JP2006239638A - Mixer and mixing method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a mixer which can respond flexibly depending on the situation in order to allow the aimed reaction to carry out, or produce the aimed reaction product. <P>SOLUTION: The mixer is for mixing one or more fluids, which has a passage block 10 in which flow channels converging mutually or branching off are formed inside, and a tube 18 connected via a joint 14 to a flow channel 12 of the passage block 10. By this mixer, the connection of the passage block 10 via the tube 18 to a material supply part 16 and a recovering part 20 for recovering the mixture product forms a necessary fluid circuit. The fluids are mixed in the converging or branching passages, and as the result, react, as the case may be, to produce the aimed product. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a mixer and a mixing method used as a flow reaction apparatus for performing chemical reactions, particularly organic chemical synthesis.

  2. Description of the Related Art In recent years, microchannel chips that cause various chemical reactions while flowing a solution or gas using a flow channel (micro flow channel) having a small flow channel cross-sectional area have attracted attention. A microchannel chip is provided with a region for mixing, heating, reaction, and the like on one chip and a flow path for communicating them, and a specific reaction is performed if a material (raw material) is supplied to this. It is comprised so that.

  The microchannel chip has an advantage that a small volume of the solution and the sample is sufficient because the cross-sectional area of the channel is very small. Furthermore, since the specific surface area (surface area per unit volume) of the fluid flowing through the flow path is increased, the heat exchange efficiency is extremely high and the temperature can be controlled quickly, so the geometric isomerism and position of the reaction product There are advantages such as high selectivity for stereochemical properties such as isomerism, and efficient reaction. For this reason, the microchannel chip is used for the synthesis reaction (micro reaction system) for the purpose of producing a predetermined substance, or for the reaction between the solution and the test object for the purpose of inspection (micro total analysis system, μTAS). Often done.

  When creating a chip to be used for a new application, the shape and dimensions of the flow path and the like are designed for a series of processes by using a simulation such as flow analysis. However, the physical properties of chemicals are not constant, and there are many uncertain factors such as changes in physical properties due to temperature, kinematic viscosity, viscosity coefficient, and heat transfer coefficient for each chemical. Lack of accuracy. In particular, no simulation method has been established by flow analysis that takes into account the movement at the molecular level. Therefore, some mixers designed and manufactured based on the result of the simulation may not function as a mixer.

  In addition, there are many types of chemical synthesis such as liquid / liquid, gas / liquid, etc., and the pattern of the specific flow path is not always versatile and compatible with all chemical synthesis. It is very unlikely that the reaction product will be obtained in high yield in the mixer.

However, in the existing flow type mixer such as a microchannel chip, the shape of the mixing channel cannot be changed flexibly and easily. Therefore, if the target chemical reaction cannot be achieved after manufacturing, it is necessary to manufacture again. For this reason, the chip becomes expensive, the working efficiency is low, and the cost is high.
Further, the existing flow mixer has a disadvantage that the cleaning performance in the mixer flow path is low. In particular, in a micromixer having a channel width of 0.1 mm or less, when a precipitation-type product is generated, it takes time and cost to clean the channel.

  The present invention has been made in view of the above circumstances, and provides a mixer that can flexibly cope with a situation in order to perform a target reaction or generate a target reaction product. For the purpose.

In order to achieve the above object, the mixer according to claim 1 is a mixer for mixing one or a plurality of fluids, and a flow channel block in which a flow channel that merges or branches is formed. And a tube connected to the flow path of the flow path block via a joint.
In the first aspect of the present invention, a necessary fluid circuit is formed by connecting a flow channel block, in which a flow channel is formed in advance, to a raw material supply unit or a collection unit for collecting mixed products through a tube. The fluid mixes in the flow path where it joins or branches, and as a result reacts in some cases.

