Method for forming striped fluid, method for producing chemical substance, and device for forming striped fluid

Abstract

In order to provide a technique capable of more easily forming a slug flow, one aspect of the present invention provides a method (M1) for forming a striped fluid in which two or more phases, each of which is composed of two or more fluids that are immiscible with each other, are alternately arranged in the longitudinal direction of a flow path, the method includes alternately repeating an introduction step (S11) in which a flow of the two or more fluids is formed by introducing the two or more fluids into the flow path together, and a formation step (S12) in which a flow of the two or more fluids is formed by introducing the two or more fluids into the flow path together. In the forming step (S12), the flow rate of some of the two or more fluids in the flow path is substantially kept constant while maintaining the flow rate in the introduction step, and at the same time, in order to form the stripe-shaped fluid, the flow rate of some of the two or more fluids in the flow path is kept substantially constant. In this way, the flow rate of the other fluid among the two or more fluids is lower than the flow rate in the introduction step or substantially 0 mL / min.

Description

Technical Field

[0001] The present invention relates to a method for forming a stripe-shaped fluid, a method for preparing a chemical substance, and a device for forming a stripe-shaped fluid. Background Art

[0002] In the preparation process of chemical substances, slug flow, in which two or more phases flow alternately along the length of a flow path, is sometimes used for the purpose of heterogeneous reaction, extraction, and separation. As a technology for generating slug flow, for example, Patent Document 1 describes a slug flow generating device comprising: a fluid storage portion for storing a plurality of fluids; a pump for continuously pumping the plurality of fluids; a flow path connecting the plurality of fluid storage portions to the pumps and the pumps to a fluid confluence; and a slug flow generating flow path disposed downstream of the fluid confluence. Valves are provided in the flow path between the fluid confluence and the pump, and the valves are used to control the flow so that one fluid is continuously pumped into the fluid confluence while the other fluids are discharged into a discharge flow path.

[0003] Prior art literature

[0004] Patent Literature

[0005] Patent Document 1: Japanese Patent Application Laid-Open No. 2023-13422 Summary of the Invention

[0006] Problems to be solved by the invention

[0007] The technology described in Patent Document 1 can form a slug flow with a large flow rate, but on the other hand, it has a problem that a complex device structure is essential.

[0008] An object of one aspect of the present invention is to provide a technique that can more easily form a slug flow.

[0009] Means used to solve problems

[0010] In order to solve the above problems, one aspect of the present invention involves a method for forming a striped fluid as described below: a method for forming a striped fluid, which is used to form a striped fluid formed by alternating two or more phases composed of two or more mutually immiscible fluids along the length direction of the flow path, the method alternately and repeatedly implementing an introduction process and a formation process, in which the introduction process is performed by introducing the two or more fluids into the flow path together, thereby forming a flow of the two or more fluids; in the formation process, the flow rate of a part of the two or more fluids in the flow path is maintained at a substantially constant flow rate in the introduction process, and at the same time, in order to form the striped fluid, the flow rate of other fluids in the two or more fluids is made lower than the flow rate in the introduction process or is substantially 0 mL / min.

[0011] To solve the above-mentioned problems, an apparatus for forming a streak-like fluid according to one aspect of the present invention is as follows: a apparatus for forming a streak-like fluid, for forming a streak-like fluid in which two or more phases, respectively composed of two or more mutually immiscible fluids, are alternately arranged along the longitudinal direction of a flow path, the apparatus comprising: two or more containers for storing the two or more fluids; a flow path communicating with the two or more containers; a pump for pressurizing the two or more fluids into the flow path; and a control unit; wherein the control unit is configured to cause the apparatus for forming the streak-like fluid to perform an introduction process, a formation process, and a process for causing the apparatus for forming the streak-like fluid to alternately repeat the introduction process and the formation process, wherein the introduction process causes the two or more fluids to be introduced into the flow path together to form a flow of the two or more fluids; and the formation process causes the flow rate of some of the two or more fluids in the flow path to be maintained substantially constant at the flow rate in the introduction process, while at the same time causing the flow rate of the other of the two or more fluids to be lower than the flow rate in the introduction process or to be substantially 0 mL / min, in order to form the streak-like fluid.

[0012] Effects of the Invention

[0013] According to one aspect of the present invention, slug flow can be formed more easily. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 This is a flowchart showing the flow of a method for forming a streak-shaped fluid according to one embodiment of the present invention.

[0015] Figure 2 Schematic diagrams showing the relationship between the temporal change in flow rate and the state of the fluid in the flow path in a method for forming a striped fluid according to one embodiment of the present invention. (a) is a diagram showing the temporal change in flow rate. (b) shows the state of the fluid in the flow path during the first introduction step shown in (a). (c) shows the state of the fluid in the flow path during the first formation step shown in (a). (d) shows the state of the fluid in the flow path during the next introduction step shown in (a). (e) shows the state of the fluid in the flow path during the next formation step shown in (a).

[0016] Figure 3 This is a block diagram showing the configuration of a device for forming a streak-shaped fluid according to one embodiment of the present invention. DETAILED DESCRIPTION

[0017] [Concept of the Invention]

[0018] When utilizing slug flow in industrial applications, in order to increase the amount of chemical substances processed, a large flow rate of slug flow is often desired. The formation of a large flow rate of slug flow usually requires increasing the flow rate of each of the two or more fluids forming the slug flow. However, if the flow rate of the two or more fluids is increased, the dynamic control of the two or more fluids in the confluence will become difficult. Specifically, if two or more fluids are introduced into the confluence at the same time, the fluid discharged from the confluence will form a slug flow in the flow path located downstream of the confluence immediately after the introduction begins. However, if the fluid temporarily forms a parallel flow in the confluence due to unstable dynamics, then when it is discharged from the confluence, the parallel flow state will be maintained and stabilized. To avoid this situation, in the technology of Patent Document 1, a valve located upstream of the confluence is switched at high speed so that only one fluid is introduced into the confluence. However, for high-speed control of the valve, a complex device structure is essential.

