JP5712610B2 - Microreactor and mixed fluid manufacturing method - Google Patents

Description

  The present invention enables uniform mixing even when mixing high-viscosity fluids, or when mixing low-viscosity fluids and fluids whose viscosity is about 10 times higher than that fluid, and obtains mixed fluids of many types of fluids. It relates to a micromixer that can

  Various stationary mixers have been proposed for the purpose of mixing at least two kinds of fluids in a fine particle production process or a chemical reaction process by crystallization or the like. Among these, a micromixer that supplies a fluid to be mixed into the microchannel has attracted attention as an efficient mixing device.

  The micromixer has a mechanism for dividing at least two kinds of fluids into minute flows in a microchannel having a channel width of about 10 μm to 1000 μm and then mixing them. Since the fluid supplied into the micromixer is divided into fine flows, the diffusion distance is shortened and the mixing speed thereof is increased. Therefore, the fluid is efficiently mixed in a shorter time than a conventional static mixer.

  As a structure of the micromixer, for example, a mixer having a Y-shaped channel (Y-shaped micromixer) is known. The Y-shaped micromixer has a structure in which the flow path for flowing the first fluid and the flow path for flowing the second fluid on one plate are acute, that is, intersect with the Y shape to form one combined flow path. ing. The fluids supplied to the mixer merge in a laminar flow state at the intersection of the flow paths and are mixed by mutual diffusion.

  When a low-viscosity fluid and a fluid whose viscosity is about 10 times higher than that fluid (heteroviscous fluid) are circulated through the Y-shaped micromixer at the same flow rate, the pressure loss of the two types of fluids tends to be the same. That is, a fluid having a low viscosity has a high flow rate, and a use cross-sectional ratio of the microchannel is reduced. A high viscosity fluid has the same pressure loss by the reverse. When the viscosity difference is large to some extent, a fluid having a low viscosity flows in an extremely small cross section at a high flow velocity, which causes unstable flow such as intermittent feeding. For this reason, there is a problem that the fluid cannot be stably distributed and the fluid cannot be mixed uniformly. As described above, in the case of mutual diffusion of liquids in a microchannel, there is often no problem in mixing low viscosity, but there is a high possibility that a problem of lowering the mixing property is often generated in a heteroviscous fluid or a high viscosity fluid. .

  As other micromixers other than the Y-shaped micromixer, for example, a plate on which a fine channel through which the reactant A to be mixed flows is formed and a plate on which a fine channel through which the reactant B flows are stacked. A laminated micromixer having such a structure is known (for example, see Patent Document 1). The fine channels of the stacked micromixer are arranged at an acute angle when viewed from the upper surface of the plate, and the fluids are joined and mixed in a merging chamber provided at the outlet of each fine channel.

  A micromixer (exit mixing type micromixer) provided with a stacked structure described in Patent Document 1 and a merging chamber for merging fluids is composed of two plates stacked one above the other. A flow path is formed, and each of the formed micro flow paths has a structure that crosses toward a mixing chamber that is a common outlet. In addition, the flow path width and depth are 250 μm or less, and are intended for fluids that are low in viscosity and easily mixed instantaneously, and are not mixers that are compatible with high viscosity fluids or heteroviscous fluids. For this reason, when a high-viscosity fluid or heteroviscous fluid is circulated through the mixer described in Patent Document 1, pressure loss, clogging, and the like occur, which makes it difficult to circulate and may prevent sufficient mixing.

JP-T 9-512742 (page 12, FIG. 3)

  An object of the present invention is to provide a micromixer that has a good mixing efficiency and can be mixed evenly when mixing high-viscosity fluids or when mixing a low-viscosity fluid and a fluid that is about 10 times higher than that fluid. It is in.

