JP2007044678A - Method for implementing chemical reaction - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for implementing a chemical reaction enhancing the efficiency of reaction in a flow channel above that of being determined by the width of the flow channel by making diffusion time shorter than that of being determined by the width of the flow channel and obtaining a larger size of a specific boundary area of a fluid boundary. <P>SOLUTION: The method for implementing the chemical reaction comprises a process for introducing fluids 211 and 212 of two kinds or more containing a different component into the flow channels 206 and 207 respectively, a process for joining the fluids 211 and 212, and a process for surrounding the periphery of the joined fluids 211 and 212 by a fluid 213 in no reaction to the fluid of the above-described two kinds or more to form a dispersed phase 215, wherein the chemical reaction is implemented inside the dispersed phase. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a method suitable for performing a chemical reaction in a minute space.

  In recent years, in the chemical industry related to the manufacture of pigments used in inkjet printers and the pharmaceutical industry related to the manufacture of pharmaceuticals, reagents, etc., development of new manufacturing processes using micro containers called micromixers or microreactors has progressed. It has been. The micromixer and the microreactor are provided with a plurality of microchannels having an equivalent diameter of about several μm to several hundreds of μm when the cross section thereof is converted into a circle, and a mixing space connected to these microchannels.

  In this micromixer and micromixer, a plurality of fluids are respectively introduced into a mixing space through a plurality of microchannels, thereby mixing a plurality of solutions or causing a chemical reaction together with the mixing. The micromixer and the microreactor have the same basic structure. In particular, a microreactor may be referred to as a microreactor that involves a chemical reaction when mixing a plurality of solutions. From this, the following description will be made assuming that the micromixer includes a microreactor.

  As such a micromixer, there is one disclosed in Patent Document 1. FIG. 7 is a conceptual diagram illustrating a conventional microreactor. FIG. 7A is a conceptual cross-sectional view of the microreactor, and FIGS. 7B and 7C are enlarged views of a part of the microreactor and the mixer channel. Two liquid supply ports 103 and 104 are provided at the front ends of the liquid supply paths 101 and 102, respectively, which open along a circular locus and are arranged so as to be substantially concentric with each other. The opening widths W1 and W2 of the liquid supply ports 103 and 104 are set to be minute widths of 1 μm or more and 500 μm or less. As a result, the two types of solutions 106 and 107 introduced into the mixing channel through the liquid supply ports 103 and 104, respectively, are laminar laminar flows corresponding to the opening widths W1 and W2 of the liquid supply ports 103 and 104, respectively. And circulates in the mixing channel 105. The molecules of the solutions 106 and 107 diffuse to each other at the contact interface between the flowing laminar flows, so that the solutions 106 and 107 are uniformly mixed in a short time, or a chemical reaction proceeds with the mixing, and the mixing channel 105 Spill from.

  Next, the difference in the mixing and reaction by the micromixer as described above from the batch method using a tank or the like will be described. The liquid phase chemical reaction generally occurs when molecules meet at the interface of the reaction solution. Therefore, when the reaction is carried out in a minute space, the area of the interface is relatively increased, and the reaction efficiency is remarkably increased. In addition, the diffusion time of the molecule itself is proportional to the square of the distance. This means that even if the reaction solution is not actively mixed as the scale is reduced, mixing proceeds by molecular diffusion and the reaction is likely to occur. Also, in the micro space, since the scale is small, the flow is dominated by laminar flow, and the solutions are in a laminar flow state and are diffused and mixed with each other.

  Using a micromixer with the above characteristics, for example, it is possible to precisely control the reaction time and temperature between solutions compared to the conventional batch method using a large volume tank as a mixing and reaction field. It becomes. In the case of the batch method, the reaction proceeds at the reaction contact surface at the initial stage of mixing between solutions having a high reaction rate, and further, the primary product generated by the reaction between the solutions is continuously subjected to the reaction in the container. There is a risk that the product is non-uniform or agglomeration or precipitation occurs in the mixing container.

  On the other hand, according to the micromixer, the solution circulates continuously with almost no stagnation in the mixing container, so that the primary product generated by the reaction between the solutions continues to react while staying in the mixing container. Can be deterred. Moreover, it becomes possible to take out a pure primary product which was difficult to take out in the past, and aggregation and precipitation in the mixing vessel are less likely to occur.

