Micromixer for flow synthesis device and flow synthesis device

The flow synthesis device addresses the challenge of mixing gas and liquid phases with different characteristics by using a hexagonal switching valve to manage pressure differences and ensure uniform mixing ratios, enabling efficient continuous gas-liquid reactions.

JP7678420B2Active Publication Date: 2025-05-16NAKAMURA CHOKO
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Patent Information

Application Number
JP2022126532
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Filing Date
2022-08-08
Publication Date
2025-05-16
Estimated Expiration
2042-08-08

AI Technical Summary

Technical Problem

Existing flow synthesis devices face challenges in efficiently mixing gas and liquid phases with different characteristics, particularly in balancing pressure differences and achieving uniform mixing, which is essential for continuous gas-liquid reactions.

Method used

A flow synthesis device equipped with a hexagonal switching valve and microfluidic channels that allow for the continuous alternation of gas and liquid phases into the synthesis channel, effectively managing pressure differences and ensuring uniform mixing ratios.

Benefits of technology

The device enables continuous and efficient gas-liquid reactions by maintaining a predetermined mixing ratio of gas and liquid phases, even with significant pressure differences, thus facilitating desired chemical synthesis outcomes.

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Abstract

To provide a micro mixer for a flow synthesis device where confluence of a gas phase and a liquid phase can be performed at a prescribed quantitative ratio without flowing back of the liquid phase to a gas phase supply flow channel side even a pressure difference between the supplied gas phase and the liquid phase occurs when the confluence of the gas phase and the liquid phase is performed and a gas-liquid reaction is continuously performed for flow synthesis.SOLUTION: In a micro mixer for a flow synthesis device having a hexagonal selector valve, a gas phase supply flow channel, a liquid phase supply flow channel, a discharge flow channel, a synthesis flow channel and a sample loop,: a first flow channel where the gas phase or liquid phase supply flow channel, the sample loop and the discharge flow channel are communicated and at the same time, the liquid phase or gas phase supply flow channel and the synthesis flow channel are communicated and a second flow channel where the gas phase or liquid phase supply flow channel, the sample loop and the discharge flow channel are communicated and at the same time, the liquid phase or gas phase supply flow channel, the sample loop and the synthesis flow channel are communicated are alternately changed by the hexagonal selector valve; and the liquid phase and the gas phase can be alternately flowed out to the synthesis flow channel.SELECTED DRAWING: Figure 1
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Description

[Technical field]

[0001] The present invention relates to a micromixer for a flow synthesis apparatus and a flow synthesis apparatus having the micromixer for a flow synthesis apparatus. [Background technology]

[0002] Flow synthesis equipment with micromixers is said to have characteristics such as enabling precise temperature control based on the size of the specific surface area by utilizing microchannels with tiny cross sections, enabling precise mixing control based on molecular diffusion between stable laminar flow interfaces, and enabling reaction time control by precise control of residence time in the microchannels. Therefore, by utilizing these characteristics, they are used in chemical synthesis, creation of new substances, etc.

[0003] In such a flow synthesis device, multiple fluids are continuously introduced into a mixing channel of a microchannel in a micromixer and mixed. As mentioned above, mixing in a micromixer utilizes molecular diffusion, but it is not necessarily easy to introduce fluids into a microchannel and mix multiple fluids uniformly by molecular diffusion.

[0004] As a solution to this problem, for example, Patent Document 1 proposes a fluid mixer that has a mixing flow path and a number of inflow paths connected to it in order to form the fluids to be mixed in a thin and uniform multilayer in the mixing section, or to slow down the flow rate while maintaining a thin layer, and at least two types of fluids are introduced into the mixing flow path from the respective inflow paths to mix the fluids, and the mixing flow path is provided with a number of flow path connections by connecting the multiple inflow paths at predetermined intervals in the flow direction, and the flow path is piped so that different types of fluids are introduced into adjacent flow path connections.