[0019] The inventors have discovered that even if a fluid temporarily forms parallel flows, as long as the flow rate of a portion of the fluid is kept constant while the flow rate of the other fluid is reduced, the overall fluid flow in the flow path will undergo a morphological change from parallel flow to striped flow. Furthermore, they have discovered that even if the flow rate of the other fluid is increased to its original flow rate, the striped fluid temporarily formed in the flow path will not easily revert to parallel flow, but will instead form a slug flow and flow. It is speculated that these phenomena are caused by the following principle: friction is generated between the temporarily formed parallel flow in the confluence and the inner wall, and this friction is particularly large at the boundary between the phases formed by the two fluids. Therefore, in order to prevent the phase boundary from forming in the portion of the fluid that contacts the inner wall, the fluid stabilizes in a parallel flow state. On the other hand, when the flow rate of the other fluid is reduced, thereby reducing the overall flow rate of the fluid, the friction decreases, and the surface tension that acts to minimize the contact area between the two fluids becomes dominant over friction, causing the parallel flow to undergo a morphological change to striped flow. Moreover, as a streak-like fluid temporarily formed in the flow path, once the flow rate is increased to the original flow rate, the friction it encounters will increase again. However, unlike the confluence section in an unstable state, the pressure applied unilaterally along the flow direction in the flow path dominates the friction, so that the streak-like fluid does not undergo morphological changes, but instead forms a slug flow and flows.

[0020] As mentioned above, to achieve high-flow slug flow, it is generally necessary to investigate how to increase the flow rates of the two or more fluids forming the slug flow. However, the present inventors have shifted their approach and discovered that by maintaining the flow rates of some fluids constant while reducing the flow rates of others, a streak-like flow pattern, one aspect of which includes slug flow, can be formed. This has led to the completion of the present invention.

[0021] 〔Striation-like fluid〕

[0022] In this specification, a striped fluid refers to a fluid in which two or more phases composed of two or more mutually immiscible fluids are arranged alternately along the length direction of the flow path. For example, a fluid in which phase PA composed of a first fluid A and phase PB composed of a second fluid B are arranged in the order of PA, PB, PA, PB, ... is a striped fluid. The number of fluids constituting a striped fluid may also be three or more. For example, a fluid in which phase PA composed of a first fluid A, phase PB composed of a second fluid B, and phase PC composed of a third fluid C are arranged in the order of PA, PB, PC, PA, PB, PC, ... is a striped fluid. In a striped fluid, as long as adjacent phases are not composed of the same fluid, the order of arrangement of the phases is not limited. For example, a fluid in which phases are arranged in an irregular order such as PA, PB, PA, PC, PB, PA, ... is also a striped fluid.

[0023] Furthermore, each of the two or more fluids need only be incompatible with at least one of the other fluids. For example, the fluids may include an aqueous solution A, an aqueous solution B that is compatible with aqueous solution A, and an organic solvent C that is incompatible with both aqueous solution A and aqueous solution B. In this case, a striped fluid comprising a phase PAB composed of a mixture of aqueous solution A and aqueous solution B and a phase PC composed of organic solvent C can be formed.

[0024] The "striated fluid" may be in a state of flowing in the flow path or in a state of not flowing in the flow path and being stopped. In this specification, the streak-shaped fluid in a state of flowing in the flow path may be referred to as a "slug flow".

[0025] [Method for forming a streak-like fluid]

[0026] An aspect of the present invention relates to a method for forming a striped fluid as described below: a method for forming a striped fluid, which is used to form a striped fluid formed by alternating two or more phases composed of two or more mutually immiscible fluids along the length direction of a flow path, wherein the method alternately and repeatedly implements an introduction process and a formation process, wherein in the introduction process, the flow of two or more fluids is formed by introducing the two or more fluids into the flow path together; in the formation process, the flow rate of a part of the two or more fluids in the flow path is maintained at a substantially constant flow rate in the introduction process, and at the same time, in order to form a striped fluid, the flow rate of other fluids in the two or more fluids is made lower than the flow rate in the introduction process or is substantially 0 mL / min.

[0027] Below, we will refer to Figure 1 and Figure 2 A method M1 for forming a streak-shaped fluid according to one embodiment of the present invention will be described. Figure 1This is a flowchart showing the flow of a method M1 for forming a streak-shaped fluid according to one embodiment of the present invention. Figure 2 Schematic diagram showing the relationship between the temporal change in flow rate and the state of the fluid in the flow path 11 in the method M1 for forming a streak-shaped fluid according to one embodiment of the present invention. Figure 2 (a) is a graph showing the temporal change of flow rate. Figure 2 (b) means Figure 2 (a) shows the state of the fluid in the flow path 11 during the initial introduction step S11. Figure 2 (c) means Figure 2 (a) shows the state of the fluid in the flow path 11 during the initial forming step S12. Figure 2 (d) means Figure 2 (a) shows the state of the fluid in the flow path 11 during the next introduction step S11. Figure 2 (e) means Figure 2 (a) shows the state of the fluid in the flow path 11 during the next forming step S12.

[0028] like Figure 1 As shown, the formation method M1 alternately repeats the introduction step S11 and the formation step S12. As described below, in the formation method M1, a streak-shaped fluid F is formed in the formation step S12. In the subsequent introduction step S11, the streak-shaped fluid F is made to flow faster in the flow path than in the formation step S12, thereby forming a slug flow.

[0029] 〔Introduction process〕

[0030] The introduction step S11 is a step of introducing two or more mutually immiscible fluids into the flow path 11 together to form a flow of the two or more fluids.

[0031] (fluid)

[0032] In one aspect of the present invention, the two or more fluids are not particularly limited as long as they are immiscible with each other. In addition, the fluids may be two fluids or three or more fluids. The two or more fluids are each independently liquid or gas.

