, one aspect of the present invention is not limited to this, and the flow rates VA and VB may be different from each other.

[0032] The total flow rate VA+VB of fluids A and B is preferably 0.1 mL / min or more, and more preferably 1.0 mL / min or more. Within this range, the larger the total flow rate VA+VB, the greater the effect of increasing the amount of processing per unit time. Furthermore, the total flow rate VA+VB is preferably 200 mL / min or less, and more preferably 100 mL / min or less. Within this range, the smaller the total flow rate VA+VB, the greater the effect of reducing the occurrence of emulsion in the striped fluid F. Note that when three or more fluids are used, it is preferable that the total flow rates of all of the three or more fluids be within the above range.

[0033] The total flow rate VA+VB of fluid A and fluid B in the introduction step S11 may be adjusted as appropriate depending on the type of fluid, the material of flow path 11, the performance of the pump that pumps the fluid, etc. For example, when glass is used as the material of flow path 11, a relatively large flow rate of striped fluid F tends to be more stably formed, so it is preferable to set the total flow rate VA+VB larger in order to form a slug flow with excellent throughput.

[0034] The ratio VA / VB of the flow rate VA to the flow rate VB is preferably 0.1 or more and 10 or less, more preferably 0.5 or more and 2.0 or less. When the ratio VA / VB is in this range, the effect of increasing the mass transfer between fluid A and fluid B is achieved. Furthermore, the ratio VA / VB may be constant or variable. If it is variable, it is preferable that the ratio VA / VB varies within the above range. Note that when three or more fluids are used, it is preferable that the ratio of the flow rates for each combination of any two of the three or more fluids is within the above range.

[0035] As will be described later, in the forming step S12, striped fluid F is formed in the flow path 11. Therefore, in the introducing step S11, fluids A and B may be introduced into the flow path together so that the newly introduced fluids A and B into the flow path 11 during the introducing step S11 do not form striped fluid F. The newly introduced fluids A and B into the flow path 11 in the introducing step S11 may form a flow other than a slug flow, such as a parallel flow, an annular flow, a droplet flow, or a dispersed flow.

[0036] An example of a condition under which fluids A and B newly introduced into flow path 11 do not form striped fluid F is a condition under which the total flow rate VA+VB of fluids A and B is greater than a certain reference value. In this embodiment, the smaller the total flow rate VA+VB, the more likely fluids A and B are to form striped fluid F. Therefore, if the above-mentioned reference value, which is the maximum value of the total flow rate VA+VB at which striped fluid F is formed, is called the "critical flow rate," then in the introduction step S11, fluids A and B may be introduced into flow path 11 at a total flow rate VA+VB that exceeds this critical flow rate. This can further improve the apparent flow rate of striped fluid F.

[0037] The critical flow rate may vary depending on the type of fluid and device, etc. Generally, whether or not striped fluid F is formed in flow path 11 can be easily determined by a known means such as visual inspection. Therefore, the critical flow rate can be easily determined by determining whether or not striped fluid F is formed in flow path 11 while changing the flow rates of fluids A and B.

[0038] (Duration of the introduction process) As shown in FIG. 2(a), in this embodiment, in the introduction step S11, two fluids A and B are introduced into the flow channel 11 for a duration T1. The duration T1 of the introduction step S11 is preferably 0.1 seconds or more, and more preferably 1.0 seconds or more. The longer the duration T1 within this range, the greater the effect of increasing the apparent flow rate of the striped fluid F. Furthermore, the duration T1 is preferably 20 seconds or less, and more preferably 5.0 seconds or less. The shorter the duration T1 within this range, the greater the effect of reducing the occurrence of emulsion within the striped fluid F.

[0039] The duration T1 of the introduction step S11 may be adjusted as appropriate depending on the type of fluid, the material of the flow path 11, the performance of the pump that pumps the fluid, etc. For example, when a fluid containing a solute that exhibits surface activity is used, emulsion tends to easily occur in the striped fluid F, so it is preferable to set the duration T1 to a longer time.

[0040] In this embodiment, the switching from the introducing step S11 to the forming step S12 is triggered by the lapse of duration T1. However, the present invention is not limited to this, and the switching may be performed according to the cumulative volume ratio of the two fluids A and B introduced into the flow path 11. That is, the forming step S12 may be performed after the cumulative volume ratio of the two fluids A and B introduced into the flow path 11 in the introducing step S11 reaches a predetermined value. By adopting such a configuration, the fluids A and B constituting the striped fluid F are maintained constant. Here, the cumulative volume ratio refers to the ratio between the cumulative volume of the first fluid A and the second fluid B introduced into the flow path 11 in one introducing step S11. The predetermined value may be, for example, within a range of 0.1 to 10.