  In addition, when a small amount of chemical substances produced by an experimental production facility is manufactured (scaled up) in a large amount by a large-scale production facility, a large-scale batch method is conventionally used. It took a great deal of labor and time to obtain reproducibility in the production facility. On the other hand, it is possible that the labor and time for obtaining such reproducibility can be greatly reduced by parallelizing production lines using micromixers according to the required production amount.

  However, in the micromixer as described above, the specific interface area between the diffusion time and the fluid boundary is determined by the width of the flow path used for the reaction, and the efficiency of the reaction is improved beyond the efficiency determined by the width of the flow path. I can't.

Hereinafter, it will be described that the reaction efficiency is determined by the width of the flow path.
First, the calculation method of the specific interface area in the microchannel will be described with reference to FIGS. 7B and 7C. FIG. 7C is a three-dimensional cross-sectional view in which a part of the mixing channel in FIG. 7B is cut out. When the channel width 108 is W [μm], the channel length 109 is L [μm], and the fluid width 110 is d [μm], the total volume of the solution L ₁ 106 is (W / 2). × d × L [μm ³ ]. The area of the fluid boundary 111 between the solution L ₁ and the solution L ₂ is d × L [μm ² ]. Accordingly, the specific interface area is (d × L) / {(W / 2) × d × L} = 2 × 10 ⁴ / W [cm ⁻¹ ], and the flow path length (L) and fluid width ( It can be seen that it is determined only by the width (W) of the channel regardless of d). For example, the specific interface area when the channel width 108 is 1000 [μm] is 20 [cm ⁻¹ ], whereas the specific interface area when the microchannel width 108 is 100 [μm] is 200 [μm]. cm ⁻¹ ]. Therefore, as the width 108 of the microchannel is reduced, the specific interface area is increased and the reaction efficiency is improved. The specific interface area means the ratio of the surface area to the unit volume or the area of the interface.

  However, in the normal case as shown in FIG. 7, the reaction proceeds mainly at the fluid boundary 111. Therefore, the efficiency of the reaction between the laminar flows as shown in FIG. 7A described above is, conversely, shortening of the diffusion time and the size of the specific interface area of the fluid boundary 111, that is, the flow path width 108. It means to be limited. That is, the specific interface area between the diffusion time and the fluid boundary 111 is determined by the width 108 of the flow path used for the reaction, and the efficiency of the reaction cannot be improved beyond the efficiency determined by the width 108 of the flow path. Further, as described above, if the channel width 108 is reduced, the diffusion time can be further shortened to increase the specific interface area and the reaction efficiency can be improved. However, the smaller the channel width 108, the more the pressure loss. However, there is a limit to reducing the width 108 of the flow path because the liquid is difficult to feed and becomes unrealistic.

On the other hand, since the path length along the flow direction of the solution in the mixing space is constant in the above-described micromixer, the time for the solution to pass through the mixing space (passing time) when the solution flow rate is constant Is constant. Therefore, when the mixing time or reaction time of the solution in the mixing space is longer than the passage time, it is necessary to reduce the flow rate of the solution in the mixing space, so that the processing speed of the solution by the micromixer decreases. At this time, in order to prevent a decrease in the processing speed of the solution, it is conceivable to extend the path length of the mixing space. However, when such measures are taken, the size of the micromixer is increased and the manufacturing cost is increased. And so on. Also, if the path length of the mixing space is extended more than necessary, the problem is that clogging occurs in the mixing space by promoting the aggregation and precipitation of the product and frequent maintenance of the micromixer is required. Also occurs.
JP 2003-210959A

  The object of the present invention has been proposed in view of such a conventional situation. By reducing the diffusion time more than determined by the width of the flow path and obtaining the size of the specific interface area of the fluid boundary, An object of the present invention is to provide a method for improving the efficiency of reaction in a channel beyond the efficiency determined by the width of the channel.

  It is another object of the present invention to provide a method for preventing clogging of a flow path due to product aggregation and precipitation by causing a chemical reaction inside a dispersed phase.