[0033] like Figure 2 As shown in Figure (b), in this embodiment, the number of fluids constituting the striped fluid F is two, and the two fluids are a combination of a first fluid A and a second fluid B. Without limitation, the first fluid A can be water or an aqueous solution, and the second fluid can be a hydrophobic organic liquid. In this case, a liquid-liquid striped fluid F is formed, with the aqueous phase consisting of the first fluid A and the organic phase consisting of the second fluid B arranged in an arrangement.

[0034] Examples of aqueous solutions include aqueous hydrochloric acid, ammonium chloride, potassium hydrogensulfate, citric acid, sodium thiosulfate, sodium hydrogencarbonate, sodium carbonate, potassium carbonate, sodium hydroxide, and 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-tert-butyl ether, ethyl acetate, isopropyl acetate, dichloromethane, toluene, xylene, hexane, heptane, and cyclohexane.

[0035] As a variation, the two or more fluids may be a combination of a first fluid, a second fluid, and a third fluid, wherein the first fluid is water or an aqueous solution, the second fluid is a hydrophobic organic liquid, and the third fluid is a gas. Examples of aqueous solutions and hydrophobic organic liquids are as described above. Examples of gases include nitrogen and carbon dioxide.

[0036] Furthermore, two or more fluids may each independently contain a solute. Examples of solutes include peptides and surfactants.

[0037] (Flow path)

[0038] like Figure 2 As shown in (b), in this embodiment, the flow path 11 is a cylindrical tube-type flow path having an inner diameter D and a length L. In one aspect of the present invention, the flow path 11 is not limited thereto, as long as it has a structure that prevents fluid from leaking from the flow path 11. The flow path 11 may be, for example, a tubular flow path with completely covered circumferential sides, or a U-shaped flow path with an opening on the upper surface. The cross-section obtained by cutting the flow path 11 in a direction perpendicular to the length L may be of any shape, for example, circular or rectangular.

[0039] The inner diameter D of the flow path 11 can be appropriately selected according to the purpose. The inner diameter D of the flow path 11 is preferably more than 0.8 mm, more preferably more than 1.0 mm. Within this range, the larger the inner diameter D is, the more it can improve the separation of two or more fluids in the recovery container. In addition, the inner diameter D is preferably less than 8.0 mm, more preferably less than 4.5 mm. Within this range, the smaller the inner diameter D is, the more it can accelerate the circulation speed of the fluid in the phase constituting the striped fluid F and increase the material exchange between the phases. In addition, when the cross section of the flow path 11 is a non-circular shape such as a rectangle, preferably, the cross section of the flow path 11 has a cross-sectional area equivalent to a circle, and the circle refers to a circle with an inner diameter D within the above-mentioned preferred range.

[0040] The inner diameter D of the flow path 11 can be appropriately adjusted depending on the type of fluid, the material of the flow path 11, the performance of the pump that pressurizes the fluid, etc. For example, when the fluid being used is prone to forming an emulsion, it tends to take time to separate two or more fluids in the recovery container, so it is preferable to set the inner diameter D larger.

[0041] The length L of the flow path 11 can be appropriately selected depending on the intended purpose. The length L of the flow path 11 is preferably 0.01 m or greater, more preferably 0.5 m or greater. Within this range, a greater length L further enhances the transfer of substances between the two phases of the fluid. Furthermore, the length L is preferably 50 m or less, more preferably 10 m or less. Within this range, a smaller length L further enhances the ability to accurately deliver liquid at the set flow rate without being affected by back pressure.

[0042] The length L of the flow path 11 can be adjusted as appropriate depending on the type of fluid, the material of the flow path 11 , the performance of a pump that pumps the fluid, and the like.

[0043] In the present invention, the material of the flow path 11 is not particularly limited. The material of the flow path 11 can be appropriately selected from substances known in the art as flow path materials, such as resin, glass, or metal. Examples of resins include perfluoroalkoxyalkane (PFA) resin and polytetrafluoroethylene (PTFE) resin.

[0044] (flow)

[0045] like Figure 2 As shown in (a), in the introduction process S11, 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, during the introduction process S11, the flow rates VA and VB are constant. However, one aspect of the present invention is not limited to this, and during the introduction process S11, the flow rates VA and VB may also be independently constant or variable. In addition, in this embodiment, the flow rate VA is smaller than the flow rate VB. However, one aspect of the present invention is not limited to this, and the size relationship between the flow rates VA and VB may be appropriately set. For example, the flow rate VA may be equal to the flow rate VB, or may be larger than the flow rate VB.

[0046] The total flow rate VA + VB of fluids A and B is preferably 0.1 mL / min or greater, more preferably 1.0 mL / min or greater. Within this range, a greater total flow rate VA + VB increases the hourly throughput. Furthermore, the total flow rate VA + VB is preferably 200 mL / min or less, more preferably 100 mL / min or less. Within this range, a smaller total flow rate VA + VB reduces the formation of emulsions within the streak-shaped fluid F. Furthermore, when using three or more fluids, the total flow rate of these three or more fluids is preferably within the above range.

[0047] The total flow rate VA + VB of fluids A and B introduced into step S11 can be appropriately adjusted depending on the type of fluid, the material of flow path 11, the performance of the pump that pumps the fluids, and the like. For example, when glass is used as the material of flow path 11, streaked fluid F tends to be more stably formed at a larger flow rate. Therefore, in order to form a slug flow with excellent throughput, the total flow rate VA + VB is preferably set to a larger value.

[0048] The ratio VA / VB of the flow rate VA to the flow rate VB is preferably 0.02 or greater and 5.0 or less, more preferably 0.05 or greater and 2.0 or less. When the ratio VA / VB is within this range, the transfer of substances between fluids A and B is increased. Furthermore, the ratio VA / VB can be constant or variable. When variable, the ratio VA / VB preferably varies within the aforementioned range. Furthermore, when using three or more fluids, the flow rate ratio for any combination of two of the three or more fluids is preferably within the aforementioned range.

[0049] As described below, in the forming step S12, streaks of fluid F are formed in the flow channel 11. Therefore, in the introduction step S11, in order to prevent the fluids A and B newly introduced into the flow channel 11 during the introduction step S11 from forming streaks of fluid F, the fluids A and B may be introduced into the flow channel together. The fluids A and B newly introduced into the flow channel 11 in the introduction 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.