[0005] In addition to the point about uniform mixing by molecular diffusion mentioned above, Patent Document 2 lists the following functions as required for achieving an ideal molecular weight distribution when synthesizing polymers by radical polymerization reactions using such a flow synthesis apparatus: (i) uniform temperature control, (ii) high-viscosity liquid delivery of the polymer product, and (iii) gas-liquid mixing / separation.Then, as a configuration for achieving function (iii), it is described that a special elastic tube that is permeable to gas but not to liquid is provided in a specified pressure chamber, and the reaction is carried out in the elastic tube. [Prior art documents] [Patent documents]

[0006] [Patent Document 1] International Publication No. 2006 / 030952 [Patent Document 2] JP 2009-274030 A Summary of the Invention [Problem to be solved by the invention]

[0007] Incidentally, starting materials used in the study of various chemical syntheses and the creation of new substances using a flow synthesis device having a micromixer include various materials in the gas phase, liquid phase, and the like. In order to introduce and mix these phases into a mixing channel of a microchannel, it is generally necessary to apply a large pressure. The characteristics of the starting materials are various, and the introduction pressure is selected according to the characteristics. To introduce them into the mixing channel, the introduction pressure is controlled so as to minimize the pressure difference between the phases to be introduced and to balance the pressures. When the starting materials are both gas phases or both liquid phases, it tends to be easy to introduce them into the mixing channel by controlling the introduction pressure, but when the starting materials are both liquid phases and gas phases, their characteristics are significantly different, and it is difficult to balance the pressures.

[0008] The inventors attempted to use a conventional T-shaped micromixer to supply gas and liquid phases to it and mix them together, but found that the pressure difference was so large that the liquid phase flowed back into the gas phase supply channel, making mixing impossible.

[0009] In the above-mentioned Patent Documents 1 and 2, gas, liquid, etc. are listed as applicable fluids. However, in the invention described in Patent Document 1, a complex microchannel is formed in order to form the fluid to be mixed into a thin and uniform multilayer and realize efficient mixing by molecular diffusion. It is considered that a considerable high pressure is required to introduce a liquid phase into such a complex microchannel. Therefore, when trying to mix a liquid phase and a gas phase into such a fluid mixer, it is necessary to introduce the gas phase at an even higher pressure, which is considered to be very difficult in practice. In addition, as described above, the invention described in Patent Document 2 describes the movement of gas inside and outside the elastic tube using a specific elastic tube, but it is considered that a considerable pressure is still required to introduce gas into the elastic tube, and it is considered difficult to realize. Patent Document 2 specifically describes the movement of gas generated by a reaction or the like in the liquid phase in the elastic tube to the outside of the elastic tube, but does not mention a specific example of moving the gas outside the elastic tube into the elastic tube.

[0010] Therefore, an object of the present invention is to provide a micromixer for a flow synthesis apparatus that, when performing flow synthesis in which a gas phase and a liquid phase are joined by a micromixer to perform a continuous gas-liquid reaction, is capable of joining the gas phase and the liquid phase in a predetermined volume ratio without the liquid phase flowing back into the gas phase supply flow path even if there is a pressure difference between the gas phase and the liquid phase being supplied, and to provide a flow synthesis apparatus that has the micromixer for a flow synthesis apparatus and is capable of performing flow synthesis by a desired gas-liquid reaction. [Means for solving the problem]

[0011] The present inventors have conducted extensive research to solve the above-mentioned problems. As a result, they have found that when performing flow synthesis in which a gas phase and a liquid phase are joined by a micromixer to perform a continuous gas-liquid reaction, it is possible to prevent the liquid phase from flowing back into the gas phase supply flow channel by continuously and alternately discharging the gas phase and liquid phase continuously supplied from each supply flow channel into the synthesis flow channel, thereby making it possible to perform a continuous gas-liquid reaction between the gas phase and the liquid phase in a desired volume ratio. The gist of the present invention is as follows.

[0012] A first aspect of the present invention is a micromixer for a flow synthesis apparatus that continuously merges a gas phase and a liquid phase, the micromixer for a flow synthesis apparatus having a six-way switching valve, a gas phase supply flow path, a liquid phase supply flow path, a discharge flow path, a synthesis flow path, and a sample loop, the six-way switching valve having a gas phase supply port connected to the gas phase supply flow path, a liquid phase supply port connected to the liquid phase supply flow path, a discharge port connected to the discharge flow path, a synthesis outlet connected to the synthesis flow path, and two sample loop openings connected to both ends of the sample loop, the six-way switching valve having a gas phase or The present invention relates to a micromixer for a flow synthesis apparatus, which is switchable between a first flow path in which a liquid phase supply flow path, a sample loop, and a discharge flow path are connected, and at the same time, a liquid phase or gas phase supply flow path and a synthesis flow path are connected, and a second flow path in which a gas phase or liquid phase supply flow path and a discharge flow path are connected, and at the same time, a liquid phase or gas phase supply flow path, a sample loop, and a synthesis flow path are connected, and which is capable of alternately flowing out the liquid phase and the gas phase into the synthesis flow path by alternately switching between the first flow path and the second flow path and causing at least the gas phase or liquid phase that has flowed into the sample loop to flow out.

