JP2016013543A - Microreactor module - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a microreactor module having high heat exchange efficiency in chemical reaction and capable of making the chemical reaction more efficient.SOLUTION: A microreactor module 100 chemically reacting a reaction liquid RL inside under the temperature control via a heat transfer medium HM is composed to comprise a cylindrical case 1 having the reaction liquid inlet 11 and outlet 12 in and out of which the reaction liquid flows, and the heat transfer medium inlet 13 and outlet 14 in and out of which the heat transfer medium HM flows, and plural hollow fibers 2 disposed between the reaction liquid inlet 11 and outlet 12. Besides, the module is composed so as to make it possible to chemically react the reaction liquid RL in the hollow part of the hollow fibers 2 under the temperature control via the heat exchange by the heat transfer medium HM by making the reaction liquid RL flow in the respective hollow parts of plural hollow fibers 2 and by making the medium HM flow so that at least outside of plural hollow fibers 2 makes it possible to heat-exchange with the reaction liquid RL.

Description

  The present invention relates to a microreactor module. More specifically, the present invention relates to a microreactor module that can improve the efficiency of chemical reactions.

  A microreactor can improve the efficiency of chemical reactions in that it can facilitate control of chemical reactions, improve the yield and purity of reaction products, and increase the ratio of surface area per volume. It is attracting attention as a means of That is, the microreactor brings about an essential change with respect to a conventional chemical reaction by performing a reaction field in a micro space in a chemical reaction. For example, in the field of synthesis of pharmaceuticals and fine chemical products, Improvement of the production efficiency is expected. In addition, it is possible to efficiently and easily shift to full-scale production by numbering up (increasing the number by paralleling) as compared with the case of conventional scale-up.

  Currently, many microreactors have a channel structure in which a number of micro-sized grooves are formed in a metal plate with good thermal conductivity, and a plurality of these metal plates are stacked to increase the surface area and heat exchange. Although the efficiency is increased, the micro processing technology and assembly technology used for manufacturing the microreactor having such a configuration are technologies that require extremely precise and difficult work, and thus the manufacturing cost increases. There were problems such as poor versatility and design freedom.

  In addition, in order to simplify the manufacturing process and increase versatility and design freedom, a microreactor manufactured by changing a conventional metal or glass to plastic as a constituent material has been proposed. For example, a microreactor is disclosed in which enzyme molecules are immobilized on the inner surface of a hollow microchannel made of an inactive constituent material such as a bendable fluororesin or silicon rubber (see, for example, Patent Document 1).

  However, the microreactor disclosed in Patent Document 1 has a problem that heat exchange efficiency is not always sufficient, although some simplification is realized.

JP 2006-238760 A

  The present invention has been made in view of the above-described problems, and an object of the present invention is to provide a microreactor module that has high heat exchange efficiency in a chemical reaction and can improve the efficiency of the chemical reaction.

  According to the present invention, the following microreactor module is provided. The microreactor module of the present invention includes a hollow fiber that provides a reaction field that efficiently supplies heat to the reaction solution, and a cylindrical case that supplies a heat medium that provides a heat source to the reaction field. According to the type of chemical reaction, the function required as a microreactor, etc., it means a basic unit used as a structural unit of a microreactor alone or in combination as appropriate by parallelization or serialization.

[1] A microreactor module in which a reaction liquid is chemically reacted under temperature control via a heat medium, the reaction liquid inlet into which the reaction liquid flows in, the reaction liquid outlet through which the reaction liquid flows out, and the heat A cylindrical case having a heat medium inlet through which the medium flows and a heat medium outlet through which the medium flows; and a plurality of hollow fibers disposed between the reaction liquid inlet and the reaction liquid outlet inside the cylindrical case; The reaction liquid is caused to flow into each hollow portion of the plurality of hollow fibers, and the heat medium is allowed to flow at least outside the plurality of hollow fibers so that heat exchange with the reaction liquid is possible. The microreactor module is characterized in that the reaction liquid is chemically reacted in the hollow portion of the hollow fiber under temperature control through heat exchange by the heat medium.

[2] The microreactor module according to [1], wherein each of the plurality of hollow fibers has an outer diameter of 2 to 1000 μm, a film thickness of 1 to 100 μm, and a length of 50 to 2000 mm.