[0050] One example of a condition for preventing the newly introduced fluids A and B into the flow channel 11 from forming streaks of fluid F is that 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 streaks of fluid F. Therefore, if the reference value, or the maximum flow rate of the total flow rate VA + VB that can form streaks of fluid F, is referred to as the "limiting flow rate," then in the introduction step S11, fluids A and B can be introduced into the flow channel 11 at a total flow rate VA + VB exceeding this limit. This can further increase the apparent flow rate of the streaks of fluid F.

[0051] The limiting flow rate can vary depending on the type of fluid and device, etc. Here, in general, whether streaks of fluid F are formed in the flow path 11 can be easily determined by known means such as visual inspection. Therefore, by varying the flow rates of fluids A and B and determining whether streaks of fluid F are formed in the flow path 11, the limiting flow rate can be easily determined.

[0052] (Duration of the introduction process)

[0053] like Figure 2 As shown in FIG. 1 (a), in this embodiment, in the introduction step S11, two fluids A and B are introduced into the flow path 11 for a duration T1. The duration T1 of the introduction step S11 is preferably 0.1 seconds or longer, more preferably 1.0 seconds or longer. Within this range, the longer the duration T1, the more effective it is to increase the apparent flow rate of the streak-shaped fluid F. Furthermore, the duration T1 is preferably 20 seconds or shorter, more preferably 5.0 seconds or shorter. Within this range, the shorter the duration T1, the more effective it is to reduce the formation of emulsions in the streak-shaped fluid F.

[0054] The duration T1 of the introduction step S11 can be appropriately adjusted depending on the type of fluid, the material of the flow path 11, the performance of the pump that pressurizes the fluid, etc. For example, when the fluid used contains a solute that exhibits surfactant, an emulsion tends to form in the streak-shaped fluid F, and therefore, the duration T1 is preferably set to a shorter time.

[0055] In the present embodiment, the switching from the introduction process S11 to the formation process S12 is implemented mainly due to the passage of duration T1. However, the present invention is not limited to this, and the switching may be implemented based on the cumulative volume ratio of the two fluids A and B introduced into the flow path 11. That is, the formation process S12 may be implemented after the cumulative volume ratio of the two fluids A and B introduced into the flow path 11 in the introduction process S11 reaches a predetermined value. By adopting such a configuration, the effect of maintaining the fluids A and B constituting the stripe-shaped fluid F constant is achieved. Here, the cumulative volume ratio refers to the ratio of the cumulative volume of the first fluid A introduced into the flow path 11 in a single introduction process S11 to the cumulative volume of the second fluid B. As a predetermined value, for example, it may be in the range of not less than 0.1 and not more than 10.

[0056] [Formation process]

[0057] The forming process S12 is a process as described below: the flow rate of a part of the two or more fluids in the flow path 11 is maintained at the flow rate in the introduction process S11 and remains substantially constant. At the same time, in order to form a striped fluid F, the flow rate of other fluids in the two or more fluids is made lower than the flow rate in the introduction process S11 or is substantially 0 mL / min.

[0058] In this specification, "maintaining the flow rate of the fluid substantially constant" refers to performing an operation known in the art for maintaining a constant amount of fluid introduced into the flow path 11, and therefore does not mean strictly maintaining the flow rate of the fluid constant. As an example, for a pump that pressurizes the fluid, although the output of the pump in the introduction step S11 is maintained and the pump operates continuously, the amount of the fluid introduced into the flow path 11 changes due to the pulsation of the pump. In this case, the flow rate of the fluid can be considered to be substantially constant. For example, without limitation, if the ratio of the flow rate of the fluid in the formation step S12 to the flow rate of the fluid in the introduction step S11 is greater than 95% and less than 105%, this case falls within the scope of "maintaining the flow rate of the fluid substantially constant."

[0059] In this specification, "making the flow rate of the fluid substantially 0 mL / min" means performing an operation known in the art for stopping the introduction of the fluid into the flow path 11, and therefore does not mean strictly making the flow rate of the fluid 0 mL / min. As an example, although the pump for pressurizing the fluid has been stopped, the fluid is introduced into the flow path 11 due to the pulsation of the pump. In this case, the flow rate of the fluid can be considered to be substantially 0 mL / min. As another example, although all valves located upstream or downstream of the flow path 11 have been closed, the fluid is introduced into the flow path 11 due to leakage of the valve. In this case, the flow rate of the fluid can be considered to be substantially 0 mL / min. Without limitation, for example, making the flow rate of the fluid 0.01 mL / min or less falls within the scope of "making the flow rate of the fluid substantially 0 mL / min."

[0060] (flow)

[0061] In this embodiment, the flow rate VA' of the first fluid A is maintained constant, while the flow rate VB' of the second fluid B is reduced or substantially reduced to 0 mL / min to form the streak-shaped fluid F. Formation step S12 can be performed using an operation known in the art. In this embodiment, the flow rate VB' of the second fluid B is reduced to less than the flow rate VB in the introduction step S11 or substantially reduced to 0 mL / min to achieve a total flow rate VA'+VB' of the flow rates VA' of the first fluid A and VB' of the second fluid B below the aforementioned limiting flow rate, thereby forming the streak-shaped fluid F.

[0062] The total flow rate VA′+VB′ of fluids A and B in step S12 is not particularly limited within the range that allows the formation of a streak-shaped fluid F. As one example, it is 0.1 mL / min or greater, and as another example, it is 5 mL / min or greater. Within this range, the greater the total flow rate VA′+VB′, the greater the hourly processing volume. Furthermore, the total flow rate VA′+VB′ is not particularly limited within the range that allows the formation of a streak-shaped fluid F. As one example, it is 20 mL / min or less, and as another example, it is 40 mL / min or less. Within this range, the smaller the total flow rate VA′+VB′, the greater the effect of reducing the formation of emulsions within the streak-shaped fluid F. Furthermore, when using three or more fluids, the total flow rate of the three or more fluids is preferably within the above-mentioned range.