[0013] In an embodiment of the micromixer for a flow synthesis apparatus, the sample loop opening may have a first opening and a second opening, and the gas phase supply port, the first opening of the sample loop opening, the synthesis outlet, the liquid phase supply port, the second opening of the sample loop opening, and the outlet may be provided in this order in a clockwise or counterclockwise direction in the six-way switching valve.

[0014] A second aspect of the present invention relates to a flow synthesis apparatus having the micromixer for a flow synthesis apparatus.

[0015] In the embodiment of the flow synthesis apparatus, a pressure regulator may not be provided downstream of the synthesis channel.

[0016] The above-mentioned micromixer and each of the flow channels constituting the flow synthesis apparatus having the micromixer are minute flow channels, and a minute flow channel refers to a flow channel having a cross-sectional width or inner diameter of 1.0 mm or less. Effect of the Invention

[0017] According to the present invention, when performing flow synthesis in which a gas phase and a liquid phase are joined by a micromixer to perform a continuous gas-liquid reaction, the gas phase and the liquid phase can be joined in a predetermined volume ratio even if there is a pressure difference between the gas phase and the liquid phase being supplied, without the liquid phase flowing back into the gas phase supply flow path, and a flow synthesis apparatus having the micromixer for a flow synthesis apparatus and capable of performing flow synthesis by a desired gas-liquid reaction can be provided. [Brief description of the drawings]

[0018] [Figure 1] FIG. 1 is an explanatory diagram for explaining an overview of a micromixer for a flow synthesis apparatus according to an embodiment of the present invention and a flow synthesis apparatus having the same, and a flow path configuration thereof. [Diagram 2] 1. FIG. 4 is an explanatory diagram for explaining a state when a gas phase is made to flow into a sample loop in the micromixer according to the embodiment shown in FIG. 1 when a six-way switching valve has a flow path configuration of a first flow path. [Diagram 3] 3 is an explanatory diagram for explaining a state immediately after the six-way switching valve is switched to a second flow path from the state shown in FIG. 2. FIG. [Figure 4] FIG. 4 is an explanatory diagram for illustrating a state in which, from the state shown in FIG. 3, a liquid phase is flowed into the sample loop, the gas phase in the sample loop is pushed out by the liquid phase and flows out into the synthesis flow channel, and the gas phase is also flowed out from the gas phase supply flow channel to the discharge flow channel. [Diagram 5] 5 is an explanatory diagram for explaining a state immediately after the six-way switching valve is switched to a first flow path from the state shown in FIG. 4. FIG. [Figure 6]FIG. 6 is an explanatory diagram for illustrating a state in which a gas phase is flowed into a sample loop from the state shown in FIG. 5, and the liquid phase in the sample loop is pushed out by the gas phase and flows out into a discharge flow channel, and the liquid phase is also flowed out from a liquid phase supply flow channel into a synthesis flow channel. [Figure 7] 7 is an explanatory diagram for explaining a state immediately after the six-way switching valve is switched to a second flow path from the state shown in FIG. 6. FIG. [Figure 8] 13 is an image showing a state in which a gas phase and a liquid phase are continuously and alternately discharged into a synthesis channel using a micromixer according to an embodiment in an experimental example. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0019] Hereinafter, an embodiment of the present invention will be described with reference to the drawings. However, the present invention is not limited to these examples, and it is of course possible to implement the present invention in various forms without departing from the spirit of the present invention.

[0020] FIG. 1 is an explanatory diagram for illustrating a flow channel configuration of a micromixer for a flow synthesis apparatus (hereinafter, may be referred to as a "micromixer") 1 according to an embodiment of the present invention and a flow synthesis apparatus 2 having the same.