[3] The plurality of hollow fibers are each formed of a fluorine resin, silicone, polyolefin resin, polyimide resin, polyether ether ketone resin, aromatic resin, metal, carbon, or glass. The microreactor module according to [1] or [2].

[4] The microreactor module according to any one of [1] to [3], wherein the plurality of hollow fibers are a bundle of 2 to thousands.

[5] The plurality of hollow fibers are an inlet bundling portion and an outlet bundling portion that are bundled in a more dense state than the central portion in the longitudinal direction at the reaction liquid inlet and the reaction liquid outlet of the cylindrical case. The microreactor module according to any one of [1] to [4], wherein:

[6] The plurality of hollow fibers expand radially from the inlet binding portion and the outlet binding portion, respectively, in the central portion between the inlet binding portion and the outlet binding portion, and the inlet binding portion and The microreactor module according to [5], wherein a central bundling portion that is bundled in a state that is less sparse than the outlet bundling portion is formed.

[7] The inside of the cylindrical case is traversed in a direction perpendicular to the longitudinal direction thereof, and the central binding portion is partitioned into 2 to 50 space areas at equal intervals, and the hollow fiber can be inserted. In addition, the microreactor module according to [6], further including 1 to 49 diffusion shelf plates having a configuration capable of passing and flowing the heat medium.

[8] The microreactor according to [7], wherein the diffusion shelf has a mesh or a plurality of through holes through which the hollow fiber can be inserted and through which the heat medium can pass and flow. module.

According to the present invention, there is provided a microreactor module having high heat exchange efficiency in a chemical reaction and capable of increasing the efficiency of the chemical reaction. Specifically, the following effects (1) to (7) can be obtained.
(1) Since it is a hollow fiber type microreactor module using a hollow fiber, there is little difficulty in micromachining, and since a wide variety of hollow fibers can be used, the applicable range can be expanded.
(2) When the flow rate of the reaction liquid is constant, the reaction time can be adjusted by changing the length of the hollow fiber. Further, the reaction time can be adjusted by changing the flow rate.
(3) The production amount can be adjusted by the number of hollow fibers bound. Furthermore, numbering up can be easily performed by using modules in parallel, and a smooth transition to full-scale production can be achieved.
(4) By changing the constituent material of the hollow fiber according to the purpose of use, heat resistance, solvent resistance, pressure strength, heat exchange efficiency, cost, and the like can be appropriately selected.
(5) By changing the outer diameter and film thickness of the hollow fiber according to the purpose of use, the pressure strength, the heat exchange efficiency, etc. can be appropriately selected.
(6) By arranging the cooling microreactor module after the reaction microreactor module, side reactions can be suppressed.
(7) A multi-stage chemical reaction through several steps can be handled by arranging a plurality of microreactor modules in series, which is optimal for flow chemistry.

It is a section explanatory view showing typically one embodiment of the microreactor module of the present invention. It is a top view which shows the diffusion shelf board used for one embodiment of the microreactor module of the present invention, (a) has a mesh, (b) is a passage of a hollow fiber and a passage of a heat carrier, A case where the flow hole has a through-hole having substantially the same size, and (c) a case where the insertion hole of the hollow fiber and the passage of the heat medium, and the flow hole have a through-hole having a different size are shown. It is a perspective view which shows typically the usage example of the diffusion plate shelf shown in FIG.2 (c). In an Example, it is a chart figure which shows typically the flow at the time of comprising a chemical reaction system using the microreactor module of this invention, giving a chemical reaction to a raw material, and commercializing. It is a chart figure which shows typically the flow at the time of combining the microreactor module for reaction, and the microreactor module for cooling. It is a chart figure which shows the flow of a multistage chemical reaction system typically. In Example 1, it is a graph which shows the relationship between the flow rate of the reaction liquid in a microreactor module, and the temperature of the reaction liquid in the exit side of a microreactor module. In Example 2, it is a graph which shows the relationship between the flow rate of the reaction liquid in the microreactor module for cooling, and the temperature of the reaction liquid on the exit side of the microreactor module for cooling. In Comparative example 1, it is a graph which shows the relationship between the flow rate of the reaction liquid in a fluorine resin tube, and the temperature of the reaction liquid in the exit side of a fluorine resin tube.

