JP6647858B2 - Micro reactor - Google Patents

Description

The present invention relates to a microreactor that performs various reactions in a microchannel.

The microreactor can efficiently perform heat exchange because the fluid is controlled in a minute space. It is difficult to control the reaction on the large scale, and it is relatively easy to control even the reaction with the risk of explosion. Microreactors are small and have a small footprint. Due to such advantages, not only research uses but also industrial uses are being studied.

For example, Patent Literature 1 describes a method of mixing an oil and water while applying a shearing force to adjust an emulsion using a microreactor. In Example 1, a 1% by mass aqueous solution of sodium dodecyl sulfate is used as an aqueous phase, and a dodecane solution is used as an oil phase.

Patent Literature 2 describes a method of manufacturing a flow path plate by sintering a synthetic resin material. FIG. 1 illustrates a microreactor in which two cover bodies and a flow path plate disposed therebetween are fastened with bolts and nuts.

Patent Document 3 describes a microreactor including a wireless device, a pressure plate, a measurement plate, and a channel plate. FIG. 7 shows screws.

Patent Document 4 describes that a flow path plate is formed of a rubber sheet. It is described that a rubber sheet or the like is sandwiched between rigid holders made of a resin plate or a metal plate and fixed with screws.

Patent Literature 5 describes a photoreaction microreactor including a housing upper part, a lid plate, a flow path plate, and a housing lower plate. The lid plate is made of a material that transmits light.

International Publication No. WO2009 / 119578 JP 2009-279468 A Japanese Patent No. 4706353 JP 2013-188677 A International Publication No. WO2012 / 157052

In Patent Documents 1 to 4, it is necessary to separately prepare a microreactor having a micropath having a different pattern for each application. For this reason, users had to purchase a microreactor specialized for each application.

The microreactor of Patent Document 5 is considered to integrate the microreactor using screws. However, the lid plate and the flow path plate are welded, and it is not intended that any one of the plurality of flow path plates be selected and replaced.

An object of the present invention is to provide a microreactor in which an arbitrary flow path plate can be selected from a plurality of flow path plates according to an application and can be easily replaced with the flow path plate.

A microreactor comprising a first cover, a second cover, and a flow path plate disposed between the first cover and the second cover, wherein the microreactor includes an outlet and a plurality of inlets, The flow path plate has a micro flow path connecting the inlet and the outlet in an arbitrary pattern, and the microreactor is a replacement plate for a plurality of flow path plates having micro flow paths of the same or different patterns from each other. The first cover and the second cover are provided with connecting holes communicating with each other, and the first cover, the flow path plate, and the second cover are connected to each other by inserting a fixture into the connecting holes. The above-mentioned problem is solved by a microreactor which can be fixed to the flow channel plate and can be exchanged by removing the fixture. For example, the user can select an arbitrary flow path plate suitable for the application from a plurality of flow path plates, and set the microplate in the microreactor to perform an arbitrary reaction.

It is preferable to arrange a transparent plate between the first cover and the flow path plate. It becomes possible to observe the micro flow channel or irradiate the micro flow channel with light through the transparent plate. Similarly, it is preferable to arrange a transparent plate between the second cover and the flow path plate.

It is preferable to provide a viewing window on at least one of the first cover and the second cover for visually recognizing the flow path plate via a transparent plate. This makes it possible, for example, to observe the progress of the reaction with an optical microscope or the like. In addition, for example, when a photocatalyst or the like is used, light can be emitted from a viewing window.

The fixing tool is a screw having a threaded portion and a non-threaded portion having no thread, and the threaded portion is provided with the first cover, the flow path plate, and the second cover in a state where the first cover and the second cover are assembled. It is preferable that one of the covers and the fixing member are disposed at a portion where the fixing member is screwed, and the non-threaded portion closes the connection hole to increase airtightness and liquid tightness. The first cover, the second cover, and the flow path plate are securely fastened by the threaded portions, and the connection holes are closed by the non-threaded portions, so that the airtightness and liquid tightness of the microchannel can be improved.

The fixture is preferably a multi-thread screw. This makes it possible to reduce the number of rotations of the screw and to quickly fasten or disassemble the first cover, the second cover, and the flow path plate.

The first cover preferably has three or more inlets. Accordingly, it is possible to increase the number of patterns of the flow path and to cope with more applications.

It is possible to provide a microreactor in which an arbitrary flow path plate can be selected from a plurality of flow path plates according to the application and can be easily replaced with the flow path plate.