[0021] As shown in FIG. 1, the micromixer 1 has a six-way switching valve 10, a gas-phase supplying flow path 11, a liquid-phase supplying flow path 12, a discharge flow path 13, a synthesis flow path 14, and a sample loop 15. The six-way switching valve 10 has ports (1) to (6), in which the port (1) corresponds to a gas-phase supply port connected to the gas-phase supplying flow path 11, the port (2) corresponds to a first sample loop opening connected to one end (first end) 15a of the sample loop 15, the port (3) corresponds to a synthesis outlet connected to the synthesis flow path 14, the port (4) corresponds to a liquid-phase supply port connected to the liquid-phase supplying flow path 12, the port (5) corresponds to a second sample loop opening connected to the other end (second end) 15b of the sample loop 15, and the port (6) corresponds to an outlet connected to the discharge flow path 13. In the example shown in FIG. 1, the ports (1) to (6) are arranged on the same circumference in the clockwise direction in that order. The intervals between the ports on the circumference are not particularly limited as long as the first and second flow paths described below are formed. In the example shown in Fig. 1, the circumference is divided into six equal parts and the ports are provided.

[0022] In the example shown in FIG. 1, the six-way switching valve 1 is configured to be switchable between the following first and second flow paths. The first flow path is formed by forming a flow path a where ports (1) and (2) communicate with each other, a flow path b where ports (3) and (4) communicate with each other, and a flow path c where ports (5) and (6) communicate with each other, and the gas phase supply flow path 11, the sample loop 15, and the discharge flow path 13 communicate with each other, and at the same time, the liquid phase supply flow path 12 and the synthesis flow path 14 communicate with each other (see FIGS. 1, 2, 5, and 6). The second flow path is formed by forming a flow path d where ports (1) and (6) communicate with each other, a flow path e where ports (2) and (3) communicate with each other, and a flow path f where ports (4) and (5) communicate with each other, and the gas phase supply flow path 11 and the discharge flow path 13 communicate with each other, and at the same time, the liquid phase supply flow path 12, the sample loop 15, and the synthesis flow path 14 communicate with each other (see FIGS. 3, 4, and 7).

[0023] The six-way switching valve 1 can be configured, for example, as a rotary valve including a stator provided with ports (1) to (6) and a rotor in which three flow passage grooves for forming the flow passages a to f are formed. By rotating the rotor, it is possible to switch between the first flow passage and the second flow passage.

[0024] 1, the sample loop 15 has a function of replacing a part of the liquid phase continuously fed to the synthesis channel 14 with a gas phase, and temporarily storing the gas phase when the gas phase and liquid phase are alternately discharged into the synthesis channel 14. In other words, the mixture ratio of the gas phase and the liquid phase can be adjusted by the amount stored in the sample loop 15. Therefore, the length of the sample loop 15 and the like can be determined in consideration of the conditions of the synthesis reaction between the gas phase and the liquid phase.

[0025] In the example shown in FIG. 1, the flow synthesis apparatus 2 includes the above-mentioned micromixer 1; a check valve 16, which is provided in this order upstream of a gas phase supply flow path 11, a mass flow controller 17 for controlling the flow rate of the gas phase, and a gas phase cylinder 18 for storing the gas phase; a check valve 19, a pump 20, and a liquid phase container 21 for storing the liquid phase, which are provided in this order upstream of a liquid phase supply flow path 12; a waste tank 22 provided downstream of a discharge flow path 13; a reaction tank 23 provided downstream of a synthesis flow path 14, and a recovery container 24 for storing a product.

[0026] In the example shown in FIG. 1, there is only one gas phase cylinder 18 and one liquid phase container 21, but multiple containers can be provided as necessary. Gas phases and liquid phases can be mixed with each other using a general micro mixer. The configuration of the reaction vessel 23 can be selected according to the synthesis reaction. For example, a catalyst column filled with a solid catalyst, a reaction tube having a spiral shape, etc. can be used. An example of the solid catalyst filled in the catalyst column is palladium carbon (Pd / C). The reaction vessel 23 can be provided with a heating device, etc., as necessary.

[0027] The flow synthesis apparatus 2 shown in FIG. 1 may have a control unit that controls the operations of the six-way switching valve 10, the pump 20, the check valves 16 and 19, and the mass flow controller 17.