  As a result of intensive studies to solve the above-mentioned problems, the present inventors have laminated a plate on which a fine channel through which the reactant A to be mixed flows is formed with a plate on which a fine channel through which the reactant B flows is formed. In the laminated micromixer having the above-described structure, each plate has an inlet portion of a microtubular channel that communicates with the fluid supply path, and an outlet portion of the microtubular channel that communicates with the mixing portion, and the outlet portion. A microtubular channel in which the fluid cross-sectional area flowing in a liquid-tight manner in the microtubular channel in the pipe is smaller than the fluid cross-sectional area flowing in a liquid-tight manner in one microtubular channel in the inlet portion The micromixer, which is a plate, has good mixing efficiency even when mixing high-viscosity fluids or when mixing low-viscosity fluids and fluids whose viscosity is 10 times higher than that fluid. It found like can be admixed in one, and have completed the present invention.

  That is, the present invention circulates the second fluid that communicates with the fluid supply path through which the second fluid circulates through the first plate having the first microtubular channel that communicates with the fluid supply path through which the first fluid circulates. And a first fluid that communicates with a laminated portion in which a second plate having a second microtubular channel is stacked, an outlet of the first microtubular channel, and an outlet of the second microtubular channel. A micromixer having a mixing portion in which the first fluid and the second fluid are mixed, wherein the first plate has an inlet portion of the microtubular channel that communicates with the fluid supply path, and an outlet portion of the microtubular channel that communicates with the mixing portion And the cross-sectional area of the fluid flowing in the liquid-tight state in the microtubular channel at the outlet is smaller than the cross-sectional area of the fluid flowing in the liquid-tight state in the microtubular channel in the inlet The second plate is a minute plate that communicates with the fluid supply path. And an outlet portion of the microtubular channel that leads to the mixing portion, and the microtubular channel of the inlet portion is a single channel, and the inside of the microtubular channel at the outlet portion A micromixer characterized in that the fluid cross-sectional area flowing in a liquid-tight manner is a plate having a smaller cross-sectional area than the fluid cross-sectional area flowing in a liquid-tight manner in one microtubular channel at the inlet It is to provide.

  In the micromixer of the present invention, the microchannel is formed so that the fluid cross-sectional area at the outlet is smaller than the fluid cross-sectional area at the inlet of the microtubular channel. Therefore, the microchannel of the micromixer of the present invention can increase the fluid velocity at the outlet without losing the fluid pressure. As a result, a strong shearing force acts on the fluid, molecular diffusion in a state accompanied by a slight turbulent flow and stable liquid flow are possible, and mixing efficiency is improved. Therefore, the micromixer of the present invention is particularly useful when mixing high-viscosity fluids that are difficult to mix, or when mixing a low-viscosity fluid and a fluid having a significantly higher viscosity than that fluid. Furthermore, since the micromixer of the present invention can easily increase the number of inlets of the microtubular channel of the second plate, it is also possible to obtain a mixed fluid of many kinds of fluids. In addition, since the micromixer of the present invention is a plate lamination type micromixer obtained by laminating the first plate and the second plate, numbering up is easy. In addition to the first plate and the second plate, the micromixer of the present invention can also be laminated with a plate having a flow path for circulating a medium for heat exchange. It is also possible to perform heat exchange of the fluid flowing through the microchannel provided in the plate. The first plate and the second plate can be manufactured using a cost-effective technique such as wet etching, and the micromixer of the present invention can be obtained at a low cost.

1 is a schematic view of a micromixer 1 according to an embodiment. The disassembled perspective view of the laminated body which the micro mixer 1 has. The perspective view of the 1st plate which is a structural member of the micro mixer 1. FIG. The perspective view of the 1st plate of another example which is a structural member of the micro mixer 1. FIG. The perspective view of the 2nd plate which is a structural member of the micro mixer 1. FIG. The perspective view of the 2nd plate of another example which is a structural member of the micro mixer 1. FIG. An exploded perspective view of a laminate having a plate provided with a flow path through which a heat exchange medium flows The schematic of the micromixer of another example. Schematic configuration diagram schematically showing the device used in the examples Schematic of the reaction microreactor used in the examples The exploded perspective view of the laminated body which the reaction microreactor used in the Example has

  Hereinafter, an embodiment embodying the present invention will be described with reference to FIGS. FIG. 1 is a schematic diagram illustrating an example of a micromixer 1.