  Hereinafter, an embodiment of a microreactor module according to the present invention will be specifically described with reference to the drawings.

  As shown in FIG. 1, the microreactor module of the present embodiment is a microreactor module 100 in which a reaction solution RL is chemically reacted under temperature control via a heat medium HM. A cylindrical case 1 having a reaction liquid inlet 11 into which RL flows in and a reaction liquid outlet 12 through which it flows out, a heat medium inlet 13 into which the heat medium HM flows in, and a heat medium outlet 14 through which it flows; A plurality of hollow fibers 2 disposed between the reaction liquid inlet 11 and the reaction liquid outlet 12, and the reaction liquid RL is caused to flow into the respective hollow portions of the plurality of hollow fibers 2 and a heat medium. The HM is flowed so that at least the outside of the plurality of hollow fibers 2 can exchange heat with the reaction liquid RL, and the reaction liquid RL is controlled in the hollow portion of the hollow fiber 2 through heat exchange with the heat medium HM. Under the by chemical reaction, is characterized in that the finally taken out as product PD. In the microreactor module 100 of the present embodiment, it is preferable that the entire cylindrical case 1 is covered with a heat insulating and heat insulating cover 4. Although not shown, when the homogeneous catalyst is not introduced before the microreactor module 100, the hollow fiber 2 can include a heterogeneous catalyst therein.

  Here, the reaction liquid RL is not particularly limited. However, since the reaction liquid RL flows in a thin hollow fiber of a micron unit, it is preferable that the reaction liquid RL has high fluidity that does not inhibit the flow. Moreover, there is no restriction | limiting in particular as the heat medium HM, For example, water, silicone oil, ethylene glycol aqueous solution etc. can be mentioned. Specific examples include commercially available silicon oil (manufactured by Shin-Etsu Chemical Co., Ltd., trade name: KF-96), ethylene glycol aqueous solution (manufactured by Tokyo Rika Kikai Co., Ltd., trade name: Nibrine Z-1), and the like. it can. The reaction liquid RL and the heat medium HM are preferably configured as flows facing each other in the microreactor module 100 in order to realize efficient heat exchange. In this case, the heat medium HM can exchange heat with the reaction liquid RL at least outside the plurality of hollow fibers 2 (preferably, a gap is provided between the plurality of hollow fibers 2 and also in this gap). It is preferable to make it flow. Note that, as described above, the microreactor module 100 of the present embodiment can be used in parallel and / or in series as necessary.

  The size of the cylindrical case 1 used in the present embodiment is not particularly limited. For example, the cylindrical case 1 has a diameter of 10 to 200 mm and a length of 50 to 50 corresponding to the size of the hollow fiber 2 described later. It is preferably 2000 mm. Moreover, it is preferable that it is formed from constituent materials, such as a metal and a synthetic resin, at the point of mechanical strength, heat resistance, corrosion resistance, and workability. For example, fluorine resins such as stainless steel and polytetrafluoroethylene (PTFE), polyether ether ketone resins, polyimide resins, polyolefin resins such as polypropylene (PP), and the like are preferably used. The cylindrical case has a heat release loss from the outer cylinder side due to heating of the heat medium, and in order to prevent this, it is preferable to have a structure in which the entire cylindrical case is covered with the heat insulating and heat insulating cover 4. There is no restriction | limiting in particular as the heat insulation heat insulation cover 4, A general purpose thing can be used.

  As shown in FIG. 1, the cylindrical case 1 has a reaction liquid inlet 11, a reaction liquid outlet 12, a heat medium inlet 13, and a heat medium outlet 14.

  The plurality of hollow fibers 2 used in the present embodiment preferably have an inner diameter of 2 to 1000 μm, more preferably 10 to 700 μm, and particularly preferably 100 to 500 μm. Since the back pressure resistance increases as the inner diameter of the hollow fiber decreases, and the heat exchange efficiency decreases as the inner diameter increases, it is preferable to employ an optimal inner diameter depending on the type of reaction, required conditions, and the like. Moreover, as a film thickness, it is preferable that it is 1-100 micrometers, and it is more preferable that it is 5-50 micrometers. When the thickness is less than 1 μm, the pressure resistance may decrease, and when it exceeds 100 μm, the heat conduction may deteriorate and the heat exchange efficiency may decrease. Furthermore, as length, it is preferable that it is 50-2000 mm. If it is less than 50 mm, a sufficient heat exchange effect may not be obtained, and if it exceeds 2000 mm, the back pressure resistance may increase excessively.