The mixer according to claim 2 is characterized in that, in the invention according to claim 1, a fluid circuit including merging and branching is configured by connecting a plurality of the flow path blocks.
The mixer according to claim 3 is characterized in that, in the invention according to claim 1 or 2, a volume body having a volume part having a diameter larger than that of the tube is connected via the tube. To do.
According to a fourth aspect of the present invention, there is provided the mixer according to the third aspect, wherein the volume member is provided with a stirring promoting element for promoting stirring of the fluid in the volume portion.

The mixer according to claim 5 is a mixer for mixing one or a plurality of fluids, and has a plurality of flow path blocks in which flow paths that merge or branch from each other are formed. At least a part of the channel block is open to the bonding surface of the channel block, and the channel is connected to each other by bonding the channel blocks to each other.
In the invention according to claim 5, a necessary fluid circuit is formed by joining a plurality of flow channel blocks in which a flow channel is formed in advance, and the fluid is mixed in the flow channel that merges or branches. As a result, it reacts.

The mixing method according to claim 6 is a mixing method in which one or a plurality of fluids are mixed, wherein a flow path block in which flow paths that merge or branch with each other are formed is used, and the flow path block is used. The one or more fluids are supplied to the fluid circuit configured.
According to a seventh aspect of the present invention, there is provided the mixing method according to the sixth aspect of the present invention, wherein a plurality of the flow path blocks are prepared, and the flow path blocks are selectively connected to each other so as to include the merging and branching. It is characterized by comprising.

  The fluid circuit manufacturing method according to claim 8 is characterized in that mixing is performed using the mixing method according to claim 6 or claim 7 and a fluid circuit in which good results are confirmed is formed on a substrate. To do.

  According to the mixer or the mixing method according to any one of claims 1 to 7, a mixer capable of flexibly responding to a situation in order to cause a target reaction and generate a target reaction product. Can be provided.

  According to the fluid circuit manufacturing method of the eighth aspect, it is possible to form a fluid circuit on the substrate that can surely obtain good results.

Embodiments of the present invention will be described below with reference to the drawings.
FIG. 1 shows one embodiment of a flow path block 10 which is a component of a mixer or a reactor according to the present invention. This flow path block 10 is made of an appropriate material such as resin, metal, ceramics or the like. The various flow paths 12 are formed in advance. In the example of FIG. 1, the flow path block 10 is formed in a flat cylindrical shape, and three flow paths 12 are formed so as to merge on the axial line of the flow path block 10 in the center in the axial direction. . The outer ends of these flow paths 12 are coupled to joints 14 provided on the outer peripheral surface of the flow path block 10, respectively. When this flow path block 10 is used as a mixer, the two flow paths 12 are used as an introduction flow path through which fluid flows, and one is used as a discharge flow path through which fluid mixes and flows out. When used as a divided flow path, the reverse is true. The two introduction flow paths are arranged at the same diameter and at the same angle with respect to the discharge flow path, and each inflow fluid flows into the discharge flow path by the same amount, but is not limited thereto.

  Such a flow path block 10 is formed into a shape having such a flow path 12, or the flow path 12 is formed by drilling or the like after the solid flow path block 10 is formed. Or you may comprise the two half flow path blocks 10 which have the flow path 12 in a joint surface by joining with an adhesive agent etc. The cross-sectional shape of the flow path 12 is appropriately selected from a circular shape as shown in FIG. 1 (c), a rectangular shape (polygon) as shown in FIG. 1 (d), or a composite shape as shown in FIG. 1 (e). Can be adopted. Further, the cross-sectional shape may be changed in each channel 12. An appropriate surface treatment is performed on the inner surface of the flow path 12 as necessary. The joint 14 is joined to the flow path block 10 by a method such as adhesion or screwing. In addition, a common joint is used for the joint 14, and the joints 14 are connected to each other by tubes that can be specified in common. In order to prevent fluid leakage, the joint 14 uses a fluid leakage sealing shape of an existing standard such as JIS standard or ISO standard.