FIG. 3 is an exploded perspective view of one embodiment of the macro reactor of the present invention. It is a perspective view of the microreactor of FIG. 1 which shows the state which fastened each member with the fixture. FIG. 2 is a diagram schematically illustrating an example of a use state of the microreactor of FIG. 1. It is a top view showing an example of a channel plate. It is a top view showing an example of a channel plate. It is a top view showing an example of a channel plate. It is a top view showing an example of a channel plate. It is sectional drawing in the AA part of FIG. It is a front view which shows an example of a fixture. It is sectional drawing in the BB part of FIG. It is sectional drawing of the microreactor of another embodiment, It cut | disconnected in the same location as FIG.

An embodiment for carrying out the present invention will be described with reference to the drawings.

1 to 5 show one embodiment of the microreactor of the present invention. The microreactor 1 according to the present embodiment includes a first cover 11, a first transparent plate 12, a set of a plurality of flow path plates 13, a second transparent plate 14, a second cover 15, and a plurality of fixed members. Tool 51.

The first cover 11 and the second cover 15 are plate-shaped members, and are made of stainless steel. As shown in FIG. 1, since the flow path plate is sandwiched between the first transparent plate 12 and the second transparent plate 14, the first cover 11 and the second cover 15 are used when the microreactor 1 is used or transported. What is necessary is just to have enough strength to easily bend or break. For example, it may be made of a synthetic resin material such as engineer plastic, a metal material such as stainless steel, aluminum or silicon, a glass such as quartz glass or heat-resistant glass, or a transparent ceramic. In the present embodiment, the first cover 11 and the twelfth cover 15 are made of SUS304 having high corrosion resistance.

The first cover 11 is provided with three inlets 16, 17, 18 and one outlet 19. The inlets 16, 17, 18 and the outlet 19 are holes penetrating through the first cover 11 in the thickness direction. The first transparent plate 12 described later is provided with a plurality of through holes communicating with the inlets 16, 17, 18 and the outlet 19, respectively.

The inlets 16, 17, 18 are provided at the 12 o'clock, 3 o'clock, and 9 o'clock positions. The discharge port 19 is provided at the position of 6 o'clock. That is, the inlet 16 and the outlet 19 are provided in a cross shape. The inner walls of the inlets 16, 17, 18 and the outlet 19 are female screws. As shown in FIG. 3, a male screw provided at an end of a pipe communicating with the reaction material supply units 20, 21, 22 can be screwed and fixed to female screws of the introduction ports 16, 17, 18. . Similarly, a male screw provided at the end of the tube communicating with the reactant storage unit 23 can be screwed and fixed to the female screw of the outlet 19. The relationship between the female screw and the male screw may be interchanged.

The reaction material supply units 20, 21, and 22 shown in FIG. 3 can be composed of, for example, a syringe and a pressurizing device that presses an end of a piston of the syringe. The reactant storage part 23 can be composed of, for example, a container such as a beaker or an airtight container.

In the microreactor 1 of the present embodiment, the flow path plate 13 is sandwiched between the first transparent plate 12 and the second transparent plate 14. The channel plate 13 is provided with a slit 24 penetrating in the thickness direction of the channel plate 13. A minute path is formed by sandwiching the flow path plate 13 provided with the slit 24 between the first transparent plate 12 and the second transparent plate 14. The plurality of flow path plates 13 of the present embodiment are plate-like members made of stainless steel. A stainless steel plate can be cut to an arbitrary size, and a slit having an arbitrary pattern can be easily formed by laser machining or electric discharge machining. Although the flow path plate 13 is a thin plate, a stainless steel plate is excellent in strength. Therefore, it is preferable that the channel plate is made of a stainless steel material because it is easy to handle when the microreactor 1 is disassembled to clean a micropath. The channel plate 13 may be made of another metal material such as silicon, a synthetic resin material, or the like.

In the present embodiment, the first transparent plate 12 and the second transparent plate 14 are made of quartz glass. The transparent plate may be made of, for example, glass such as quartz glass or heat-resistant glass, transparent ceramics, or synthetic resin such as silicone. Quartz glass is preferable because it is chemically stable and suitable for observing the flow path.