[0063] The total flow rate VA′+VB′ of fluids A and B can be appropriately adjusted depending on the type of fluid, the material of flow path 11, the performance of the pump that pumps the fluids, and the like. For example, when glass is used as the material of flow path 11, streaked fluid F tends to be more stably formed at a larger flow rate. Therefore, in order to achieve a slug flow with excellent throughput, the total flow rate VA′+VB′ is preferably set to a larger value.

[0064] (Duration of the forming process)

[0065] like Figure 2 As shown in (a), in this embodiment, during the duration T2 of the formation step S12, the flow rate of the second fluid B is reduced or substantially reduced to 0 mL / min. The duration T2 of the formation step S12 is preferably 0.01 seconds or longer, more preferably 1.0 seconds or longer. Within this range, the longer the duration T2, the easier it is to form a more stable streak-shaped fluid F. In addition, the duration T2 is preferably 6.0 seconds or shorter, more preferably 3.0 seconds or shorter. Within this range, the shorter the duration T2, the more effective it is to increase the apparent flow rate of the streak-shaped fluid F and the hourly processing volume.

[0066] The duration T2 of the formation step S12 can be appropriately adjusted 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. For example, when a high-viscosity fluid is used, the time required for the parallel-flowing streak-shaped fluid F to undergo a morphological change tends to be long, so it is preferable to set the duration T2 to a longer time. As a specific example, when any one of the two or more fluids is silicone oil, the duration T2 is preferably set to be at least 2 seconds.

[0067] The duration T2 of the formation step S12 can be selected in consideration of the ratio T2 / T1 relative to the duration T1 of the introduction step S11. For example, the ratio T2 / T1 is preferably 60 or less, and more preferably 5 or less. Within this range, a smaller ratio T2 / T1 increases the average flow rate through the formation process M1, that is, the apparent flow rate of the streak-shaped fluid F.

[0068] [Flow behavior during repeated introduction and formation steps]

[0069] Below, we will refer to Figure 2 (b)~ Figure 2 (e) The state of the two fluids A and B in the flow channel 11 during the period in which the introduction step S11 and the formation step S12 are alternately and repeatedly performed will be described.

[0070] like Figure 2As shown in (b), in the first introduction step S11, a first fluid A with a flow rate VA and a second fluid B with a flow rate VB are introduced into the flow path 11 together, thereby forming a flow of two fluids A and B. Here, the two fluids A and B merge at a confluence portion (not shown) located upstream of the flow path 11 and then flow into the flow path 11. The two fluids A and B are in a stable state with respect to the friction generated between them and the inner wall of the flow path 11, forming parallel flows and flowing in the flow path 11. The parallel flows are formed by the two fluids A and B being arranged in a manner perpendicular to the length L of the flow path 11. In addition, the larger the flow rate VA of the first fluid A and the flow rate VB of the second fluid B, the stronger the tendency of the two fluids A and B to form parallel flows.

[0071] like Figure 2 As shown in (c), in the initial formation step S12, the flow rate VA' of the first fluid A is maintained constant at the flow rate VA in the introduction step S11, while the flow rate VB' of the second fluid B is maintained at substantially 0 mL / min. This causes the parallel-flowing striped fluid F formed in the initial introduction step S11 to undergo a morphological change. The striped fluid F consists of a phase PA composed of the first fluid A and a phase PB composed of the second fluid B, alternating along the length L of the flow path 11. In the initial formation step S12, the phase PA composed of the first fluid A occupies the upstream portion of the striped fluid F, while the flow rate of the first fluid A remains constant.

[0072] like Figure 2 As shown in (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 that have recently flowed into the flow channel 11 from the confluence portion form parallel flows, similar to the initial introduction step S11. Meanwhile, the streak-shaped fluid F formed in the initial formation step S12 flows through the flow channel 11 while maintaining the alignment of the phases PA and PB, thereby forming a slug flow.

[0073] like Figure 2 As shown in (e), in the next forming step S12, the same operation as the first forming step S12 is performed. As a result, the parallel flow formed in the next introducing step S11 changes its form to the streak-shaped fluid F again.

[0074] Generally, if the goal is to create a slug flow, forming a parallel flow is considered undesirable. However, as described above, in this embodiment, the parallel flow formed undergoes a morphological change to a striped fluid F during the formation step S12. Therefore, according to this embodiment, there is no need to suppress the flow rate of the fluid to avoid the formation of parallel flows, and a slug flow with a large flow rate can be formed. In addition, in this embodiment, two or more fluids are introduced into the flow path 11 simultaneously, so there is no need to limit the fluid temporarily introduced into the flow path 11 to a single type, nor is there a need to perform high-speed valve control. Therefore, according to this embodiment, a slug flow can be more easily formed.

[0075] [Variation]

[0076] In this embodiment, the introduction step S11 is first performed, followed by the formation step S12, and then the introduction step S11 and the formation step S12 are repeated alternately. However, in one aspect of the present invention, the order of the steps is not limited to this. For example, the formation step S12 may be first performed, followed by the introduction step S11, and then the formation step S12 and the introduction step S11 may be repeated alternately.

[0077] [Methods for preparing chemical substances]

[0078] The method M1 for forming a striped fluid according to one aspect of the present invention can be used, for example, in a chemical preparation process. Specifically, the method M1 for forming a striped fluid according to one aspect of the present invention includes treating a chemical substance or its precursor using the method M1 for forming a striped fluid according to one aspect of the present invention.

[0079] In one aspect of the present invention, a method for producing a chemical substance involves treating a chemical substance or its precursor using a slug flow formed during a formation method M1. Examples of treatment objectives include, but are not limited to, heterogeneous reactions, extraction, and separation. Furthermore, the method for producing a chemical substance may also comprise a multi-stage reaction. The target of treatment using the streak-shaped fluid formation method M1 is not limited to the final product, i.e., the target substance to be produced; it may also be a precursor generated initially or midway through a multi-stage reaction.