  In addition, the hollow fiber 2 is made of fluorine resin, silicone, polyimide resin, polyether ether ketone resin, polyolefin resin, aromatic resin, metal (for example, stainless steel), carbon, or glass, respectively, as a constituent material. It is preferably formed. Among them, taking into consideration the difficulty, versatility, design freedom, etc. of manufacturing hollow fibers, synthetic resins such as fluorine resins, silicones, polyolefin resins, polyimide resins, polyether ether ketone resins, aromatic resins, etc. More preferably. In addition to the above synthetic resins, hollow fiber materials with excellent mechanical strength (pressure strength), heat resistance, corrosion resistance, etc., such as stainless steel (specifically, depending on the type of reaction and required functions) Specifically, SUS316) or the like may be used.

  Moreover, it is preferable that 2 to several thousand hollow fibers are bundled, and more preferably 5 to 1000 hollow fibers. If it exceeds several thousand, manufacturing difficulty and cost may increase.

  Further, the hollow fiber 2 forms an inlet bundling portion 22 and an outlet bundling portion 23 that are bundled in a denser state than the central portion in the longitudinal direction at the reaction liquid inlet 11 and the reaction liquid outlet 12 of the cylindrical case 1. It is preferable to do. In particular, when the number of bundles increases, it is preferable because operations such as bundling can be simplified.

  Further, the hollow fiber 2 expands radially from the inlet binding portion 22 and the outlet binding portion 23 in the central portion between the inlet binding portion 22 and the outlet binding portion 23, respectively, and from the inlet binding portion 22 and the outlet binding portion 23. Forming the central bundling portion 24 that is bundled in a sparse state can secure a passage for the heat medium and realize efficient heat exchange.

  As shown in FIGS. 1 to 3, the inside of the cylindrical case 1 is traversed in a direction perpendicular to the longitudinal direction thereof, and the central binding portion 24 is partitioned into space regions of 2 to 50 at equal intervals, and the hollow fiber It is preferable that 1 to 49 diffusion shelf plates 3 having a configuration in which 2 can be inserted and the heat medium HM can pass and flow are further provided. FIG. 1 shows a case where three diffusion shelf boards 3 are installed. With this configuration, the hollow fiber 2 can be arranged in a balanced manner for efficient heat exchange with the heat medium HM, and the heat medium HM can be evenly distributed over the entire surface of the hollow fiber 2. It becomes possible to spread.

  As the diffusion shelf 3, for example, a mesh diffusion shelf 31 (see FIG. 2A) having a mesh through which the hollow fiber 2 can be inserted and through which the heat medium HM can pass and flow. Uniform hole diffusion shelf 32 (see FIG. 2 (b)) having a plurality of through holes of uniform hole diameter and different diameter hole diffusion shelf 33 (FIG. 2 (c) and FIG. 3) having through holes of different diameters. Reference).

  Examples of the constituent material of the diffusion shelf 3 include those formed from stainless steel, fluorine resin, and the like in consideration of heat resistance, corrosion resistance, strength, and the like. Moreover, it is preferable that the hole diameter of the diffusion shelf board 3 is made slightly larger than the outer diameter of the hollow fiber 2 so that the heat medium can pass therethrough. Specifically, in the case of the mesh diffusion shelf 31, the size of the mesh is preferably about twice the outer diameter of the hollow fiber 2. In the case of the uniform hole diffusion shelf 32, the size of the uniform hole is preferably about twice the outer diameter of the hollow fiber 2. In addition, in the case of the different-diameter hole diffusion shelf plate 33, it is preferable to configure the hole for the hollow fiber 2 and the hole for the heat medium HM. The total size of the holes for the heat medium HM is preferably about 20 to 30% of the entire area of the different-diameter diffusion shelf 33. Furthermore, it is preferable that the hole for the heat medium HM is divided into 3 to 4 small holes instead of one hole, and is unevenly distributed on one of the left and right sides. As for the arrangement, as shown in FIG. 3, the holes for the heat medium HM are alternately shifted to the left and right for each different-diameter diffusion shelf 33 to stir and replace the heat medium HM to form a cylinder. It is preferable in that the entire case 1 can be distributed without any hesitation.