  FIG. 2 shows a flow channel block 10 having another flow channel 12 shape, wherein (a) and (b) show three flow channels 12 arranged in a T shape, (c) and (d) show four channels 12, and (e) and (f) show six channels 12 arranged at equal intervals. Also, FIG. 3 shows that the flow path 12 is also arranged in the vertical direction of the flow path block 10, and these flow paths 12 merge three-dimensionally at the center of the flow path block 10. Yes. 3, (a) and (b) are provided with upper and lower flow paths opening on the upper surface and upper and lower surfaces of the flow channel block 10 of FIG. 1, and (c) and (d) are those of FIG. 2 (a). The flow path block 10 is provided with a vertical flow path that opens on the upper surface and the upper and lower surfaces, and FIGS. (G) and (h) are provided with a flow path in the vertical direction that opens on the upper surface and the upper and lower surfaces of the flow channel block 10 in FIG. The flow path 12 provided in these flow path blocks 10 can set the angle of each other, a space | interval, each diameter, and cross-sectional shape suitably. Any one of these flow paths 12 may be set as the introduction flow path 12 and any of the flow paths 12 may be set as the discharge flow path 12. Moreover, the flow path 12 can be formed so that it may branch into many, such as 5 directions, 8 directions, and 10 directions, as needed. The outer peripheral shape of the flow path block 10 is not limited to a circle.

  These channel blocks 10 are standardized for each type, and by preparing a number corresponding to the frequency of use in advance, a fluid circuit for reaction designed by the user is combined with these channel blocks 10. Can be configured. These flow path blocks 10 can be prepared by the user, or can be prepared by the side providing them as products.

  FIG. 4 is an example of a fluid circuit configured by combining these flow path blocks 10, and the flow of the fluid is shown in FIG. 4A. The two reagents supplied by the syringe 16 are respectively introduced into the first flow path block 10a (3-way flow path block: 1 introduction flow path, 2 discharge flow path) through the tube 18a. Here, the flow rate (flow velocity) of the fluid branched into two branches is halved. Thereafter, the fluids are merged (mixed) in the second flow path block 10b (4-direction flow path block: 2 introduction flow path, 2 discharge flow path) through the tube 18b with this flow rate. At this time, each fluid is synthesized (mixed) at a flow rate of ½ at the time of initial introduction, so the synthesis (mixing) time becomes longer, and mixing is promoted during this time. Next, after the third merge (mixing) is performed again by the third flow path block 10c (3-direction flow path block: 2 introduction flow path, 1 discharge flow path), the fourth flow path block 10d (3 directions) A third merging (mixing) is performed by the flow path block: 2 introduction flow paths and 1 discharge flow path, and is discharged to the collection container 20.

  In this embodiment, the fluid is mixed through the above four steps (“first: branch” → “second: merge / branch” → “third: merge” → “fourth: merge”). . Thus, a plurality of fluids are reliably mixed by performing a plurality of branches and merging. In the case of fluids that react with each other, a reaction occurs at the time of mixing, and a new substance is synthesized. In this embodiment, the synthesis is reliably performed in four steps. In this example, the syringe 16 is used as a fluid feeding element. However, a normal piston pump or a diaphragm ram pump may be used, and the liquid feeding element is not limited to this example.

  These flow path blocks 10 are basic components of a fluid circuit having a function of branching fluid and a function of mixing (reacting), but other functional blocks can be used. Shown in FIG. 5 is a volume 22 that stirs the fluid to promote mixing and possibly reaction. This is installed between each flow path block 10 as needed.