[0041] [Formation process] The forming step S12 is a step of simultaneously reducing the flow rates of all of the two or more fluids in the flow channel 11 to less than the respective flow rates of the two or more fluids in the introducing step S11 and to more than 0 mL / min, so that a striped fluid F is formed.

[0042] (flow rate) The forming step S12 can be performed by an operation known in the art for reducing the flow rate of each of the fluids flowing through the flow path 11. For example, the forming step S12 may be performed by reducing the output of a pump that pumps each of the two or more fluids or by throttling a valve located upstream or downstream of the flow path 11. In this embodiment, the striped fluid F is formed by reducing the flow rate VA' of the first fluid VA below the flow rate VA in the introducing step S11 and by reducing the flow rate VB' of the second fluid B below the flow rate VB in the introducing step S11 so that the total flow rate VA'+VB' of the flow rate VA' of the first fluid A and the flow rate VB' of the second fluid B is equal to or less than the limit flow rate described above.

[0043] As shown in FIG. 2(a), in the forming step S12, the first fluid A is introduced into the flow path 11 at a flow rate VA', and the second fluid B is introduced into the flow path 11 at a flow rate VB'. In this embodiment, the flow rates VA' and VB' are constant during the forming step S12. However, one aspect of the present invention is not limited to this, and the flow rates VA' and VB' may be independently constant or variable during the forming step S12. Also, in this embodiment, the flow rates VA' and VB' are equal to each other. However, one aspect of the present invention is not limited to this, and the flow rates VA' and VB' may be different from each other. The flow rate VA' may be set appropriately as long as it is less than the flow rate VA and greater than 0 mL / min. Similarly, the flow rate VB' may be set appropriately as long as it is less than the flow rate VB and greater than 0 mL / min.

[0044] 2(a), in this embodiment, the ratio between the flow rates of the first fluid A and the second fluid B is constant throughout the introducing step S11 and the forming step S12, i.e., VA:VB = VA':VB' = 1:1. However, one aspect of the present invention is not limited to this, and the ratio in the introducing step S11 may be different from the ratio in the forming step S12. As an example, the flow rates VA' and VB' may be set so that the difference between the flow rates VA and VA' and the difference between the flow rates VB and VB' are both a predetermined reduction width VX.

[0045] The total flow rate VA'+VB' of fluids A and B in the forming step S12 is not particularly limited within the range in which the striped fluid F is formed, but is, for example, 0.1 mL / min or more, and as another example, 2 mL / min or more. Within this range, the larger the total flow rate VA'+VB', the greater the effect of increasing the processing volume per unit time. Furthermore, the total flow rate VA'+VB' is not particularly limited within the range in which the striped fluid F is formed, but is, for example, 40 mL / min or less, and as another example, 10 mL / min or less. Within this range, the smaller the total flow rate VA'+VB', the less the effect of reducing the occurrence of emulsion within the striped fluid F. When three or more fluids are used, it is preferable that the total flow rates of all of the three or more fluids be within the above range.

[0046] The total flow rate VA'+VB' of fluid A and fluid B may be adjusted as appropriate depending on the type of fluid, the material of flow path 11, the performance of the pump that pumps the fluid, etc. For example, when glass is used as the material of flow path 11, a relatively large flow rate of striped fluid F tends to form more stably, so it is preferable to set the total flow rate VA'+VB' larger in order to form a slug flow with excellent throughput.

[0047] (Duration of the formation process) As shown in FIG. 2(a), in this embodiment, during the formation step S12, the flow rates VA' and VB' of the two fluids A and B are simultaneously set to less than the flow rates VA and VB of the two fluids, respectively, during the introduction step S11 and greater than 0 mL / min for a duration T2. ​​The duration T2 of the formation step S12 is preferably 0.01 seconds or longer, and more preferably 1.0 seconds or longer. A longer duration T2 within this range provides the effect of more easily forming a more stable striped fluid F. Furthermore, the duration T2 is preferably 6.0 seconds or shorter, and more preferably 3.0 seconds or shorter. A shorter duration T2 within this range provides the effect of increasing the apparent flow rate of the striped fluid F, thereby increasing the throughput per unit time.