  As described above, in the chemical reaction, when the homogeneous catalyst CA (see FIG. 4) is not introduced before the microreactor module 100, the hollow fiber 2 can contain a heterogeneous catalyst therein. In this case, the heterogeneous catalyst can be configured, for example, as a wire catalyst formed in the shape of a wire having a micro size diameter, a coated catalyst applied to the inner wall thereof, or a filled porous catalyst. It is preferable that any heterogeneous catalyst arrangement does not hinder the flow of the reaction liquid RL.

  As shown in FIG. 4, a chemical reaction system can be configured around the microreactor module 100 of the present invention. That is, it can be composed of components such as a liquid feed pump (P1 to P3), a mixer module 200, a heat medium circulation thermostat 300, a pressure sensor PS, a temperature sensor (TS1, TS2, TS3), and piping. There is no restriction | limiting in particular as a liquid feeding pump (P1-P3), According to a use, it can select suitably. For example, a plunger type pump, a syringe type pump, a tube pump, a valveless plunger pump, etc. can be mentioned.

  The mixer module 200 is used to uniformly mix the raw material M1, the raw material M2, and the uniform catalyst CA supplied via the liquid feed pumps (P1 to P3) and introduce them into the microreactor module 100. For example, when mixing the raw materials M1 and M2 and the uniform catalyst CA, there can be mentioned a mixer module or the like that is introduced from three branch inlets and filled with glass balls of about 10 μm as shown in FIG.

  The heat medium circulation thermostat 300 is used to supply the heat medium HM corresponding to the reaction temperature to the microreactor module 100. In addition, if necessary, the liquid after the reaction is rapidly cooled to stop the side reaction, and a cooling heat medium circulation thermostat (hereinafter referred to as “refrigerant circulation thermostat”) 400 is already used as shown in FIG. One unit can be prepared to handle it. In this case, the microreactor module 100 for cooling can be attached after the microreactor module 100 for reaction.

  The pressure sensor PS is installed at the reaction solution inlet 11 (see FIG. 1) of the microreactor module 100 and is used for monitoring the pressure during the reaction. Moreover, as shown in FIGS. 4-6, temperature sensor (TS1-TS7) is a reaction liquid inlet_port | entrance of the microreactor module 100 according to the number of stages of the chemical reaction (the number of installed microreactor modules 100). 11 and the reaction liquid outlet 12 and the temperature of the heat medium in the cylindrical case 1 are used for monitoring. For example, in the case shown in FIG. 4, in the flow direction, in the order of TS1, TS3, and TS2, in the case of FIG. 5, in the order of TS1, TS3, TS2, TS5, and TS4, and in the case shown in FIG. TS1, TS3, TS2, TS5, TS4, TS7, and TS6 are arranged in this order. TS3, TS5, and TS7 are used to monitor the temperature of the heat medium in the cylindrical case 1.

  The reaction system shown in FIG. 4 is a one-stage chemical reaction system. However, as described above, for a multi-stage chemical reaction system that undergoes several steps according to the number of chemical reaction stages, etc., a reaction micro reaction system is used. This can be dealt with by arranging a plurality of reactor modules in series. As an example, a three-stage chemical reaction system is shown in FIG.

  Hereinafter, the present invention will be described more specifically with reference to examples. However, the present invention is not limited to these examples.

(Example 1)
Example 1 shows a configuration centering on a microreactor module 100 as shown in FIG. That is, a tube-type roller pump was used as the liquid feed pump (P1), a heating circulation thermostat was used as the heat medium circulation thermostat 300, and a temperature sensor (TS2) was used.

  As the microreactor module 100, the following was used. That is, as the hollow fiber 2 in FIG. 1, a bundle of 56 fluororesin hollow fibers having an inner diameter of 500 μm, a film thickness of 35 μm, an outer diameter of 570 μm, and a length of 300 mm was used. As the cylindrical case 1, a fluorine-based resin having an outer diameter of 22 mm and a length of 412 mm was used, and the whole was covered with a heat insulating heat insulating cover 4. Further, as the diffusion shelf plate 3, one fluororesin diffusion shelf plate (see FIG. 2B) having a hole diameter of 1.0 mm was used.