  The volume body 22 shown in FIGS. 5A and 5B forms a space (volume section) 24 having an inner diameter larger than the inner diameter of the tube 18, and the passing fluid enters the volume section to reduce the flow velocity and It simply ensures the residence time. In the volume body 22 shown in FIG. 5C, an actuator such as a piezoelectric element that is driven by energization is installed as the vibration element 26. The volume body 22 vibrates in accordance with the operation of the vibration element 26, and when the fluid (chemical solution) passes through the volume body 22, stirring and mixing by vibration is performed, and fluid mixing is promoted. Further, in the volume body 22 shown in FIG. 5D, a magnetic piece 28 is provided inside the volume body 22, and an exciting element 30 that generates magnetic force by applying electricity (current or voltage) to the outside of the volume body 22. Is attached. In the volume body 22, a magnetic force is generated by applying electricity to the exciting element 30, and the magnetic piece 28 inside the volume body 22 freely moves. Thereby, the fluid (chemical solution) passing through the volume body 22 is forcibly mixed. The shape of the magnetic piece 28 is not limited to this.

  The volume 22 shown in FIG. 5 (e) is filled with beads 32 made of glass, resin, or ceramics, and the turbulence is generated in the passing flow to promote mixing. The beads 32 may be modified with a catalyst to have a function of promoting the reaction. The shape of the beads 32 is not limited to a spherical shape, and any appropriate shape can be adopted. Furthermore, the volume body 22 shown in FIG. 5 (f) forms a labyrinth wall 34 and forms a labyrinth type flow path. Thereby, a turbulent flow is generated in the passing fluid to promote mixing. In addition, the labyrinth wall 34 can be provided with a function of promoting the reaction by modifying the catalyst. Several types of these volume members 22 are prepared in advance, and in the case of a table or the like, they can be used by being coupled to another flow path block 10 via the joint 14 and the tube 18.

  By using the flow path block 10 of the present invention, the combination pattern of the flow path blocks 10 can be flexibly changed and a trial can be performed. A pattern in which the target product for branching can be obtained at high speed and in high yield by combining the flow path block 10 by performing deceleration one or more times by decelerating or converging the flow velocity and mixing at each angle collision angle. Can be searched in a timely manner to find the optimum flow path pattern. Therefore, it is possible to achieve a high yield by configuring a mixing device or a reaction device in accordance with the target chemical (synthesis) reaction.

  In FIG. 6A and below, some patterns will be described by way of example. 6A shows a simple configuration using one flow path block 10. In FIG. 6A, mixing by the flow path block 10 of three flow paths is performed in (a), and two volume bodies 22 are connected to it in (b). It is. In chemical reactions where high yields can be obtained in a short time even in the synthesis by the conventional method (batch), it is only necessary to obtain reaction products continuously, so such a relatively simple pattern Can be selected.

  On the other hand, in the conventional method (batch), for a reaction that takes a long time to obtain a high yield, as shown in FIG. 6A (c), two flow path blocks 10 are connected and mixed and branched twice. Select a relatively complex configuration to be performed. Further, when the reaction is slow, a fluid circuit having a more complicated pattern as shown in FIG. 4 is adopted. Of course, the pattern of the fluid circuit is not limited to these, and those shown in FIG. FIG. 6B shows a configuration using three channel blocks 10, FIG. 6C shows a configuration using four channel blocks 10, FIG. 6D shows a configuration using five channel blocks 10, and FIGS. 6E and 6F. FIG. 6G shows a configuration using seven flow path blocks 10 as in FIG. 4.

  In the above embodiment, each example is given in the case of 2 (drug) liquid mixing. However, 3 (drug) liquid mixing, A plurality of mixings such as 4 (drug) liquid mixing can also be performed with the same configuration as described above.

  Moreover, according to this invention, the length of each tube 18 installed between each flow path block 10 can be set arbitrarily, and the mixing time of the chemical | medical solution which passes the inside of the tube 18 can also be set arbitrarily. That is, if the length of the tube 18 is increased, the reaction time can be extended even with the same reagent flow rate (flow rate). Further, as shown in FIGS. 6A (b) and 6B (c), a volume member 22 can be installed in the tube 18 to generate a flow turbulence when the chemical solution passes to promote mixing. The installation position and the number of the volume bodies 22 are not limited to these examples. In addition, the tube 18 can be modified in advance with a chemical catalyst on its inner surface to produce an effect of promoting the reaction.