[0048] The duration T2 of the forming step S12 may be adjusted as appropriate depending on the type of fluid, the material of the flow path 11, the performance of the pump that pumps the fluid, etc. For example, when a highly viscous fluid is used, it tends to take a long time for the parallel flow to change form into the striped fluid F, so it is preferable to set the duration T2 to a longer time. As a specific example, when any of the two or more fluids is silicone oil, the duration T2 is preferably 2 seconds or more.

[0049] The duration T2 of the forming step S12 may be selected taking into consideration the ratio T2 / T1 to the duration T1 of the introducing step S11. For example, the ratio T2 / T1 is preferably equal to or less than 60, and more preferably equal to or less than 5. A smaller ratio T2 / T1 within this range has the effect of increasing the average flow rate through the forming method M1, i.e., the apparent flow rate of the striped fluid F.

[0050] [State of fluid during repeated introduction and formation processes] The state of the two fluids A and B in the flow channel 11 while the introducing step S11 and the forming step S12 are alternately and repeatedly performed will be described below with reference to FIGS. 2(b) to 2(e).

[0051] As shown in FIG. 2(b), in the first introduction step S11, a first fluid A is introduced at a flow rate VA and a second fluid B is introduced at a flow rate VB into the flow channel 11, thereby forming two flows of the fluids A and B. Here, the two fluids A and B join at a joining point (not shown) located upstream of the flow channel 11 before flowing into the flow channel 11. The two fluids A and B form parallel flows in the flow channel 11, perpendicular to the length L of the flow channel 11, which are stable against friction generated between the two fluids A and B and flow through the flow channel 11. The tendency of the two fluids A and B to form parallel flows becomes stronger as the flow rate VA of the first fluid A and the flow rate VB of the second fluid B increase.

[0052] 2(c), in the initial forming step S12, the first fluid A is introduced into the flow channel 11 at a flow rate VA' that is less than the flow rate VA in the introducing step S11 and greater than 0 mL / min, and the second fluid B is introduced into the flow channel 11 at a flow rate VB' that is less than the flow rate VB in the introducing step S11 and greater than 0 mL / min. As a result, the parallel flow formed in the initial introducing step S11 changes form into a striped fluid F in which a phase PA composed of the first fluid A and a phase PB composed of the second fluid B are alternately arranged along the length L of the flow channel 11.

[0053] As shown in Figure 2(d), in the next introduction step S11, the same operation as in the initial introduction step S11 is performed. As a result, the two fluids A and B newly flowing into the flow path 11 from the confluence form parallel flows, as in the initial introduction step S11. Meanwhile, the striped fluid F formed in the initial formation step S12 flows through the flow path 11 while maintaining the alignment of the phases PA and PB, forming a slug flow.

[0054] 2(e), in the next forming step S12, the same operation as in the first forming step S12 is performed, whereby the parallel flow formed in the next introducing step S11 is transformed into a new striped fluid F.

[0055] Generally, the formation of parallel flows has been considered undesirable for the purpose of forming a slug flow. However, as described above, in this embodiment, the formed parallel flows are transformed into striped fluid F in the forming step S12. Therefore, according to this embodiment, it is not necessary to suppress the flow rate of the fluid to avoid the formation of parallel flows, and a slug flow can be formed at a large flow rate. Furthermore, in this embodiment, two or more fluids are introduced into the flow channel 11 at the same time, so it is not necessary to limit the number of fluids introduced into the flow channel 11 to one at a time, and there is no need to control the valves at high speed. Therefore, according to this embodiment, a slug flow can be formed more easily.

[0056] [Modification] In this embodiment, the introducing step S11 is first performed, followed by the forming step S12, and then the introducing step S11 and the forming step S12 are alternately repeated. However, in one aspect of the present invention, the order of the steps is not limited to this, and for example, the forming step S12 may be first performed, followed by the introducing step S11, and then the forming step S12 and the introducing step S11 may be alternately repeated.

[0057] [Method of manufacturing chemical substances] The striped fluid formation method M1 according to one embodiment of the present invention can be used, for example, in a chemical manufacturing process. That is, a chemical manufacturing method according to one embodiment of the present invention includes processing a chemical or a precursor thereof using the striped fluid formation method M1 according to one embodiment of the present invention.