[0080] The chemical substance to be prepared is not particularly limited and can be selected from substances known in the art. Examples of the chemical substance include, but are not limited to, peptides.

[0081] In the case of peptide production, slug flow can be used to separate the peptide from byproducts. In this case, an organic liquid and an aqueous solution can be used as fluids, the organic liquid containing the peptide and byproducts as solutes, and the aqueous solution used to remove only the byproducts into the aqueous solution.

[0082] [Apparatus for forming a streak-shaped fluid]

[0083] An apparatus for forming a striped fluid according to one aspect of the present invention is as follows: a apparatus for forming a striped fluid, which is used to form a striped fluid in which two or more phases, respectively composed of two or more mutually immiscible fluids, are alternately arranged along the length direction of a flow path, the apparatus comprising: two or more containers for storing the two or more fluids respectively; a flow path connected to the two or more containers; a pump for pressurizing the two or more fluids into the flow path respectively; and a control unit; wherein the control unit is configured to: cause the apparatus for forming the striped fluid to perform an introduction process, a formation process, and a process for causing the apparatus for forming the striped fluid to alternately and repeatedly perform the introduction process and the formation process, wherein in the introduction process, the flow of the two or more fluids is formed by introducing the two or more fluids into the flow path together; in the formation process, the flow rate of a portion of the two or more fluids in the flow path is maintained substantially constant at the flow rate in the introduction process, and at the same time, in order to form the striped fluid, the flow rate of the other fluids in the two or more fluids is made lower than the flow rate in the introduction process or is substantially 0 mL / min.

[0084] Below, we will refer to Figure 3 A device 100 for forming a streak-shaped fluid according to an embodiment of the present invention will be described. Figure 3 This is a block diagram illustrating the structure of an apparatus 100 for forming a streak-shaped fluid according to one embodiment of the present invention. Without limitation, apparatus 100 can execute the aforementioned forming method M1. For ease of description, components having the same functions as those described in forming method M1 are designated with the same reference numerals, and their descriptions will not be repeated.

[0085] (Parts forming the device)

[0086] like Figure 3 As shown, the forming apparatus 100 includes a flow path 11 , two containers 12A and 12B, two pumps 13A and 13B, a merging portion 14 , a recovery container 15 , and a control portion 16 .

[0087] The flow path 11 is a flow path connecting the merging portion 14 and the recovery container 15. Figure 3 As shown, the flow path 11 is connected to the containers 12A and 12B via the junction 14, the pumps 13A and 13B, respectively. The structure of the flow path 11 is as described in the formation method M1 above, and its description will not be repeated.

[0088] Two containers 12A and 12B respectively store two immiscible fluids A and B.

[0089] Pump 13A is in communication with container 12A and confluence portion 14, and is used to pressure-transfer fluid A contained in container 12A to flow path 11 connected to confluence portion 14. Similarly, pump 13B is in communication with container 12B and confluence portion 14, and is used to pressure-transfer fluid B contained in container 12B to flow path 11 connected to confluence portion 14.

[0090] The confluence portion 14 is a three-branch pipe that communicates with the pumps 13A and 13B and the recovery container 15. The confluence portion 14 and the recovery container 15 are communicated via the flow path 11. Examples of the confluence portion 14 include a T-tube, a Y-tube, a spiral mixer, and a static mixer.

[0091] The recovery container 15 is in communication with the merging portion 14 and is used to recover and store the streak-shaped fluid F flowing in the flow path 11 as a slug flow.

[0092] In addition, in the present embodiment, the component provided downstream of the flow path 11 is not limited to the recovery container 15. For example, a settler may be provided downstream of the flow path 11. In this case, the settler can continuously separate two or more mutually immiscible fluids that flow into the settler from the flow path 11 as streak-shaped fluids while discharging them. In addition, a recovery container 15 may be provided downstream of the settler to recover the separated fluids. Alternatively, any external component may be provided downstream of the flow path 11 to discharge the two or more fluids discharged from the flow path 11 to the outside of the forming device 100.

[0093] The control unit 16 is communicably connected to the pumps 13A and 13B. In addition, the connection object of the control unit 16 is not limited to the pumps 13A and 13B. As long as it is connected to each part of the forming device 100 so that the forming device 100 can perform the introduction process and the formation process described below, it can be obtained. For example, the control unit 16 can also be communicably connected to a valve, which is arranged at an arbitrary position in the flow path for connecting the containers 12A and 12B and the recovery container 15. As the control unit 16, a processor such as a central processing unit (CPU), a microprocessor (MPU) or a microcontroller can be used.

[0094] In addition, in the present embodiment, the forming device 100 is described for using two fluids and having the same number of containers and pumps (i.e., two containers and two pumps). However, one aspect of the present invention is not limited to this. When using three or more fluids, three or more containers and pumps can also be respectively provided on the forming device 100. In addition, the number of pumps can also be different from the number of fluids. For example, one pump can also be provided to jointly pressure-feed two or more fluids. In addition, when using three or more fluids, as the confluence portion, a pipe with one more branch than the number of fluids can be used, or a pipe having two or more three-branch pipes connected can also be used.

[0095] (Processing by the control unit)

[0096] The control unit 16 causes the forming device 100 to perform an introduction process (introduction step S11) and a formation process (formation step S12). The introduction process is a process that performs the introduction step S11, and the formation process is a process that performs the formation step S12. Furthermore, the control unit 16 causes the forming device 100 to perform a process that causes the forming device 100 to alternately and repeatedly perform the introduction process and the formation process. Thus, the forming device 100 alternately and repeatedly performs the introduction step S11 and the formation step S12.

[0097] The various processes performed by the forming apparatus 100 are achieved by the control unit 16 sending command signals to the pumps 13A and 13B. Specifically, the control unit 16 sends command signals to the pumps 13A and 13B to adjust the amount of fluid pumped according to the flow rate and duration of the introduction step S11 and the forming step S12. Pumps 13A and 13B receive the command signals and pump fluids A and B into the flow path 11 according to the flow rate and duration included in the command signals.