  The present invention for solving the above problems is a method for performing a chemical reaction, the step of introducing two or more kinds of fluids containing different components into a flow path, the step of joining the fluids, and the joined fluids And a step of forming a dispersed phase by surrounding the substrate with a fluid that does not react with the two or more kinds of fluids, and performing a chemical reaction inside the dispersed phase.

  Further, the present invention is a method for producing fine particles by a chemical reaction, the step of introducing two or more kinds of fluids containing the raw material of the fine particles into the flow path, the step of joining the fluids, and the joined fluid Forming a dispersed phase by surrounding the substrate with a fluid that does not react with the two or more types of fluids, and performing a chemical reaction inside the dispersed phase to generate fine particles. Regarding the method.

  In the method for carrying out a chemical reaction according to the present invention, two or more kinds of fluids containing different components are introduced into a micro flow path, the fluids are merged, and the periphery of the fluid is surrounded by a fluid that does not react with the fluid to form a dispersed phase. The specific interface area obtained by generating a dispersed phase in the microchannel by performing a chemical reaction inside the dispersed phase is simply larger than the specific interface area of the laminar flow formed in the microchannel. The diffusion time of the two types of fluid inside the dispersed phase is also shorter than the diffusion time when the laminar flow is simply formed in the microchannel, so it is more than determined by the width of the microchannel. The diffusion time can be shortened and the specific interface area of the fluid boundary can be obtained, and the efficiency of the chemical reaction in the microchannel can be improved beyond the efficiency determined by the width of the microchannel.

  Further, by performing a chemical reaction inside the dispersed phase, it is possible to prevent clogging of the flow path due to product aggregation and precipitation.

Hereinafter, the present invention will be described in detail.
As the two or more kinds of fluids containing different components used in the method for carrying out a chemical reaction of the present invention, any fluid may be used as long as the object of the present invention can be achieved. For example, a solution such as a diazonium salt solution and a coupler solution for synthesizing an azo pigment, or a solution for biological reaction such as protein synthesis may be used.

  Two or more kinds of fluids containing such different components and a fluid that does not react with the fluid are introduced into the microchannel, and in the portion where the two or more types of fluid merge in the microchannel, Is surrounded by a fluid that does not react with the fluid. This is a phenomenon caused by the collision of fluid that is continuously transported in a space with a very small cross-sectional area called a micro-channel, and the present invention skillfully uses a unique fluid flow in a special environment of a micro-space. It is what. In the present invention, this dispersed fluid is referred to as “dispersed phase”. Further, the fluid other than the dispersed phase is a fluid that does not react with two or more kinds of fluids containing different components, and the fluid other than the dispersed phase is referred to as a “continuous phase”.

  Here, when the “dispersed phase” is formed, depending on the characteristics of the dispersed phase and the continuous phase, the flow rate A of two or more fluids containing different components and two or more fluids containing the different components are used. This is the case where the flow rate ratio of the fluid that does not react with the flow rate B = B / A is large. When the flow rate ratio is small, a “laminar flow” is formed. For example, the flow rate ratio is 2 or more, preferably 10 to 1000.

  Further, the micro channel refers to a channel having an equivalent diameter of about several μm to several hundred μm when the cross section is converted into a circle. The size of the “dispersed phase” is generally smaller in diameter than the width or depth of the microchannel. For example, the size of a dispersed phase generated in a microchannel having a width of 100 μm and a depth of 50 μm is smaller than 50 μm assuming that the dispersed phase is a perfect sphere.

Hereinafter, embodiments of the present invention will be described in detail.
FIG. 1 is a conceptual diagram showing an example of an embodiment of a method for carrying out a chemical reaction of the present invention. The microchannel structure 200 is configured to flow the fluid introduction ports 201, 202, 203, and 204, the introduction channels 205, 206, 207, and 208 communicated therewith, and the fluid introduced and communicated with the introduction channel. , And a discharge port 210 for discharging fluid from the transfer channel 209. The chemical reaction method of the present invention can be carried out by introducing fluids 211 and 212 containing different components and a fluid 213 that does not react with the fluid into the fluid inlet.