The microreactor 1 of the present embodiment includes a total of four replaceable flow path plates 13 as shown in FIG. As shown in FIG. 4, the first flow path plate 13 a has a first path 26 inclined toward the junction 25, a second path 27 inclined toward the junction, and a discharge port 19 from the junction 25. A Y-shaped slit is provided at the center of the third path 28 extending toward the center. The first path 26, the second path 27, and the third path 28 communicate with each other via the junction 25. The first path 26 connects to the inlet 16, the second path 27 connects to the inlet 18, and the third path 28 connects to the outlet 19. Since the inlet 17 is not used, it is sealed with a lid (not shown). The black dots in FIG. 4 indicate the positions of the introduction ports 16, 17, and 18. The same applies to FIGS. 5 to 7. The flow path plate 13a in FIG. 4 is suitable for, for example, mixing an aqueous substance, an oily substance, and an emulsifier to form an emulsion. For example, a mixture of an aqueous substance and an emulsifier is supplied from the first path 26, an oily substance is supplied from the second path 27, and the emulsion is discharged from the third path 28.

The flow path plate 13b in FIG. 5 has a pattern in which a fourth path 29 extending toward the junction 25 is added to the flow path plate 13a. The fourth path 29 is provided between the first path 26 and the second path 27, and communicates with the third path 28 via the junction 25. The first route 26, the second route 27, the third route 28, and the fourth route 29 communicate with each other via the junction 25. The first path 26 connects to the inlet 16, the second path 27 connects to the inlet 18, and the fourth path 29 connects to the inlet 17. The third path 28 connects to the outlet 19. The flow path plate 13b in FIG. 5 is suitable, for example, when mixing any reaction substrate A, any reaction substrate B, and any catalyst to obtain a reactant. At this time, for example, the reaction substrate A is supplied from the first path 26, the reaction substrate B is supplied from the second path 27, the catalyst is supplied from the fourth path 29, and the reactant is discharged from the third path 28. In the flow path plate 13b, three kinds of substances are mixed at the same time.

The flow path plate 13c of FIG. 6 includes a first path 31 extending toward the first junction 30, a second path 32 extending toward the first junction 30, a first path 30 and a second path 32. A third path 34 connecting the first junction 33 to the second junction 33, a fourth path 35 extending toward the second junction 33, and a fifth path 36 extending from the second junction 33 toward the outlet 19. It has a communicating pattern. The first path 31 connects to the inlet 17, the second path 32 connects to the inlet 18, the fourth path connects to the inlet 16, and the fifth path connects to the outlet 19. The flow path plate 13c of FIG. 6 is suitable for the following uses, for example. For example, in the presence of any catalyst A, any reaction substrate A is reacted with any reaction substrate B to generate any reactant C. Thereafter, it is suitable for a case where the reactant C is reacted with an arbitrary reaction substrate D in the presence of the catalyst A to obtain an arbitrary reactant E. In this example, the reaction substrate A and the catalyst A are supplied from the first path 31, the B reaction substrate B is supplied from the second path 32, the reactant C is generated in the course of flowing through the third path, and the reaction substrate D is The reactant E is supplied from the fourth path, is generated in the course of flowing through the fifth path 36, and is discharged from the discharge port 19. In the flow path plate 13d of FIG. 7, it is possible to mix two types of substances and then mix another type of substance. In this flow path plate 13c, it becomes possible to mix another substance after mixing two substances.

The flow path plate 13d in FIG. 7 includes a first path 38 extending toward the first junction 37, a second path 39 extending toward the first junction 37, the first junction 37 and the second A third path 41 connecting the second junction 40 to the second junction 40, a fourth path 42 extending toward the second junction 40, and a fifth path 43 extending from the second junction 40 toward the outlet 19 It has a communicating pattern. The first path 38 connects to the inlet 17, the second path 37 connects to the inlet 18, the fourth path 42 connects to the inlet 16, and the fifth path 43 connects to the outlet 19. The third path 41 has a plurality of curved points 44 and has a shape meandering left and right. The flow path plate 13d in FIG. 7 is suitable for the following uses, for example. Any reaction substrate A is reacted with any reaction substrate B in the presence of any catalyst A to generate any reactant C. Thereafter, it is suitable for a case where the reactant C is reacted with an arbitrary reaction substrate D in the presence of the catalyst A to obtain an arbitrary reactant E. In this example, the reaction substrate A and the catalyst A are supplied from the first path 38, the reaction substrate B is supplied from the second path 39, and the resulting reactant C flows through the meandering third path 41. Occurs in The reaction substrate D is supplied from the fourth passage 42 and is mixed with the reactant C at the junction 40. As a result, a reactant E is generated in the fifth route 43. Reactant E exits from fifth path 36. In the flow path plate 13d, since the third path 41 is meandering to the left and right, a sufficient time is required to allow the substance supplied from the first path 38 and the substance supplied from the second path 39 to react with each other and to mix well. Can be. Therefore, when the reaction substrate A supplied from the first path and the reaction substrate B supplied from the second path do not have enough time to react in the third linear path 34 of the flow path plate 13c, or when the compound A and B The channel plate 13d may be used when the compound is not well mixed.