[0098] As a modified example, when the control unit 16 is communicatively connected to the valve, each process performed by the forming apparatus 100 is achieved by the control unit 16 sending a command signal to the valve. Specifically, the control unit 16 sends the command signal to the valve to adjust the opening and closing degree to a flow rate and duration that allows for smooth flow through the introduction step S11 and the forming step S12. The valve receives the command signal and adjusts its opening and closing degree based on the opening and closing degree indicated in the command signal.

[0099] 〔Summarize〕

[0100] Based on the above description, it can be understood that the present invention includes the following aspects.

[0101] The first aspect: A method for forming a striped fluid, which is used to form a striped fluid formed by alternating two or more phases composed of two or more mutually immiscible fluids along the length direction of the flow path. The method alternately and repeatedly implements an introduction process and a formation process. In the introduction process, the flow of the two or more fluids is formed by introducing the two or more fluids into the flow path together; in the formation process, the flow rate of a part of the two or more fluids in the flow path is maintained at a substantially constant flow rate in the introduction process. At the same time, in order to form the striped fluid, the flow rate of other fluids in the two or more fluids is made lower than the flow rate in the introduction process or is substantially 0 mL / min.

[0102] A second aspect: The method for forming a striped fluid according to the first aspect, wherein the forming step is performed after a cumulative volume ratio of the two or more fluids introduced into the flow path in the introducing step reaches a predetermined value.

[0103] A third aspect: A method for forming a striped fluid according to the first aspect or the second aspect, wherein the two or more fluids are a combination of a first fluid and a second fluid, the first fluid is water or an aqueous solution, and the second fluid is a hydrophobic organic liquid.

[0104] Aspect 4: A method for forming a striped fluid according to aspect 1 or aspect 2, wherein the two or more fluids are a combination of a first fluid, a second fluid and a third fluid, the first fluid is water or an aqueous solution, the second fluid is a hydrophobic organic liquid, and the third fluid is a gas.

[0105] A fifth aspect: A method for preparing a chemical substance, comprising: using the method for forming a striped fluid described in any one of the first to fourth aspects to process the chemical substance or its precursor.

[0106] In the sixth aspect, a striped fluid forming device is used to form a striped fluid formed by alternating two or more phases of two or more mutually immiscible fluids along the length direction of a flow path, the device comprising: two or more containers for storing the two or more fluids respectively; a flow path connected to the two or more containers; a pump for pressurizing the two or more fluids to the flow path respectively; and a control unit; wherein the control unit is configured to: cause the striped fluid forming device to perform an introduction process, a formation process, and a process for causing the striped fluid forming device to alternately and repeatedly perform the introduction process and the formation process, in which the introduction process forms a flow of the two or more fluids by introducing the two or more fluids into the flow path together; in which the formation process maintains a flow rate of a portion of the two or more fluids in the flow path substantially constant while maintaining a flow rate in the introduction process. At the same time, in order to form the striped fluid, the flow rate of the other fluids in the two or more fluids is lower than the flow rate in the introduction process or is substantially 0 mL / min.

[0107] [Notes]

[0108] 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 technical means disclosed in different embodiments are also included in the technical scope of the present invention.

[0109] Example

[0110] In the following, an embodiment of the present invention is described. In this embodiment, the formation of streaky fluids when two or more fluids are introduced into a flow path under various conditions is verified.

[0111] [Example 1]

[0112] Use the following device to assemble Figure 3 The forming device shown is the same device.

[0113] Pump: Diaphragm pump "QI-100-TT-PS" (manufactured by Tekmina);

[0114] Junction: PFA Union Tee "PFA-220-3" (outer diameter 1 / 8 inch, manufactured by Swagelok);

[0115] Flow path: PFA tube (inner diameter 1.59 mm, length 2 m, manufactured by Flon Industry Co., Ltd.)

[0116] 4-Methyltetrahydropyran (MTHP) was used as the first fluid A, and water was used as the second fluid B. The two pumps pumping fluids A and B, respectively, were repeatedly operated as follows: the first fluid A was pumped at a flow rate of 5 mL / min and the second fluid B was pumped at a flow rate of 50 mL / min for 1 second (introduction step), followed by pumping the first fluid A at a flow rate of 5 mL / min for 1 second while the pump pumping the second fluid B was stopped for 1 second (formation step). An animation of the operating flow path was taken to visually determine whether streaked fluid had formed in the flow path during the formation step. Furthermore, if streaked fluid had formed, the length of each phase constituting the streaked fluid along the length of the flow path was measured. The results are shown in Table 3.

[0117] [Examples 2 to 25]

[0118] Examples 2 to 25 were performed using the same method as Example 1, except that the type of fluid, the device, and the operating conditions of the pump were changed as shown in Tables 1 and 2. In Examples 20 and 21, MTHP containing RHEODOLTW-0120V as a solute at a concentration of 0.1 M was used as Fluid A. The results are shown in Table 3.

[0119] [Comparative Examples 1 to 8, Reference Examples 1 and 2]

[0120] Comparative Examples 1 to 8 and Reference Examples 1 and 2 were conducted using the same method as Example 1, except that all fluids were continuously pumped at a constant flow rate and the fluid types, equipment, and pump operating conditions were varied as shown in Tables 1 and 2. In Comparative Example 7, MTHP containing RHEODOL TW-0120V at a solute concentration of 0.1 M was used as fluid A. The results are shown in Table 3.

[0121] [Comparative Examples 9 to 12]

[0122] Comparative Examples 9 to 12 were carried out in the same manner as in Example 1 except that the type of fluid, the device, and the operating conditions of the pump were changed as shown in Tables 1 and 2. The results are shown in Table 3.