  First, using FIG. 1, two types of liquids containing different components are introduced into the microchannel structure, the liquids are merged, and the liquid is surrounded by a liquid that does not react with the liquid at the merged portion. A method for forming a dispersed phase and performing a chemical reaction inside the dispersed phase will be described.

Two types of fluids 211 and 212 containing different components are referred to as liquids L ₂₁₁ and L _212, and a fluid 213 that does not react with the liquid is referred to as a liquid L ₂₁₃ . The liquids L ₂₁₁ and L ₂₁₂ are sent to the transfer channel 209 that communicates with the introduction channels 206 and 207. At this time, the liquid L ₂₁₃ is also fed to the conveying passage 209 which communicates with the introduction passage 205, 208, the merging unit 214 of the L ₂₁₁ and L _212, surround the liquid L _211, L ₂₁₂ by liquid L ₂₁₃ This forms a dispersed phase. While the dispersed phase 215 is conveyed through the conveying channel 209, the components contained in the liquid L ₂₁₁ and the liquid L ₂₁₂ diffuse into each other inside the dispersed phase 215, thereby causing a chemical reaction.

Furthermore, in order to suitably perform the chemical reaction execution method of the present invention, the two types of liquids L ₂₁₁ and L ₂₁₂ containing different components are water-soluble, and the liquid L ₂₁₃ that does not react with the liquid is water-insoluble. Is preferred.
Examples of the liquid L ₂₁₃ that does not react with two or more kinds of liquids containing different components include silicone oil, fluorinate, and liquid paraffin.

  Next, using FIG. 1, two types of liquids containing different components are introduced into the microchannel structure, the liquids are merged, and the liquid is surrounded by a gas that does not react with the liquid at the merged portion. A method of forming a dispersed phase and performing a chemical reaction inside the dispersed phase will be described.

Two types of fluids 211 and 212 containing different components are liquids L ₂₁₁ and L _212, and a fluid 213 that does not react with the liquid is a gas A ₂₁₃ . The liquids L ₂₁₁ and L ₂₁₂ are sent to the transfer channel 209 that communicates with the introduction channels 206 and 207. At this time, the gas A ₂₁₃ is also fed to the conveying passage 209 which communicates with the introduction passage 205, 208, the merging unit 214 of the liquid L _211, L _212, a surrounding liquid L _211, L ₂₁₂ by the gas A ₂₁₃ The dispersed phase 215 is formed by surrounding. While the dispersed phase 215 is conveyed through the conveying channel 209, the components contained in the liquid L ₂₁₁ and the liquid L ₂₁₂ diffuse into each other inside the dispersed phase 215, thereby causing a chemical reaction.

The two types of liquids L ₂₁₁ and L ₂₁₂ containing different components may be either water-soluble or water-insoluble, and are not particularly limited.
Examples of the gas A ₂₁₃ that does not react with the two kinds of liquids containing different components include Ar and N ₂ .

  Next, using FIG. 1, two types of gases containing different components are introduced into the microchannel structure, the gases are merged, and the gas is surrounded by a liquid that does not react with the gas at the merged portion. A method of forming a dispersed phase and performing a chemical reaction inside the dispersed phase will be described.

Two types of fluids 211 and 212 containing different components are referred to as gases A ₂₁₁ and A _212, and a fluid 213 that does not react with the gas is referred to as a liquid L ₂₁₃ . The two types of gases A ₂₁₁ and A ₂₁₂ are transferred to a transfer channel 209 communicating with the introduction channels 206 and 207. At this time, the liquid L _{213 is} also sent to the transfer flow path 209 communicating with the introduction flow paths 205 and 208, and a dispersed phase is formed by surrounding the joined A ₂₁₁ and A ₂₁₂ with L ₂₁₃ . While the dispersed phase 215 is conveyed through the conveying channel 209, components contained in the gas A ₂₁₁ and the gas A ₂₁₂ diffuse to each other inside the dispersed phase 215 to cause a chemical reaction.

Examples of the liquid L ₂₁₃ that does not react with the two kinds of gases containing different components include silicone oil, fluorinate, and liquid paraffin.

Furthermore, in order to suitably perform the chemical reaction execution method of the present invention, the flow rate ratio of two or more kinds of fluids containing different components may be different. At this time, the concentration of the product can be controlled by changing the ratio of the fluid contained in the dispersed phase.
Furthermore, by changing the flow rate ratio between the dispersed phase and the continuous phase, the diameter of the dispersed phase can be reduced and the reaction efficiency can be improved.