[0058] In one embodiment of the present invention, a chemical substance or its precursor is processed using a slug flow formed during the formation method M1. Examples of the purpose of the processing include, but are not limited to, heterogeneous reactions, extraction, and separation. The chemical substance production method may also be comprised of a multi-step reaction. Here, the target of processing using the striped fluid formation method M1 is not limited to the final product, i.e., the chemical substance to be produced, but may also be a precursor generated at the beginning or during the multi-step reaction.

[0059] The chemical substance to be produced is not particularly limited and can be selected from those known in the art, including, but not limited to, peptides.

[0060] In the production of peptides, a slug flow can be used to separate the peptides from by-products. In this case, an organic liquid containing the peptides and by-products as solutes and an aqueous solution for removing only the by-products into the aqueous solution can be used as fluids.

[0061] [Device for forming striped fluid] One embodiment of the striped fluid forming device of the present invention is a device that forms a striped fluid in which two or more phases, each composed of two or more mutually incompatible fluids, are arranged alternately along the length of a flow path, and the striped fluid forming device comprises two or more tanks that hold each of the two or more fluids, flow paths connected to the two or more tanks, a pump that pressurizes each of the two or more fluids into the flow paths, and a control unit.The control unit causes the striped fluid forming device to perform an introduction process in which the two or more fluids are introduced together into the flow path to form a flow of the two or more fluids, a formation process in which the flow rate of all of the two or more fluids in the flow path is simultaneously reduced to less than the flow rate of each of the two or more fluids in the introduction process and greater than 0 mL / min so as to form a striped fluid, and a process in which the striped fluid forming device alternately repeats the introduction process and the formation process.

[0062] An apparatus 100 for forming a striped fluid according to one embodiment of the present invention will be described below with reference to FIG. 3. FIG. 3 is a block diagram showing the configuration of the apparatus 100 for forming a striped fluid according to one embodiment of the present invention. The forming apparatus 100 can execute the above-described forming method M1, although it is not limited thereto. For ease of explanation, components having the same functions as those described above for forming method M1 will be denoted by the same reference numerals, and their description will not be repeated.

[0063] (Each component of the forming device) As shown in FIG. 3, the forming apparatus 100 includes a flow path 11, two tanks 12A and 12B, two pumps 13A and 13B, a confluence section 14, a recovery tank 15, and a control section 16.

[0064] Flow path 11 is a flow path that connects junction 14 and collection tank 15. As shown in Fig. 3, flow path 11 communicates with tanks 12A and 12B via junction 14 and pumps 13A and 13B, respectively. The configuration of flow path 11 is as described above in forming method M1, and the description thereof will not be repeated.

[0065] Two tanks 12A and 12B hold two mutually immiscible fluids A and B, respectively.

[0066] Pump 13A is in communication with tank 12A and junction 14, and pumps fluid A held in tank 12A to flow path 11 connected to junction 14. Similarly, pump 13B is in communication with tank 12B and junction 14, and pumps fluid B held in tank 12B to flow path 11 connected to junction 14.

[0067] Junction 14 is a three-branch pipe that communicates with pumps 13A and 13B and recovery tank 15. Flow path 11 is interposed between junction 14 and recovery tank 15. Examples of junction 14 include a T-shaped pipe, a Y-shaped pipe, a helix mixer, and a static mixer.

[0068] The recovery tank 15 is in communication with the confluence 14, and recovers and stores the striped fluid F that has flowed through the flow path 11 as a slug flow.

[0069] In this embodiment, the component provided downstream of the flow path 11 is not limited to the collection tank 15. For example, a settler may be provided downstream of the flow path 11. In this case, the settler may continuously separate and discharge two or more mutually incompatible fluids that have flowed into the settler from the flow path 11 as striped fluids. Alternatively, a collection tank 15 may be provided downstream of the settler, and the separated fluids may be collected by the collection tank 15. Alternatively, an optional external component may be provided downstream of the flow path 11, and the two or more fluids discharged from the flow path 11 may be discharged outside the forming apparatus 100.

[0070] The control unit 16 is communicatively connected to the pumps 13A and 13B. Note that the connection targets of the control unit 16 are not limited to the pumps 13A and 13B, but may be connected to each part of the forming apparatus 100 so that the forming apparatus 100 can perform the introduction process and the forming process described below. For example, the control unit 16 may be communicatively connected to a valve provided at any position in the flow path connecting the tanks 12A and 12B and the recovery tank 15. A processor such as a central processing unit (CPU), a micro processing unit (MPU), or a microcontroller can be used as the control unit 16.