  The micromixer 1 has a hollow case C. In the case C, a first plate having a first microtubular channel that leads to a fluid supply channel through which the first fluid (F1) flows is provided. A laminated body 110 having a laminated portion in which a second plate having a second microtubular channel that circulates the second fluid that communicates with the fluid supply path through which the second fluid (F2) circulates is laminated. .

  The micromixer of the present invention is a temperature control plate having a heat exchange medium flow path for circulating a heat exchange medium as exemplified in the micromixer 1 in addition to the laminated portion in which the first plate and the second plate are laminated. In which the first flow path forming part and the first medium flow path correspond in the stacking direction, and the second flow path forming part and the second medium flow path correspond in the stacking direction. It is preferable that the layers are laminated so that the heat exchange efficiency is good.

  Furthermore, the temperature control plate having the heat exchange medium flow path through which the heat medium H11 that exchanges heat between the fluid F1 and the fluid F2 is laminated on the laminated body 110 can equalize the temperatures of the fluid F1 and the fluid F2. It is preferable because a decrease in mixing efficiency due to a difference in temperature between the fluid F1 and the fluid F2 can be reduced.

  The left end C1 of the case C of the micromixer 1 is provided with a first fluid supply unit 1A for supplying the first fluid (F1) into the case C. The lower right end C2 of the case C has a second fluid. A second fluid supply unit 2A for supplying (F2) into the case C is provided. Hereinafter, when the fluid supply units 1A and 2B are not distinguished from each other, the fluid supply unit 1 will be described.

  1 A of fluid supply parts have the opening part 1B formed in the left end part of case C, and the connector 1C connected with the opening part 1B. The connector 1C communicates with a fluid supply path through which the first fluid (F1) flows. Therefore, the fluid supply path communicates with the first microtubular flow path of the first plate. The fluid supply path is connected to a tank for storing the first fluid (F1), a pressurizing pump, and a pressure feeding mechanism including a pipe line connected to the pump, and the first fluid (F1). Is fed to the connector 1C side in a pressurized state by the mechanism. A space is provided in the side surface 11a of the laminated body 11 fixed in the opening 1B and the case C, and the space functions as a storage portion S1 for temporarily storing the first fluid (F1) delivered from the pressure feeding mechanism. To do.

  2 A of fluid supply parts have the opening part 2B formed in the lower right end of case C, and the connector 2C connected with the opening part 2B. The connector 2C communicates with a fluid supply path through which the second fluid (F2) flows, and thus the fluid supply path communicates with the second microtubular channel of the second plate. The fluid supply path is connected to a tank for storing the second fluid (F2), a pressurizing pump, a pressure feeding mechanism including a pipe connected to the pump, and the like. The second fluid (F2) Is fed to the connector 3B side in a pressurized state by the mechanism. A space is provided in the side surface 11b of the laminate 11 fixed in the opening 1B and the case C, and the space functions as a storage portion S2 for temporarily storing the second fluid (F2) sent from the pressure feeding mechanism. To do.

  Further, a heat medium supply part 3A for supplying the heat medium H1 into the case C is formed at the lower left end C3 of the case C. The heat medium supply unit 3A has an opening 3B and a connector 3C, similar to the fluid supply units 1A and 2A. The heat medium H1 supplied to the heat medium supply part 3A passes through the flow path formed in the laminated body 11, and is sent out of the case C from the heat medium supply part 4A formed at the upper end C4 of the case C. . 4 A of heating medium delivery parts have the opening part 4B and the connector 4C similarly to the said fluid supply parts 1A and 2A, respectively.