[0028] The operation of the micromixer 1 and flow synthesis device 2 shown in Fig. 1 will be described with reference to Figs. 2 to 7. Fig. 1 shows a stopped state before operation, and in Figs. 2 to 7, the flow of the gas phase in the flow channel is shown by a solid line, and the flow of the liquid phase is shown by a wavy line. The flow direction is also shown by an arrow.

[0029] First, as shown in FIG. 1, the 6-way switching valve 10 is set to the first flow path state to prepare the desired gas phase, liquid phase, etc. Then, as shown in FIG. 2, the gas phase and liquid phase are sent in the first flow path state. The gas phase is sent from the flow path 11 to the flow path a, the sample loop 15, the flow path c, and the flow path 13 while controlling the flow rate by the mass flow controller 17. In some cases, it may reach the waste tank 22. The waste tank 22 is configured so that the gas phase can be safely discharged to the outside. In addition, it may be configured so that the gas phase discharged to the outside can be collected and reused. The liquid phase is sent to the flow path 12, the flow path b, and the flow path 14 while controlling the flow rate by the pump 20. In some cases, it may reach the reaction tank 23 and the collection container 24. After the gas phase is stored in the entire sample loop 15 and the liquid phase reaches the flow path 14, the valve 10 is switched to the second flow path as shown in FIG. 3.

[0030] FIG. 3 shows the state of the gas phase and liquid phase in the flow path of the micromixer 1 immediately after the valve 10 is switched from the state of the first flow path shown in FIG. 2 to the second flow path. As shown in FIG. 3, flow paths a, b, and c are formed in the first flow path, and the gas phase or liquid phase present in each flow path moves to flow paths e, f, and d in the second flow path, respectively. The gas phase in flow path d is pushed into flow path 13 by the gas phase flowing in from flow path 11, and flows into the waste tank 22 while being sandwiched between the gas phases present in flow path 13. The gas phase flowing into the sample loop 15 is pushed into flow path 14 by the liquid phase present in flow path f and the liquid phase flowing in from flow path 12, together with the gas phase in flow path e. At this time, since a liquid phase is also present in flow path 14 downstream of the gas phase, the gas phase flows into flow path 14 while being sandwiched between the liquid phases. That is, the liquid phase, the gas phase, and the liquid phase flow out into the flow path 14 in this order. Then, as shown in FIG. 4, the entire gas phase in the sample loop 15 is caused to flow into the flow channel 14 from the state shown in FIG.

[0031] After that, the valve 10 is switched to the first flow path. FIG. 5 shows the state of the gas phase and the liquid phase in the flow path of the micromixer 1 immediately after the valve 10 is switched from the state of the second flow path shown in FIG. 4 to the first flow path. As shown in FIG. 5, flow paths e, f, and d are formed in the second flow path shown in FIG. 4, and the gas phase or liquid phase present in each flow path moves to flow paths a, b, and c in the first flow path, respectively. The liquid phase present in flow path b is pushed out by the liquid phase flowing in from flow path 12, and flows into flow path 14 while being sandwiched between the liquid phase (which may be a gas phase in some cases) that was present in flow path 14. The liquid phase that has flowed into the sample loop 15 is pushed into flow path 13 by the gas phase flowing in from flow path 11, together with the liquid phase of flow path a and the gas phase of flow path c. Then, as shown in FIG. 6, the gas phase is flowed into the sample loop 15 and stored in the entirety thereof.

[0032] Then, the valve 10 is switched to the second flow path. FIG. 7 shows the state of the gas phase and the liquid phase in the flow path of the micromixer 1 immediately after the valve 10 is switched from the state of the first flow path shown in FIG. 6 to the second flow path. As shown in FIG. 7, flow paths a, b, and c are formed in the first flow path shown in FIG. 6, and the gas phase or liquid phase present in each flow path moves to flow paths e, f, and d in the second flow path, respectively. The gas phase in flow path d is pushed into flow path 13 by the gas phase flowing in from flow path 11, and flows into the waste tank 22 while being sandwiched between the liquid phase that was present in flow path 13. In this way, the gas phase and the liquid phase can flow into the waste tank 22. The liquid phase that has flowed in may be configured to be released to the outside and reused, as in the case of the gas phase described above. The gas phase that has flowed into the sample loop 15 is pushed into the flow path 14 together with the gas phase in flow path e by the liquid phase present in flow path f and the liquid phase flowing in from flow path 12. At this time, since a liquid phase is also present in flow path 14 downstream of the gas phase, the gas phase flows into flow path 14 while being sandwiched between the liquid phases. That is, the liquid phase, gas phase, and liquid phase flow out into flow path 14 in this order. Then, after all of the gas phase present in sample loop 15 has been pushed out into flow path 14, as shown in FIG. 4, for example, the valve 10 is switched back to the first flow path as shown in FIG.