[0123] Table 1

[0124]

[0125]

[0126] Table 2

[0127]

[0128]

[0129] Table 3

[0130]

[0131]

[0132] 〔result〕

[0133] (Reference Examples 1-2)

[0134] The results of Reference Example 1 show that, when the total flow rate of the introduction step is low, a streak-like fluid is formed without performing the formation step. However, due to the low apparent flow rate, the processing volume of the streak-like fluid in Reference Example 1 is expected to be small. Furthermore, the results of Reference Example 2 show that, when glass is used as the flow path material, streak-like fluid can be formed without performing the formation step even at a higher total flow rate than with PFA.

[0135] (Comparative Examples 1 to 8)

[0136] The results of Comparative Examples 1 to 8 and Reference Examples 1 and 2 show that the larger the total flow rate in the introduction step, the more likely it is that a streak-shaped fluid cannot be formed without performing the formation step.

[0137] (Examples 1 to 25)

[0138] According to the results of Examples 1 to 25 and Comparative Examples 1 to 8, it can be seen that even when the total flow rate of the introduction process is the same as that of Comparative Examples 1 to 8, a striped fluid is formed by implementing the formation process. In addition, in Examples 1 to 25, the time (T1+T2) of one cycle of the introduction process and the formation process is as short as 1.1 seconds to 6 seconds, and the length of the phase is as short as 0.5 cm to 7.0 cm. In the technology of Reference 1, in order to achieve the same phase length, the valve is controlled with a shorter cycle, so the device structure tends to be complicated. Therefore, in order to form a slug flow with a certain phase length, it can be said that according to the present invention, the slug flow can be more easily formed with a simpler device structure.

[0139] By comparing Examples 1, 4, 5, 8 to 10 with Comparative Examples 1, 9 to 11, it can be seen that by reducing the flow rate of fluid B in the formation process to a certain reference value (limiting flow rate) lower than the flow rate in the introduction process or to 0 mL / min, a streak-like fluid is formed. Combined with the above comparison and the comparison of Examples 6 and 7 with Comparative Examples 2 and 12, the results show that the limiting flow rate can vary depending on the type of fluid and device. However, according to the results of Examples 1 to 3, 6, 8 to 20, and 22, when the flow rate of fluid B in the formation process is 0 mL / min, a streak-like fluid is formed in any of the Examples. In addition, under normal circumstances, it can be easily determined by known means such as visual inspection whether a streak-like fluid has been formed. Therefore, it can be said that by changing the flow rate of fluid B in the formation process within a range less than the flow rate in the introduction process and above 0 mL / min, while determining whether a streak-like fluid has been formed, the limiting flow rate can be easily determined. Furthermore, in one aspect of the present invention, as long as the flow rate of fluid B during the formation step is below the predetermined limiting flow rate and above 0 mL / min, streaky fluid formation can be achieved. Furthermore, based on the results of Examples 22 to 25, these considerations also apply when using three or more fluids.

[0140] The results of Example 8 and Comparative Example 1 show that even when the apparent flow rate is so high that streaked fluid cannot be formed without the formation step, streaked fluid is formed by performing the formation step. Therefore, it can be said that according to the present invention, the processing volume achieved by utilizing slug flow is greater.

[0141] The results of Examples 8 to 11 demonstrate that, even when the total flow rate during 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, it can be said that the present invention allows for appropriate adjustment of the time the fluid remains in the flow path, thereby achieving the desired level of treatment.

[0142] The results of Reference Example 1 and Comparative Example 7 show that streaked flow tends to be difficult to form when the fluid contains a solute. However, the results of Examples 20 and 21 and Comparative Example 6 show that, by performing the formation process, streaked flow can be formed even when the fluid contains a solute. Therefore, it can be said that the present invention can form slug flow with a wider variety of fluids.

[0143] Furthermore, in Example 17, which had the highest total flow rate during the introduction process, the streak-like fluid that was temporarily formed did not change its form to a parallel flow during the introduction process, but instead flowed as a slug flow. Therefore, it can be said that the present invention can achieve a slug flow with a higher apparent flow rate.

[0144] Industrial applicability

[0145] The present invention can be used for the preparation of chemical substances, etc.

[0146] Description of Reference Numerals

[0147] 11 flow path

[0148] 12A, 12B containers

[0149] 13A, 13B pumps

[0150] 16 Control Unit

[0151] 100 forming device

Claims

1. A method for forming a striped fluid, wherein two or more phases of two or more mutually immiscible fluids are alternately arranged along the length of a flow path. The method alternately and repeatedly performs the introduction step and the formation step, In the introducing step, the two or more fluids are introduced into the flow path together, thereby forming a flow of the two or more fluids; In the formation process, the flow rate of a part of the two or more fluids in the flow path is maintained at the flow rate in the introduction process and remains substantially constant. At the same time, in order to form the striped fluid, the flow rate of other fluids in the two or more fluids is made lower than the flow rate in the introduction process or is substantially 0 mL / min.

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

3. The method for forming a striped fluid according to claim 1 or 2, wherein: The two or more fluids are a combination of a first fluid and a second fluid, the first fluid is water or an aqueous solution, and the second fluid is a hydrophobic organic liquid.

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

5. A method for preparing a chemical substance, comprising: A chemical substance or a precursor thereof is treated using the method for forming a striped fluid according to any one of claims 1 to 4.

6. A stripe-shaped fluid forming device for forming a stripe-shaped fluid in which two or more phases composed of two or more mutually immiscible fluids are alternately arranged along the length direction of a flow path. The device comprises: Two or more containers for storing the two or more fluids respectively; a flow path communicating with the two or more containers; A pump for pressure-feeding the two or more fluids to the flow paths respectively; and Control Department; in, The control unit is configured to: cause the stripe-shaped fluid forming device to perform an introduction process, a formation process, and a process for causing the stripe-shaped fluid forming device to alternately repeat the introduction process and the formation process; In the introduction process, the two or more fluids are introduced into the flow path together, thereby forming a flow of the two or more fluids; During the formation process, the flow rate of a part of the two or more fluids in the flow path is maintained at the flow rate in the introduction process and remains substantially constant. At the same time, in order to form the striped fluid, the flow rate of other fluids in the two or more fluids is made lower than the flow rate in the introduction process or is substantially 0 mL / min.

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