[0071] In this embodiment, the forming apparatus 100 employs two fluids and includes the same number of tanks and pumps, i.e., two each. However, one aspect of the present invention is not limited to this. When three or more fluids are employed, the forming apparatus 100 may also be provided with three or more tanks and pumps. The number of pumps does not have to be the same as the number of fluids. For example, one pump may be provided to commonly pump two or more fluids. When three or more fluids are employed, the confluence may be a pipe having one more branch than the number of fluids, or a pipe connecting two or more three-branch pipes.

[0072] (Processing of control unit) The control unit 16 causes the forming apparatus 100 to perform an introduction process (introduction step S11) and a formation process (formation step S12). The introduction process is a process of performing the above-mentioned introduction step S11, and the formation process is a process of performing the above-mentioned formation step S12. The control unit 16 also causes the forming apparatus 100 to perform a process of causing the forming apparatus 100 itself to alternately and repeatedly perform the introduction process and the formation process. As a result, the forming apparatus 100 alternately and repeatedly performs the introduction step S11 and the formation step S12.

[0073] Each process that the control unit 16 causes the forming apparatus 100 to execute is realized by the control unit 16 sending a command signal to the pumps 13A and 13B. Specifically, the control unit 16 sends a command signal to the pumps 13A and 13B to adjust the amount of fluid to be pumped at a flow rate and duration according to the introduction step S11 and the forming step S12. The pumps 13A and 13B receive the command signal and pump the fluids A and B into the flow path 11 by referring to the flow rate and duration included in the command signal.

[0074] As a modified example, when the control unit 16 is communicatively connected to the valve, each process that the control unit 16 causes the forming apparatus 100 to execute is realized by the control unit 16 sending a command signal to the valve. Specifically, the control unit 16 sends a command signal to the valve to adjust the degree of opening or closing so as to achieve the flow rate and duration in accordance with the introduction step S11 and the forming step S12. The valve receives the command signal and adjusts the degree of opening or closing by referring to the degree of opening or closing included in the command signal.

[0075] 〔summary〕 As can be understood from the above description, the present invention includes the following aspects.

[0076] Aspect 1: A method for forming a striped fluid in which two or more phases, each of which is composed of two or more mutually incompatible fluids, are arranged alternately along the length of a flow channel, the method comprising alternately repeating an introduction step in which the two or more fluids are introduced together into the flow channel to form a flow of the two or more fluids, and a formation step in which the flow rates of all of the two or more fluids in the flow channel are simultaneously reduced to less than the flow rates of each of the two or more fluids in the introduction step and greater than 0 mL / min, so as to form the striped fluid.

[0077] Aspect 2: The method for forming striped fluids according to Aspect 1, wherein the forming step is carried out after the cumulative volume ratio of the two or more fluids introduced into the flow channel in the introducing step reaches a predetermined value.

[0078] Aspect 3: The method for forming fluid stripes of Aspect 1 or 2, wherein the two or more fluids are a combination of a first fluid that is water or an aqueous solution and a second fluid that is a hydrophobic organic liquid.

[0079] Aspect 4: The method for forming striped fluids of Aspect 1 or 2, wherein the two or more fluids are a combination of a first fluid that is water or an aqueous solution, a second fluid that is a hydrophobic organic liquid, and a third fluid that is a gas.

[0080] Aspect 5: A method for producing a chemical substance, comprising treating the chemical substance or a precursor thereof using the method for forming a striped fluid according to any one of Aspects 1 to 4.

[0081] Aspect 6: An apparatus for forming a striped fluid in which two or more phases, each of which is composed of two or more mutually incompatible fluids, are arranged alternately along the length of a flow path, the apparatus comprising: two or more tanks for holding each of the two or more fluids; flow paths connected to the two or more tanks; a pump for pressurizing each of the two or more fluids into the flow paths; and a control unit, wherein the control unit causes the apparatus for forming a striped fluid to perform an introduction process for introducing the two or more fluids together into the flow paths to form a flow of the two or more fluids; a formation process for simultaneously adjusting the flow rates of all of the two or more fluids in the flow paths to be less than the flow rates of each of the two or more fluids in the introduction process and greater than 0 mL / min so as to form the striped fluid; and a process for causing the apparatus for forming a striped fluid to alternately and repeatedly perform the introduction process and the formation process.