[0033] As described above, by repeatedly switching between the first and second flow paths of the valve 10, it becomes possible to repeatedly and continuously cause the gas phase flowing into the sample loop 15 to flow between the liquid phases when the liquid phase flows from the flow path 12 to the flow path 14 without being affected by the pressure difference. In addition, since the capacity of the sample loop 15 is constant, the liquid phase and the gas phase can be alternately discharged into the flow path 14 at a desired volume ratio by controlling the flow rate of the liquid phase.

[0034] The liquid phase and the gas phase thus alternately discharged into the flow path 14 at a predetermined volume ratio can be continuously subjected to a predetermined gas-liquid reaction in the reaction vessel 23 adjusted to the desired conditions. In particular, when the reaction vessel 23 is equipped with a catalyst column filled with a solid catalyst, the gas phase and the liquid phase are considered to move between the catalyst particles while being agitated in the catalyst column, and therefore the gas phase and the liquid phase are considered to tend to react efficiently.

[0035] The product produced by the gas-liquid reaction in the reaction vessel 23 is collected together with unreacted materials in the collection vessel 24. The collection vessel 24 can be configured so as to be capable of discharging the gas phase to the outside.

[0036] In this embodiment, the hexagonal switching valve 10 is configured to be switchable between a first flow path that connects the gas phase supply flow path 11, the sample loop 15, and the discharge flow path 13, and at the same time connects the liquid phase supply flow path 12 and the synthesis flow path 14, and a second flow path that connects the gas phase supply flow path 11 and the discharge flow path 13, and at the same time connects the liquid phase supply flow path 12, the sample loop 15, and the synthesis flow path 14. The first flow path and the second flow path are alternately switched to allow at least the gas phase that has flowed into the sample loop 15 to flow out into the synthesis flow path 14, thereby allowing the liquid phase and the gas phase to alternately flow out into the synthesis flow path 14.

[0037] As a modified example of this embodiment, for example, the arrangement of the gas phase and the liquid phase can be interchanged. In this case, the ports (1) and (4) of the six-way switching valve 10 are a liquid phase supply port connected to the liquid phase supply flow path and a gas phase supply port connected to the gas phase supply flow path, respectively, and the other configurations are the same as those of the above-mentioned embodiment. The six-way switching valve is configured to be switchable between a first flow path in which the liquid phase supply flow path (corresponding to reference numeral 11 in Figs. 1 to 7) communicates with the sample loop 15 and the discharge flow path 13, and at the same time, the gas phase supply flow path (corresponding to reference numeral 12 in Figs. 1 to 7) communicates with the synthesis flow path 14, and a second flow path in which the liquid phase supply flow path communicates with the discharge flow path 13, and at the same time, the gas phase supply flow path communicates with the sample loop 15 and the synthesis flow path 14. Furthermore, in the same manner as in the above-described embodiment, the first flow path and the second flow path can be alternately switched to allow at least the liquid phase that has flowed into the sample loop 15 to flow out into the synthesis flow path 14, thereby making it possible to allow the liquid phase and the gas phase to flow out alternately into the synthesis flow path 14. This modification is applicable to the case where the pressure in the reaction vessel 23 is lower than the pressure in the gas phase supply flow path (corresponding to reference symbol 12 in FIGS. 1 to 7).

[0038] As described above, the micromixer 1 has the six-way switching valve 10, so that the gas phase and the liquid phase can be alternately discharged into the flow path 14 and merged together regardless of the pressure difference between the gas phase and the liquid phase. Therefore, even if a pressure regulator is not provided downstream of the flow path 14, particularly downstream of the reaction vessel 23, the gas phase and the liquid phase can be supplied to the reaction vessel 23 at a desired ratio.