Conventionally, a three-hole microreactor having two inlets and one outlet has been widely used. Such a microreactor was poor in versatility. As in the microreactor 1 of the present embodiment, by setting the number of inlets to three or more and making the flow path plate replaceable, the versatility of the microreactor can be significantly improved. In other words, by making the flow path plate 13 having three or more inlets replaceable, it is possible to perform various reactions with one microreactor.

The microreactor 1 of the present embodiment includes one flow path plate 13a, 13b, 13c, 13d. For this reason, by exchanging the flow channel plate by the reaction performed using the microreactor 1, it is possible to cope with various types of reactions with one microreactor.

Although the microreactor of the present embodiment uses one channel plate of a different kind one by one, it may be configured to include a plurality of channel plates of the same type. That is, it is preferable that a plurality of at least one or more flow path plates selected from the group consisting of the flow path plates 13a, 13b, 13c, and 13d to be allowed to overlap is provided. For example, a plurality of flow path plates 13a and a plurality of flow path plates 13b may be provided. Further, for example, a plurality of flow path plates 13b may be provided. If the same type of channel plate is prepared, the reaction can be continued by replacing the micro channel of one channel plate with the other channel plate when the micro channel is clogged or broken. The replaced channel plate can be cleaned or repaired during that time. In addition, if a plurality of the same type of flow path plates are used, the volume of the micro flow path can be increased. Thus, one microreactor 1 can flexibly cope with a small reaction scale and a large reaction scale.

In the present embodiment, as shown in FIG. 8, the viewing windows 45 a and 45 b are provided on both the first cover 11 and the second cover 15. The viewing windows 45a and 45b are holes penetrating in the thickness direction of the cover. The flat and bottom surfaces of the microchannel are formed of transparent plates 12 and 14. For this reason, the state of the microchannel can be observed through the viewing windows 45a and 45b. For example, it is possible to observe whether or not the microchannel is blocked. Further, for example, in the case of a photocatalytic reaction, the reaction can be caused by irradiating light through a viewing window. For example, a quantitative analysis of a specific component can be performed using a change in absorbance.

The second cover 15, the second transparent plate 14, the flow path plate 13, the first transparent plate 12, and the first cover 11 are stacked in the stated order, and the fixtures 51 are inserted into the plurality of connection holes 46, respectively. Fix it. The second cover 15, the second transparent plate 14, the flow path plate 13, the first transparent plate 12, and the first cover 11 are rectangles of the same size in plan view. For this reason, the shape of the microreactor 1 in which these are stacked is a rectangular parallelepiped having no irregularities on the side surfaces. In the microreactor 1 of the present embodiment, as shown in FIG. 9, as the fixing tool 51, a screw having a head 47, a screw portion 48, and a non-thread portion 49 having no thread is used. The road plate 13 and the cover are fastened. In the present embodiment, the second cover 15, the second transparent plate 14, the flow path plate 13, the first transparent plate 12, and the first cover 11 are provided with connection holes 46 that allow them to communicate with each other. The inner wall of the connection hole of the second cover 15 is a female screw portion. Passage 46 other than the second cover is not provided with a female screw, the inner wall is a flat smooth surface.

As shown in FIG. 10, the screw portion 48 is attached to the second cover 15 with the first cover 11, the first transparent plate 12, the flow path plate 13, the second transparent plate 14, and the second cover 15 assembled. The female screw portion and the male screw portion of the fixing tool 51 are arranged at a portion where the female screw portion is screwed. Other portions of the screw shaft are non-threaded portions 49. The non-threaded portion 49 closes the connection holes 46 of the first cover 11, the first transparent plate 12, the flow path plate 13, and the second transparent plate 14 to improve airtightness and liquid tightness. For this reason, airtightness and liquid tightness are enhanced at the locations indicated by arrows in FIG. 10, that is, between the flow path plate 13 and the first transparent plate 12 and between the flow path plate 13 and the second transparent plate 14. . The inner diameter of these connecting holes 46 are so as to exhibit a gas-tightness and liquid-tightness in sliding contact to the extent that rotation is not impeded fixture 51. In the microreactor 1 of the present embodiment, the tip of the fixture 51 does not protrude from the bottom surface of the microreactor. For this reason, as shown in FIG. 3, the reaction can be performed by installing the microreactor 1 such that the bottom surface of the microreactor 1 is in contact with an experimental bench or the like.