  In general, in chemical reactions (organic chemical synthesis), the specific interfacial area increases only if the reaction (synthesis / mixing) is performed in a narrow space, and molecular diffusion mixing is promoted. Rate is obtained. There exists a microreactor etc. as a mixer or a reactor which has the characteristics mentioned above. However, when the reaction space is narrowed, in a reaction in which precipitates are generated as a result of a chemical reaction (product or by-product), if the reaction space is simply narrowed, the precipitates become narrower as the reaction proceeds, that is, The flow path 12 inside the reactor may be blocked and may not function as a mixer or a reactor.

  As one embodiment in which this problem of clogging is eliminated, even when precipitates are generated as a result of a chemical reaction, while maintaining a high yield by diffusion mixing of molecules using specific interface, In order to suppress the blockage, it is recommended that the cross-sectional area of the flow path 12 and the cross-sectional area of the tube 18 in the flow path block 10 be 1 mm 2 or less (upper limit 1 mm 2). Moreover, the material of the flow path block 10 and the tube 18 is various resins such as PTFE, glass, metal, ceramics, and the like, and the cost can be reduced especially by processing with resin.

  FIG. 7 shows the result of acetylation of phenol using a mixer (fluid circuit) configured using the flow path block 10 according to the present invention. The flow path pattern of the mixer is that shown in FIG. 6D (a) described above. This experimental result shows the yield of the product with respect to the reaction time. From this result, it can be seen that the mixer according to the present invention achieves high speed (short time) and high yield.

  FIG. 8 shows an example in which phenol acetylation is performed using a mixer according to another embodiment of the flow path block 10 according to the present invention. The flow path pattern of the mixer is one in which the volume body 22 shown in FIG. 6B (c) in the above example is installed. The volume body 22 installed here has a simple structure shown in FIGS. 5 (a) and 5 (b). As in the case of FIG. 7, it can be seen that the mixer according to the present invention achieves high speed (short time) and high yield.

  FIG. 9 shows a structure in which the flow path blocks 10 are stacked to reduce the size while maintaining the function (flow path). Each flow path block 10 is provided with a flow path 12 that connects the flow path blocks 10 on the upper and lower surfaces, and is further provided with annular unevenness or positioning pins. Therefore, when stacking the respective flow path blocks 10, the communication flow paths between the flow path blocks 10 are easily positioned, and replacement (removal and attachment) is also facilitated. Further, a seal such as an O-ring is installed between the lamination flow path blocks 10 so that the fluid passing between the flow path blocks 10 does not leak. The flow path pattern of the mixer is that shown in FIG. 6D (a) described above.

  FIG. 10 shows the result of acetylation of phenol using the mixer according to the embodiment of FIG. This experimental result shows the yield of the product with respect to the reaction time. From this, it can be seen that the mixer according to the present invention achieves high speed (short time) and high yield.

  FIG. 11 shows an example of application of the present invention, in which an optimal flow path pattern found experimentally using the flow path block 10 is processed into a flat substrate 36 to form a chip. It is. The flow path 38 opened to the substrate 36 has the flow path pattern shown in FIG. 9 described above. FIG. 11A is a perspective view of the substrate 36 in which the flow path pattern is processed, and FIG. 11B is a top view. The flow path 38 of the substrate 36 is connected to another device via a joint 42. Even in this configuration, it is considered that a high yield result can be obtained in a short time as in each of the configuration examples and examples.

  As described above, according to the present invention, it is possible to easily change the mixing pattern in the flow organic chemical synthesis. As a result, a mixer for flow chemical synthesis can be manufactured at low cost.