[0039] Such a micromixer and a flow synthesis apparatus having the same can be applied to various gas-liquid reactions in which a gas phase and a liquid phase are reacted with each other, such as, but not limited to, catalytic hydrogenation. EXAMPLES

[0040] (Experimental Example) In the following, an experiment was conducted in which the steps shown in FIGS. 2 to 7 were carried out using a micromixer 1 according to the embodiment as shown in FIG. 1 described above, and the gas phase and liquid phase, which were supplied separately and continuously, were alternately discharged into the synthesis channel 14 at a predetermined volume ratio.

[0041] The conditions are as follows: Gas phase: Nitrogen, flow rate 10cc / min Liquid phase: Polyethylene glycol 300, flow rate 1.0 ml / min Sample loop 15: Length 100 mm, inner diameter 1.0 mm Width (inner diameter) of channels 11 to 14: 1.0 mm Width of channels a(e), b(f), c(d): 0.25 mm

[0042] As a result, it was confirmed by visual inspection that colorless nitrogen gas (gas phase) and pale yellow colored polyethylene glycol (liquid phase) alternately flowed out continuously into the flow channel 14, and that there was no backflow of the liquid phase into the flow channel 11. An image of the fluid flowing out into the synthesis flow channel 14 at that time is shown in FIG. 8. As shown in FIG. 8, in the flow channel 14, a boundary between the gas phase and the liquid phase was observed at the positions of the arrows indicated by the symbols A to D, and it can be seen that the liquid phase (for example, between AB in FIG. 8) and the gas phase (for example, between BC in FIG. 8) flow out continuously and alternately. Therefore, it can be seen that when the gas phase and the liquid phase are used as substrates for a desired gas-liquid reaction system, it is possible to continuously carry out a desired gas-liquid reaction in a reaction vessel downstream of the flow channel 14. [Explanation of symbols]

[0043] 1 Micromixer for flow synthesis apparatus; 2 Flow synthesis apparatus; 10 Six-way switching valve; 11 Gas phase supply flow path; 12 Liquid phase supply flow path; 13 Discharge flow path; 14 Synthesis flow path; 15 Sample loop; 15a One end; 15b Other end; 16, 19 Check valves; 17 Mass flow controller; 18 Gas phase cylinder; 20 Pump; 21 Liquid phase container; 22 Waste tank; 23 Reaction tank; 24 Recovery container; A, B, C, D Boundary between gas and liquid phases.

Claims

1. A micromixer for a flow synthesis apparatus that continuously merges a gas phase and a liquid phase, The micromixer for a flow synthesis apparatus includes a six-way switching valve, a gas phase supply flow path, a liquid phase supply flow path, a discharge flow path, a synthesis flow path, and a sample loop; the six-way switching valve has a gas phase supply port connected to the gas phase supply flow path, a liquid phase supply port connected to the liquid phase supply flow path, a discharge port connected to a discharge flow path, a synthesis outlet connected to a synthesis flow path, and two sample loop openings connected to both ends of the sample loop, the six-way switching valve is switchable between a first flow path in which the gas or liquid phase supply flow path, the sample loop, and the discharge flow path communicate with each other, and at the same time, the liquid or gas phase supply flow path communicates with the synthesis flow path, and a second flow path in which the gas or liquid phase supply flow path communicates with the discharge flow path, and at the same time, the liquid or gas phase supply flow path, the sample loop, and the synthesis flow path communicate with each other, A micromixer for a flow synthesis apparatus, which is capable of alternately discharging the liquid phase and the gas phase into the synthesis flow path by alternately switching between the first flow path and the second flow path and discharging at least the gas phase or the liquid phase that has been flowed into the sample loop into the synthesis flow path.

2. the sample loop opening has a first opening and a second opening, 2. The micromixer for a flow synthesis apparatus according to claim 1, wherein the gas phase supply port, the first opening of the sample loop opening, the synthesis outlet, the liquid phase supply port, the second opening of the sample loop opening, and the outlet are provided in this order in a clockwise or counterclockwise direction on the hexagonal switching valve.

3. A flow synthesis apparatus comprising the micromixer for flow synthesis apparatus according to claim 1 or 2.

4. The flow synthesis apparatus according to claim 3 , wherein no pressure regulator is provided downstream of the synthesis channel.

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