In the microreactor 1 of the present embodiment, the thread is provided only on the inner wall of the connection hole 46 of the second cover 15, but the thread may also be provided on the inner wall of the connection hole 46 of the first cover 11. This is because airtightness and liquid tightness can be enhanced by the connection holes 46 of the first transparent plate 12 and the connection holes 46 of the second transparent plate 14.

In the present embodiment, the head 47 of the fixture 51 is located on the side of the first cover 11. As another embodiment, a fixture may be inserted from the side of the second cover 15. In this case, a thread is provided at least on the inner wall of the communication hole 46 of the first cover 11.

In the microreactor 1 of this embodiment, a multi-thread screw is used as the fixing tool 51. The following relationship exists between the amount of movement of the screw when the screw makes one rotation, that is, the lead, the number of threads of the screw, and the pitch. Lead (L) = pitch (P) x number of threads (n). By using a multi-thread screw, it is possible to increase the amount of movement per rotation of the screw. Thereby, the work of disassembling and assembling the microreactor 1 can be easily and quickly performed. In the microreactor 1 of the present embodiment, a plurality of fixtures are used to improve airtightness and liquid tightness. Use of the multi-threaded screw facilitates replacement of the flow path plate 13.

As the number of threads of the screw increases, the screw is likely to be loosened. Therefore, n is preferably 1 or more and 6 or less, and n is preferably 2 or more and 3 or less. P is preferably 0.2 or more and 6 or less.

FIG. 11 shows another embodiment. The microreactor 2 of this embodiment differs from the microreactor 1 in that it does not include the first transparent plate 12 and the second transparent plate 14. The first cover 11b and the second cover 15b are made of quartz glass, are excellent in heat resistance and corrosion resistance, and can observe the microchannel from outside. The connection hole 50 of the second cover is a concave portion and differs from the microreactor 1 also in that it does not penetrate the second cover 15b. Since the connection hole 50 does not penetrate, airtightness and liquid tightness can be improved. Since the fixture 51b having the screw portion 48b, the non-thread portion 49b, and the head 47b is used similarly to the microreactor 1, the connection hole 50 of the first cover 11b is closed by the non-thread portion 49b. Thereby, airtightness and liquid tightness are enhanced. The fixing tool 51b is a multi-threaded screw similar to the microreactor 1, and can perform the fastening operation quickly. For this reason, it is possible to easily and quickly replace with another flow path plate by attaching and detaching the fixing tool 51b.

DESCRIPTION OF SYMBOLS 1 Microreactor 11 1st cover 15 2nd cover 13 Flow path plate 19 Outlets 16 and 18 Inlets 12 and 14 Transparent plate

Claims (4)

A first cover, a second cover, a channel plate disposed between the first cover and the second cover, and a glass plate disposed to be in contact with the first cover and the channel plate. A microreactor comprising: a transparent plate; and a second transparent plate made of glass disposed so as to be in contact with the second cover and the channel plate .
The microreactor has an outlet and a plurality of inlets,
The flow path plate has a micro flow path connecting the inlet and the outlet in an arbitrary pattern,
The microreactor includes a plurality of flow path plates having micro flow paths having the same or different patterns as replacement plates,
The first cover, the first transparent plate, the flow path plate, the second transparent plate, and the second cover are provided with connecting holes communicating with each other, and the first cover, the first cover, and the first cover are inserted by inserting a fixture into the connecting holes . The transparent plate, the flow path plate, the second transparent plate and the second cover can be fixed to each other, and the flow path plate can be exchanged by removing the fixture,
The first cover, the second cover, the flow path plate, the first transparent plate, and the second transparent plate have the same rectangular shape in a plan view, and the flow path plate, the first transparent plate, and the second transparent plate are laminated. In such a case, there is no unevenness on the side,
A microreactor in which a viewing window for visually recognizing the flow path plate via the first transparent plate or the second transparent plate is provided on at least one of the first cover and the second cover . The fixing tool is a screw including a thread portion and a non-thread portion having no thread,
The screw portion is disposed at a portion where one of the first cover and the second cover and the fixing member are screwed together with the first cover, the flow path plate, and the second cover assembled. 2. The microreactor according to claim 1, wherein the microreactor closes a connection hole to increase airtightness and liquid tightness. The microreactor according to claim 1, wherein the fixing tool is a multi-thread screw. The microreactor according to any one of claims 1 to 3 , wherein the first cover has three or more inlets.

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