  Here, the introduction port provided in the microchannel structure used in the chemical reaction execution method of the present invention is an opening for introducing two or more kinds of fluids containing different components into the microchannel structure. The fluid to be introduced is conveyed from the introduction port through an introduction flow path communicating therewith. Furthermore, a fluid inlet that does not react with the fluid for dispersing the fluid is required. In the present invention, in order to perform a chemical reaction, in order to introduce two or more kinds of fluids containing different components, it is essential to have three or more introduction ports and introduction flow paths.

Moreover, there is no restriction | limiting in particular about each angle of an introduction flow path, if each fluid is a structure which does not mix before a junction part.
FIG. 2 is a conceptual diagram showing that the reaction efficiency is improved by applying light irradiation or heat to the chemical reaction execution method of the present invention. As shown in FIG. 2, the chemical reaction product is irradiated with light by a light irradiation device 301 as needed [FIG. 2 (a)] or heated by a heating device 302 [FIG. (B)], it is also possible to supply energy to the transport channel and to efficiently perform the chemical reaction.

  In addition, when a small amount of chemical substances produced by experimental production equipment is produced in large quantities by large-scale production equipment, production lines using microchannel structures are arranged in parallel according to the required production quantity. Therefore, the labor and time for obtaining reproducibility can be greatly reduced, which is a preferable mode.

  Next, the method for carrying out a chemical reaction according to the present invention reduces the diffusion time more than determined by the width of the microchannel, and obtains the size of the specific interface area of the fluid boundary so that the reaction efficiency in the microchannel is increased. 3 will be described with reference to FIG. 3 to improve the efficiency more than the efficiency determined by the width of the microchannel.

As shown in FIG. 3A, when the diameter 401 of the spherical dispersed phase in the microchannel 402 is D [μm], the total volume of the dispersed phase is (4π / 3) × (D / 2) ^3. [Μm ³ ]. If two types of fluids containing different components are combined in a hemispherical shape, one volume is {(4π / 3) × (D / 2) ³ } / 2. Further, the surface area where the two kinds of fluids contact is π × (D / 2) ² [μm ² ]. Therefore, the specific interface area of the two kinds of fluids is {π × (D / 2) ² } / {{(4π / 3) × (D / 2) ³ } / 2} = 3 × 10 ⁴ / D [cm ^-1 ]. On the other hand, as shown in FIG. 3B, when the width 405 of the flow path is W, the specific interface area of the fluid formed in the micro flow path 402 is 2 × 10 ⁴ / W [cm ⁻¹ ].

  In general, the diameter D of the microchannel formed by the microchannel 402 is smaller than the width W of the microchannel, so that D <W. The specific interfacial area is simply larger than the specific interfacial area of the fluid boundary 404 formed by the microchannel 402, and the diffusion time of the two types of fluids is also diffusion when a laminar flow is simply formed in the microchannel. Shorter than time. Therefore, if a dispersed phase of two or more kinds of fluids containing different components is formed, the diffusion time and the specific interface area of the fluid boundary can be shortened more than determined by the width 402 of the microchannel. The reaction efficiency in the microchannel 402 can be improved beyond the efficiency determined by the width of the microchannel.

  In general, there are methods for forming a dispersed phase, such as rotating a stirring blade or rotor at high speed or using a mechanical method using ultrasonic waves. However, the fluid that forms the dispersed phase can be selected, and the specific interfacial area is accurately controlled. Therefore, it is more preferable that the particle size of the dispersed phase can be easily controlled. Considering these, as shown in FIG. 1, two or more types of fluids containing different components are separately introduced into the microchannel, the fluids are merged, and the fluid is surrounded by the fluid at the junction. A method of forming a dispersed phase by surrounding with a fluid that does not react is more preferable. In addition, the diameter of the dispersed phase can be controlled by controlling the flow velocity, the angle at which the microchannels are united, the width and depth of the microchannels, or a combination of these, and the specific interface area can be controlled more accurately. .