[0082] [Additional Notes] The present invention is not limited to the above-described embodiments, and various modifications are possible within the scope of the claims. Embodiments obtained by appropriately combining the technical means disclosed in different embodiments are also included in the technical scope of the present invention. [Example]

[0083] An example of the present invention will be described below: In this example, two or more fluids were introduced into a channel under various conditions to verify the formation of striped fluids.

[0084] Example 1 The same forming apparatus as shown in FIG. 3 was assembled using the following equipment. Pump: Diaphragm pump "QI-100-TT-PS" (Takumina) Confluence: T-pipe PFA union tee "PFA-220-3" (outer diameter 1 / 8 inch, Swagelok) Flow path: PFA tube (inner diameter 1.59 mm, length 2 m, Furon Industries Co., Ltd.)

[0085] 4-Methyltetrahydropyran (MTHP) was used as the first fluid A, and water was used as the second fluid B. Two pumps, one for each of fluids A and B, were used to pump first fluid A at a flow rate of 10 mL / min and second fluid B at a flow rate of 10 mL / min for 1 second (introduction step), followed by pumping first fluid A at a flow rate of 1 mL / min and second fluid B at a flow rate of 1 mL / min for 1 second (forming step). The flow channel was videotaped during operation, and visual inspection was performed to determine whether striped fluids were formed in the flow channel during the forming step. If striped fluids were formed, the lengths of each of the phases constituting the striped fluid along the length of the flow channel were measured. The results are shown in Table 3.

[0086] Examples 2 to 20 Examples 2 to 20 were carried out in the same manner as Example 1, except that the type of fluid, the apparatus, and the operating conditions of the pump were changed as shown in Tables 1 and 2. In Example 19, MTHP containing Rheodol TW-0120V at a concentration of 0.1 M as the solute was used as Fluid A. The results are shown in Table 3.

[0087] [Comparative Examples 1-2, 4-8, Reference Examples 1-2] Comparative Examples 1-2, 4-8, and Reference Examples 1-2 were carried out in the same manner as in Example 1, except that all fluids were continuously pumped at a constant flow rate and that the types of fluids and the operating conditions of the apparatus and pumps were changed as shown in Tables 1 and 2. In Comparative Example 7, MTHP containing 0.1 M Rheodol TW-0120V as the solute was used as Fluid A. The results are shown in Table 3.

[0088] Comparative Example 3 Comparative Example 3 was carried out in the same manner as Example 1, except that the type of fluid, the apparatus, and the operating conditions of the pump were changed as shown in Tables 1 and 2. The results are shown in Table 3.

[0089] [Table 1]

[0090] [Table 2]

[0091] [Table 3]

[0092] 〔result〕 (Reference examples 1~2) As can be seen from the results of Reference Example 1, when the total flow rate in the introduction step was relatively small, striped fluid was formed without the formation step. However, because the apparent flow rate was relatively small, it is expected that the processing volume of the striped fluid in Reference Example 1 was small. Furthermore, as can be seen from the results of Reference Example 2, when glass was used as the flow path material, striped fluid was formed without the formation step even at a larger total flow rate compared to the case of PFA.

[0093] (Comparative Examples 1-2, 4-8) As can be seen from the results of Comparative Examples 1 to 2, 4 to 8 and Reference Example 1, it was confirmed that the greater the total flow rate in the introducing step, the less likely striped fluid was formed without the forming step.

[0094] (Examples 1 to 20) As can be seen from the results of Examples 1 to 20 and Comparative Examples 1 to 2 and 4 to 8, even when the total flow rate of the introduction step was comparable to that of Comparative Examples 1 to 8, a striped fluid was formed by performing the formation step. Furthermore, in Examples 1 to 20, the time (T1 + T2) for one cycle of the introduction and formation steps was short, ranging from 1.5 to 6 seconds, and the phase length was short, ranging from 0.3 to 5.0 cm. The technology of Cited Document 1 requires valve control in a shorter cycle to achieve comparable phase lengths, which tends to complicate the device structure. Therefore, in order to form a slug flow with a certain phase length, the present invention can be said to enable the formation of the slug flow more easily with a simpler device structure.