BRIEF DESCRIPTION OF THE DRAWINGS It is a figure which shows one embodiment of the flow path block which is the principal part of the mixer of this invention, (a) is plane sectional drawing, (b) is a perspective view, (c)-(e) is (a) It is an II arrow directional view of). (A), (c), (e) is sectional drawing which shows other embodiment of a flow-path block, respectively, (b), (d), (f) is each perspective view. (A), (c), (e), (g) is sectional drawing which shows other embodiment of a flow-path block, respectively, (b), (d), (f), (h) is each perspective view. FIG. It is a perspective view which shows the mixer comprised using the flow path block. It is a figure which shows the fluid circuit of the mixer of FIG. 4A. (A), (b) is the perspective view and sectional drawing which show one embodiment of a volume body, (c)-(f) is sectional drawing of other embodiment. (A) is a fluid circuit diagram of a mixer using one channel block, (b) is a fluid circuit diagram of a mixer using one channel block and a volume body, and (c) is two channel blocks. It is a fluid circuit diagram of the mixer using the. (A), (b) is a fluid circuit diagram of a mixer using three channel blocks, and (c) is a fluid circuit diagram of a mixer using three channel blocks and a volume member. It is a fluid circuit diagram of a mixer using four flow path blocks. (A)-(c) is a fluid circuit diagram of the mixer using five flow path blocks. (A) And (b) is a fluid circuit diagram of the mixer using six flow path blocks. It is a fluid circuit diagram of the mixer of other embodiment using six flow path blocks. (A) And (b) is a fluid circuit diagram of the mixer using seven flow path blocks. It is a graph which shows the result of having implemented the acetylation of phenol using the mixer shown to FIG. 6D (a). It is a graph which shows the result of having implemented the acetylation of phenol using the mixer shown to FIG. 6B (c). 1 shows a mixer configured by stacking channel blocks, where (a) is a fluid circuit diagram, (b) is an exploded view of the stacked structure of the channel block, and (c) is an external view of the stacked structure. It is. It is a graph which shows the result of having implemented the acetylation of phenol using the mixer shown in FIG. The embodiment which comprised the fluid circuit of the mixer shown in FIG. 9 on the board | substrate is shown, (a) is a perspective view, (b) is a top view.

Explanation of symbols

10 channel block 10a channel block 10b channel block 10c channel block 10d channel block 12 channel 14 joint 16 syringe (raw material supply unit)
18, 18 a, 18 b Tube 20 Recovery container 22 Volume body 26 Vibration element 28 Magnetic piece 30 Excitation element 32 Bead 34 Labyrinth wall 36 Substrate 38 Flow path 42 Joint

Claims (8)

A mixer for mixing one or more fluids,
A flow path block in which flow paths that merge or branch into each other are formed;
A mixer having a tube connected to a flow path of the flow path block via a joint.   The mixer according to claim 1, wherein a fluid circuit including a merging and branching is configured by connecting a plurality of the flow path blocks.   The mixer according to claim 1 or 2, wherein a volume body having a volume portion whose diameter is larger than that of the tube is connected via the tube.   The mixer according to claim 3, wherein the volume member is provided with a stirring promoting element that promotes stirring of the fluid in the volume portion.   It is a mixer for mixing one or a plurality of fluids, and has a plurality of flow channel blocks in which flow channels that merge or branch together are formed, and at least a part of the flow channels is joined to the flow channel blocks A mixer having an opening on the surface and communicating the flow path block by joining the joint surfaces to each other. A mixing method for mixing one or more fluids,
Using a channel block in which channels that merge or branch together are formed inside,
A mixing method comprising supplying the one or more fluids to a fluid circuit configured using the flow path block.   The mixing method according to claim 6, wherein a fluid circuit including merging and branching is configured by preparing a plurality of the flow path blocks and selectively connecting the flow path blocks. 8. A fluid circuit manufacturing method, wherein mixing is performed by using the mixing method according to claim 6 or 7 and a fluid circuit whose good result is confirmed is formed on a substrate.

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