  As shown in FIG. 4, a liquid feed pump (P1) and a heat medium circulation thermostat 300 were connected to the microreactor module 100 obtained as described above. Silicon oil (trade name, manufactured by Shin-Etsu Chemical Co., Ltd.), in which 20 ° C. water is sent as a reaction solution RL from the liquid feed pump (P1) to the microreactor module 100 and heated from the heat medium circulating thermostat 300 to 80 ° C. : KF-96) was circulated as a heat medium. A temperature sensor TS2 was attached to the outlet side of the microreactor module 100, and a change in temperature was measured. The flow rate of the heat medium in the heat medium circulation thermostat 300 was 600 ml / min. The flow rate of water at 20 ° C. from the liquid feed pump (P1) was changed to 8, 22, 32, 40, 65, 85, 110, and 130 ml / min, and the heat exchange efficiency at each flow rate was evaluated. From the value of 3.3 ml of the internal capacity of the microreactor module 100, the residence time at each flow rate is 24.8 seconds at 8 ml / min, 9.0 seconds at 22 ml / min, 6.2 seconds at 32 ml / min, 40 ml / min. It is 5.0 seconds in minutes, 3.0 seconds at 65 ml / min, 2.3 seconds at 85 ml / min, 1.8 seconds at 110 ml / min, and 1.5 seconds at 130 ml / min. The relationship between the flow rate of the reaction liquid in the microreactor module 100 and the temperature of the reaction liquid on the outlet side of the microreactor module 100 is shown in FIG. As a result, it was found that the microreactor module 100 was suitable as a microreactor because the high temperature was maintained even at 1.5 seconds on the high flow rate side and heat exchange was performed instantaneously.

(Example 2)
Example 2 shows a configuration in which a reaction microreactor module and a cooling myloreactor module are combined as shown in FIG. As shown in FIG. 5, similarly to Example 1, 20 ° C. water was fed from the liquid feed pump (P1) to the microreactor module 100 as the reaction liquid RL. After the microreactor module 100, the same microreactor module 100 was connected in series. The former was used for reaction, and silicon oil (trade name: KF-96, manufactured by Shin-Etsu Chemical Co., Ltd.) heated to 80 ° C. from the heat medium circulation thermostat 300 was circulated as a heat medium. The latter was used for cooling, and an ethylene glycol aqueous solution (manufactured by Tokyo Rika Kikai Co., Ltd., trade name: Nybrine Z-1) was flowed as a cooling heat medium (refrigerant) from the newly added refrigerant circulating thermostat 400. . The flow rate of water at 20 ° C. from the liquid feed pump (P1) was changed to 8, 22, 32, 40, 65, 85, 110, and 130 ml / min, and the heat exchange efficiency at each flow rate was evaluated. From the value of 3.3 ml of the internal capacity of the cooling microreactor module 100, the residence time at each flow rate is 24.8 seconds at 8 ml / min, 9.0 seconds at 22 ml / min, 6.2 seconds at 32 ml / min, It is 5.0 seconds at 40 ml / min, 3.0 seconds at 65 ml / min, 2.3 seconds at 85 ml / min, 1.8 seconds at 110 ml / min, and 1.5 seconds at 130 ml / min. The relationship between the flow rate of the reaction liquid in the cooling microreactor module 100 and the temperature of the reaction liquid on the outlet side of the cooling microreactor module 100 is shown in FIG. As in Example 1, it was found that the heat exchange efficiency is very good and the reaction can be stopped and side reactions can be suppressed by being able to cool instantaneously.