[0095] As can be seen from a comparison between Examples 2, 4, 6-10 and Comparative Example 3, striped fluids were formed by lowering the flow rates of fluids A and B in the forming step to a certain reference value (critical flow rate) lower than the flow rate in the introducing step or exceeding 0 mL / min. As can be seen from the above comparison and the results of Reference Example 2, the critical flow rate varies depending on the type of fluid and device. Generally, whether striped fluids are formed can be easily determined by known means, such as visual inspection. Therefore, it can be said that the critical flow rate can be easily determined by determining whether striped fluids are formed while changing the flow rates of fluids A and B in the forming step within a range of less than the flow rate in the introducing step and exceeding 0 mL / min. Furthermore, in one embodiment of the present invention, striped fluids can be formed by setting the flow rate of fluid B in the forming step to a value equal to or less than the determined critical flow rate or exceeding 0 mL / min. Furthermore, based on the results of Example 20, these points also apply when three or more fluids are used.

[0096] As can be seen from the results of Example 1 and Reference Example 1, even though the apparent flow rate was almost the same, the formation process enabled the formation of striped fluids with shorter phase lengths. The shorter the phase length, the larger the contact area between the fluids, so it is expected that the effect of treatment using slug flow will be greater according to the present invention.

[0097] As can be seen from the results of Example 3 and Comparative Example 2, even when the apparent flow rate was large enough that striped fluid would not be formed without the formation step, striped fluid was formed by performing the formation step. Therefore, it can be said that the present invention can increase the throughput by treatment using slug flow.

[0098] As can be seen from the results of Examples 7 to 10, even if the total flow rate of the introduction step is the same, the apparent flow rate can be adjusted by adjusting the duration T1 of the introduction step and the duration T2 of the formation step. Therefore, according to the present invention, it is possible to suitably adjust the residence time of the fluid in the flow path, and therefore it can be said that the desired degree of processing can be achieved.

[0099] As can be seen from the results of Comparative Example 7, when the fluid contains a solute, striped fluid tends to be difficult to form. However, as can be seen from the results of Example 19 and Comparative Example 7, by carrying out the forming process, striped fluid was formed even when a fluid containing a solute was used. Therefore, it can be said that according to the present invention, slug flow formation is possible for a wider variety of fluids.

[0100] Even in Example 3, where the total flow rate in the introduction step was the largest, the striped fluid once formed flowed as a slug flow without changing into a parallel flow even in the introduction step. Therefore, it can be said that the present invention can realize a slug flow with a larger apparent flow rate. [Industrial Applicability]

[0101] The present invention can be used in the production of chemical substances, etc. [Explanation of symbols]

[0102] 11 Flow path 12A, 12B tank 13A, 13B Pump 16 Control Unit 100 Forming device

Claims

1. A method for forming a striped fluid in which two or more phases each composed of two or more mutually immiscible fluids alternate along the length of a flow channel, comprising: an introducing step of introducing the two or more fluids together into the flow path to form flows of the two or more fluids; a forming step of simultaneously setting the flow rates of all of the two or more fluids in the flow path to less than the flow rates of each of the two or more fluids in the introducing step and greater than 0 mL / min so that the striped fluid is formed; A method for forming striped fluids by repeating the above steps alternately.

2. the forming step is performed after an integrated volume ratio of the two or more fluids introduced into the flow path in the introducing step reaches a predetermined value. The method for forming fluid stripes according to claim 1 .

3. The two or more fluids are a combination of a first fluid that is water or an aqueous solution and a second fluid that is a hydrophobic organic liquid. The method for forming fluid stripes according to claim 1 .

4. The two or more fluids are a combination of a first fluid that is water or an aqueous solution, a second fluid that is a hydrophobic organic liquid, and a third fluid that is a gas. The method for forming fluid stripes according to claim 1 .

5. The method for forming a striped fluid according to any one of claims 1 to 4 includes treating a chemical substance or a precursor thereof. Chemical manufacturing methods.

6. An apparatus for forming striped fluids in which two or more phases each composed of two or more mutually immiscible fluids alternate along the length of a flow path, comprising: two or more tanks for holding the two or more fluids, respectively; a flow path communicating with the two or more tanks; a pump that pumps each of the two or more fluids into the flow path; A striped fluid forming device comprising: The control unit may be configured to: an introduction process for introducing the two or more fluids together into the flow path to form a flow of the two or more fluids; a forming process in which the flow rates of all of the two or more fluids in the flow path are simultaneously set to less than the flow rates of each of the two or more fluids in the introducing process and greater than 0 mL / min so that the striped fluid is formed; causing the striped fluid forming device to alternately and repeatedly perform the introducing process and the forming process; Fluid stripe forming device.

Citation Information

Patent Citations

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