  Moreover, the chemical reaction implementation method of this invention conveys the disperse | distributed phase which the chemical reaction completed to the discharge port as it is with a continuous phase. In particular, when the continuous phase is an oil-based liquid and the dispersed phase is a water-soluble liquid, the continuous phase and the dispersed phase can be separated simultaneously with the recovery of the continuous phase and the dispersed phase in the container at the outlet. .

  The micro-channel substrate having the micro-channel used in the method for carrying out the chemical reaction of the present invention is, for example, glass, quartz, ceramic, silicon, or a substrate material such as metal or resin directly by machining, laser processing, etching, or the like. It can be manufactured by processing. Further, when the substrate material is ceramic or resin, it can also be manufactured by molding using a mold such as a metal having a channel shape. Generally, the microchannel substrate is laminated and integrated with a cover body having a small hole with a diameter of about several millimeters at a position corresponding to the fluid inlet, the fluid outlet, and the outlet of each microchannel. Used as a microchannel structure. As a method for joining the cover body and the micro-channel substrate, solder or adhesive is used when the substrate material is ceramics or metal, or hundreds of degrees Celsius to thousands when the substrate material is glass, quartz, or resin. Bonding methods suitable for each substrate material are used, such as thermal bonding by applying heavy weight at a high temperature of ° C., or when the substrate material is silicon, by activating the surface by washing and bonding at room temperature.

  Hereinafter, the present invention will be described in more detail with reference to examples. Note that dimensions, shapes, materials, and manufacturing processes in the examples are merely examples, and can be arbitrarily changed as design matters within a range that satisfies the requirements of the present invention.

Example 1
As Example 1, a microchannel structure 500 as shown in FIG. 4 is used. FIG. 4A shows a top view of the microchannel structure 500, FIG. 4B shows an AA ′ sectional view, and FIG. 4C shows a BB ′ sectional view. The width of the microchannel 506 is W = 220 [μm], the depth of the microchannel 506 is d = 80 [μm], and the length of the microchannel 506 is 40 [mm]. The microchannel structure is formed on a Pyrex (registered trademark) substrate 507 of 70 mm × 38 mm × 1 mm (thickness) by general photolithography and wet etching to form a microchannel substrate. Further, a Pyrex (registered trademark) substrate 508 of the same size provided with a small hole having a diameter of 0.6 mm at the position of the introduction ports 501, 502, 503, 504 and the discharge port 505 by mechanical processing means is used as a cover body. The microchannel is sealed by joining by fusion bonding.

Next, two types of solutions containing different components will be described.
A diazonium salt solution is prepared as the first solution 509. In the diazonium salt solution, 2-methoxy-4-nitroaniline is added to water and an aqueous hydrochloric acid solution and stirred, and ice is added to cool to 0 ° C. Thereafter, sodium nitrite is dissolved in water and added, and after stirring for 60 minutes, sulfamic acid is added to eliminate nitrous acid.

  A coupler solution is prepared as the second solution 510. The coupler solution can be prepared by dissolving 2-methoxyacetocetanilide together with water and caustic soda and setting the water temperature to 20 ° C.

  A diazo coupling reaction can be performed by introducing the two kinds of solutions into the microchannel structure. Hereinafter, the liquid feeding of each liquid will be described with reference to FIG. A first solution 509 made of a diazonium salt solution is fed from the inlet 502 of the microchannel structure 500, and a second solution 510 in which a dispersant is added to the coupler solution is fed from the inlet 503. Further, silicone oil (viscosity 2 cp) 511 is fed from the inlets 501 and 504 as a continuous phase. Each liquid is fed by a pump 513. By this reaction, an azo pigment (Pigment Yellow (PY) 74) 512 is synthesized.

  By adjusting the liquid feeding speed, the two types of solutions react when forming a laminar flow, and the two types of solutions are surrounded by a continuous phase to form a dispersed phase. It can be compared with the case. The flow rate of the solution when forming the laminar flow is 20 [μl / min], and the flow rate of the silicone oil is 1 [μl / min]. The flow rate for forming the dispersed phase is 1 [μl / min] for both the solution and 150 [μl / min] for the silicone oil.