(Comparative Example 1)
In Example 1, except that the hollow fiber 2 of the microreactor module 100 was replaced with one fluororesin tube (inner capacity 3.3 ml) having an outer diameter of 3 mm, an inner diameter of 2 mm, and a length of 1030 mm. Same as Example 1. Evaluation was performed in the same manner as in Example 1. The flow rate of 20 ° C. water from the liquid feed pump (P1) was changed to 8, 22, 32, 40, 65, 85, and 110 ml / min, and the heat exchange efficiency at each flow rate was evaluated. From the value of 3.3 ml of the internal capacity of the fluororesin tube, the residence time at each flow rate is 24.8 seconds at 8 ml / minute, 9.0 seconds at 22 ml / minute, 6.2 seconds at 32 ml / minute, 40 ml / minute. It is 5.0 seconds at minutes, 3.0 seconds at 65 ml / min, 2.3 seconds at 85 ml / min, and 1.8 seconds at 110 ml / min. FIG. 9 shows the relationship between the flow rate of the reaction liquid in the fluororesin tube and the temperature of the reaction liquid on the outlet side of the fluororesin tube. Compared to Example 1, the heat exchange efficiency was very poor, and it was found that the above-mentioned fluororesin tube was not suitable as a microreactor.

  The microreactor module of the present invention is effectively used in the fields of various synthetic chemical industries for producing pharmaceuticals, fine chemical products, and the like that are required to make chemical reactions more efficient.

DESCRIPTION OF SYMBOLS 1 Cylindrical case 2 Hollow fiber 3 Diffusion shelf board 4 Thermal insulation heat insulation cover 11 Reaction liquid inlet 12 Reaction liquid outlet 13 Heat medium inlet 14 Heat medium outlet 22 Inlet binding part 23 Outlet binding part 24 Central binding part 31 Mesh diffusion shelf 32 Uniform Hole diffusion shelf 33 Different diameter hole diffusion shelf 100 Microreactor module 200 Mixer 300 Heat medium circulation thermostat 400 Refrigerant circulation thermostat CA Uniform catalyst HM Heat medium M1 to M4 Raw material P1 to P3 Feed pump PD Product PS Pressure sensor RL reaction liquid TS1-TS7 Temperature sensor

Claims (8)

Inside, a microreactor module that chemically reacts a reaction solution under temperature control via a heat medium,
A cylindrical case having a reaction liquid inlet and a reaction liquid outlet through which the reaction liquid flows, a heat medium inlet and a heat medium outlet through which the heat medium flows; and
A plurality of hollow fibers disposed between the reaction solution inlet and the reaction solution outlet inside the cylindrical case,
The reaction liquid is caused to flow in the respective hollow portions of the plurality of hollow fibers, and the heat medium is caused to flow at least outside of the plurality of hollow fibers so that heat exchange with the reaction liquid is possible. A microreactor module, wherein a reaction liquid is chemically reacted in the hollow portion of the hollow fiber under temperature control through heat exchange with the heat medium.   2. The microreactor module according to claim 1, wherein each of the plurality of hollow fibers has an inner diameter of 2 to 1000 μm, a film thickness of 1 to 100 μm, and a length of 50 to 2000 mm.   The plurality of hollow fibers are each formed of fluorine resin, silicone, polyolefin resin, polyimide resin, polyether ether ketone resin, aromatic resin, metal, carbon, or glass. The microreactor module described in 1.   The microreactor module according to any one of claims 1 to 3, wherein 2 to several thousand of the plurality of hollow fibers are bundled.   The plurality of hollow fibers form an inlet bundling portion and an outlet bundling portion that are bundled in a denser state than the central portion in the longitudinal direction at the reaction liquid inlet and the reaction liquid outlet of the cylindrical case. The microreactor module according to any one of claims 1 to 4.   The plurality of hollow fibers expand radially from the inlet binding portion and the outlet binding portion, respectively, at the central portion between the inlet binding portion and the outlet binding portion, and thereby the inlet binding portion and the outlet binding portion. The microreactor module according to claim 5, wherein a central bundling portion is formed in a state of being sparser than a portion.   It is possible to cross the inside of the cylindrical case in a direction perpendicular to the longitudinal direction, partition the internal space of the cylindrical case into 2 to 50 space areas at equal intervals, and allow the hollow fiber to be inserted. The microreactor module according to claim 6, further comprising 1 to 49 diffusion shelf plates having a configuration capable of passing and flowing the heat medium.   The microreactor module according to claim 7, wherein the diffusion shelf plate has a mesh or a plurality of through holes through which the hollow fiber can be inserted and through which the heat medium can pass and flow.

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