In this microchannel, the specific interface area obtained when forming a laminar flow is 2 × 10 ⁴ / W [cm ⁻¹ ] =, since the width of the microchannel is W = about 220 [μm]. about ^{2 × 10 4/220 [cm} -1] = approximately 90 [cm ^-1]. Moreover, when forming a dispersed phase, the diameter of a dispersed phase is calculated | required by measuring using a high-speed camera. When the diameter of the dispersed phase is 80 μm, the specific interface area is 250 [cm ⁻¹ ]. From this, it is presumed that the specific interfacial area is larger in the case where the dispersed phase is formed with silicone oil than in the case where the laminar flow is formed with two kinds of solutions, and the reaction efficiency is increased.

  In addition, by using the present invention, since a chemical reaction is performed inside the dispersed phase, fine particles are synthesized inside the dispersed phase. After completion of the reaction, the fine particles can be recovered in a dispersed phase from the liquid discharge port, so that the fine particles do not adhere to the transport channel.

Example 2
As Example 2, a microchannel structure as shown in FIG. 5 is used. FIG. 5A shows a top view of the microchannel structure 600, and FIG. 5B shows a CC ′ cross-sectional view. The inner diameters of the introduction channels 601 and 602 are 250 [μm], the diameter of the transfer channel 603 is 500 [μm], and the length of the transfer channel 603 is 50 [mm]. The microchannel structure 600 is formed on a quartz substrate of 70 mm × 20 mm × 10 mm (thickness) by a general mechanical processing means to form a microchannel substrate. The introduction channels 601 and 602 are formed by inserting a glass tube having an outer diameter of 1.0 [mm], an inner diameter of 250 [μm], and a length of 5.0 [mm]. The introduction channel and the conveyance channel can be connected to a pipe by using a Teflon (registered trademark) connector 604.

  By using the microchannel structure 600, a diazo coupling reaction can be performed. Hereinafter, the liquid feeding of each liquid will be described with reference to FIG. A diazonium salt solution 605 is fed from the inlet 601 of the microchannel structure 600, and a solution 607 obtained by adding a dispersant to the coupler solution is fed from the inlet 602. Further, silicone oil (viscosity 2 cp) 606 is fed from the inlet 604 as a continuous phase. Each liquid is fed by a pump 609. By this reaction, an azo pigment (Pigment Yellow (PY) 74) 608 is synthesized.

  By adjusting the liquid feeding speed, the two types of solutions react when forming a laminar flow, and the two types of solutions are surrounded by a continuous phase to form a dispersed phase. It can be compared with the case. When forming a laminar flow, the flow rates of the two types of solutions are both 50 [μl / min], and the flow rate of the continuous phase is 5 [μl / min]. The flow rate for forming the dispersed phase is 5 [μl / min] for the two types of solutions and 200 [μl / min] for the continuous phase.

FIG. 6 shows a schematic diagram of a merging portion of the microchannel structure 600. FIG. The solution 607 and the solution 608 are merged at opposite positions of the introduction flow paths 601 and 602, and a dispersed phase is formed by surrounding the solution 607 and the solution 608 with a continuous phase 703, and a chemical reaction is performed inside the dispersed phase. . Hereinafter, the reaction efficiency will be described with reference to FIG. First, as shown in FIG. 6B, the specific interface area obtained when forming a laminar flow is obtained. The laminar flow width 702 can be obtained by measurement using a microscope. Specific interfacial area, when the width 702 of the laminar flow W = about 400 [μm], 2 × 10 4 / W [cm -1] = about ^{2 × 10 4/400 [cm} -1] = about 50 [ cm ⁻¹ ]. When forming a dispersed phase, the diameter 701 of the dispersed phase can be measured using a high-speed camera. When the diameter 701 of the dispersed phase is about 25 μm, the specific interface area is 800 [cm ⁻¹ ]. From this, it is presumed that the specific interfacial area is larger in the case of forming a dispersed phase than in the case of forming a laminar flow with two kinds of solutions, and the reaction efficiency is increased.

  Further, since a chemical reaction occurs inside the dispersed phase, fine particles are synthesized inside the dispersed phase. After the reaction is completed, the particles are collected in a dispersed phase from the liquid discharge port, so that the fine particles do not adhere to the channel wall surface.

  From the above, two types of solutions containing different components are introduced into the microchannel, the two types of solutions are merged, and the periphery of the solution is surrounded by a liquid that does not react with the solution at the merged portion. By forming a chemical reaction inside the dispersed phase, the efficiency of the chemical reaction can be improved beyond the efficiency determined by the width of the microchannel, and the clogging of the channel due to the product is prevented. be able to.

  The method for carrying out a chemical reaction of the present invention improves the efficiency of the reaction in the flow path of two or more kinds of fluids containing different components more than the efficiency determined by the width of the flow path, and performs the chemical reaction inside the dispersed phase. This can prevent clogging of the flow path due to product aggregation, precipitation, etc., so it can be used for the production of fine particles such as pigments and toners, or for the reaction of liquid fine particles in the field of medicine and biotechnology. be able to.

It is a conceptual diagram which shows the method of performing a chemical reaction inside a dispersed phase. It is a conceptual diagram which shows improving reaction efficiency by adding light irradiation and a heat | fever to the chemical reaction implementation method of this invention. It is a conceptual diagram which shows the reaction system in the case of forming a dispersed phase and the case of forming a laminar flow. 1 is a conceptual diagram of a microchannel structure used in Example 1. FIG. It is a conceptual diagram of the microchannel structure used in Example 2. It is the schematic which shows the confluence | merging part of a microchannel structure. It is a conceptual diagram explaining the conventional microreactor.

Explanation of symbols

101, 102 Liquid supply path 103, 104 Liquid supply port 105 Mixing flow path 106, 107 Solution 108 Flow path width 109 Flow path unit length 110 Fluid width 111 Fluid boundary 200 Micro flow path structure 201, 202, 203 , 204 Fluid introduction port 205, 206, 207, 208 Introduction flow channel 209 Transport flow channel 210 Discharge port 211, 212 Fluid containing different components 213 Fluid not reacting with fluid containing different components 214 Merge portion 215 Dispersed phase 301 Light irradiation device 302 Heating device 401 Dispersed phase diameter 402 Microchannel 403 Dispersed phase 404 Fluid boundary 500 Microchannel structure 501, 502, 503, 504 Fluid inlet 505 Fluid outlet 506 Microchannel 507, 508 Substrate 509, 510 Solution 511 Silicone oil 512 Azo pigment 513 Pon 600 flow of fine channel 601 the fluid introducing passage 603 fluid delivery flow path 604 connectors 605, 607 solution 606 silicone oil 608 azo pigment 609 pump 701 dispersed phase diameter 702 laminar flow width 703 continuous phase

Claims (9)

  A method for performing a chemical reaction, the step of introducing two or more kinds of fluids containing different components into the flow path, the step of joining the fluids, and the periphery of the joined fluid reacting with the two or more kinds of fluids And a step of forming a dispersed phase surrounded by a fluid that does not conduct, and performing a chemical reaction inside the dispersed phase.   A method of producing fine particles by a chemical reaction, the step of introducing two or more kinds of fluids containing the raw material of the fine particles into the flow path, the step of joining the fluids, and the two kinds of surroundings of the joined fluids And a step of forming a dispersed phase surrounded by a fluid that does not react with the above fluid, and performing a chemical reaction inside the dispersed phase to produce fine particles.   The chemical reaction execution method according to claim 1 or 2, wherein the two or more kinds of fluids containing the different components are liquids, and the fluid that does not react with the two or more kinds of fluids is a liquid.   The method for carrying out a chemical reaction according to claim 1 or 2, wherein the two or more kinds of fluids containing the different components are liquids and the fluid that does not react with the two or more kinds of fluids is a gas.   The chemical reaction execution method according to claim 1 or 2, wherein the two or more kinds of fluids containing the different components are gases, and the fluid that does not react with the two or more kinds of fluids is a liquid.   6. The chemical reaction execution method according to claim 1, wherein energy is supplied to the flow path.   The chemical reaction execution method according to claim 6, wherein the energy supplied to the flow path is light energy.   The chemical reaction execution method according to claim 6, wherein the energy supplied to the flow path is thermal energy.   The method for carrying out a chemical reaction according to claim 2, wherein the fine particles are pigments.

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