  The right end C4 of the case C has an opening 5B formed at the right end of the case C and a delivery part 5A including a connector 5C connected to the opening 5B. A space is provided in the opening 5B and the side surface 11c of the laminate 11 fixed in the case C, and the space communicates with the outlet of the first microtubular channel and the outlet of the second microtubular channel. The first fluid and the second fluid function as a mixing unit S3. As the volume of S3, the generated pressure loss, stable flow of high-viscosity fluid and heteroviscous fluid, mixing force, and device strength are considered. It can be changed according to the viscosity of each fluid, the desired degree of mixing, and the like. In particular, when the difference in viscosity between the first fluid and the second fluid is large, for example, 10 times or more, it is necessary to increase the cross-sectional area of the mixing unit S3 in order to perform stable circulation. This is preferable because a uniform mixture with the two fluids can be obtained. In addition, when the viscosity difference between the first fluid and the second fluid is large and the flow rate of the high-viscosity fluid is larger than that of the low-viscosity fluid, it is necessary to further increase the cross-sectional area of the mixing portion.

The area of the cross section leading to the outlet of the first microtubular channel and the outlet of the second microtubular channel of the mixing part S3 is such that a uniform mixture of the first fluid and the second fluid is obtained. To 1.0 mm ² or more.

  In addition, the cross-sectional area leading to the outlet of the first microtubular channel and the outlet of the second microtubular channel of the mixing unit S3 is equal to the cross-sectional area of the outlet of the first microtubular channel and the second A micromixer that is 2 to 200 times the total cross-sectional area of the outlet of the microtubular channel is preferable because the flow is stable and good mixing without stagnating can be achieved even in the mixing part S3 part. Is more preferable.

  The first fluid (F1) and the second fluid (F2) are supplied from the fluid supply portions 1A and 2A to the inside of the case C, and the first microtubular channel and the second fluid are formed in the laminate 11. Each flows through the microtubular channel. The first fluid (F1) that has reached the outlet of the first microtubular channel and the second fluid (F2) that has reached the outlet of the second microtubular channel are mixed to these outlets. It is discharged to the part S3 and mixed. The obtained mixed fluid (F3) is sent out of the case C from the sending part 5A. The positions of the case C of the micromixer 1, the fluid supply units 1 </ b> A, 2 </ b> A, and the delivery unit 5 </ b> A are not limited to the above configuration and can be changed as appropriate.

  Next, the laminate 11 will be described. As shown in FIG. 2, the laminate 11 includes a plate group 13 in which a flow path is formed between the rectangular cover plates P <b> 1 and P <b> 2.

  The plate group 13 is configured by laminating two first plates 5 and two second plates 7. In the present embodiment, a laminated body in which the first plate and the second plate are alternately laminated is formed.

  The cover plates P1, P2, the first plate 5, and the second plate 7 are formed in the same rectangular shape. Further, the materials of the cover plates P1, P2, the first plate 5 and the second plate 7 are not particularly limited, and for example, metal material, resin, glass, ceramics and the like can be easily processed to form a flow path, Any material may be used as long as the plates can be fixed to each other in a close contact state in which liquid leakage is unlikely to occur. Moreover, each plate may be formed from the same material, and may be formed from a different material. For example, each plate may be formed from stainless steel and fixed in a tight contact state by diffusion bonding. As a processing method of each plate, a suitable method according to the material can be selected from various known methods such as injection molding, solvent casting method, melt replica method, cutting, etching, photolithography, laser application, and the like.

  Next, the first plate 5 and the second plate 7 will be described in detail. As shown in FIG. 3, the first plate 5 has a rectangular and plate-like first microtubular channel forming portion 6 </ b> A.

  The first microtubular channel forming portion 6A has one or more first microtubular channels 6 at the center of the upper surface 6a in the short direction (Y direction in the figure). The first microtubular channel 6 is formed in a groove shape from the left end 6b to the right end 6c of the first microtubular channel forming portion 6A, and is open at the left end 6b, the right end 6c, and the upper surface 6a. doing. The opening at the left end 6 b is the inlet 6 d of the first microtubular channel 6, and the opening at the right end 6 c is the outlet 6 e of the first microtubular channel 6. The inlet 6d communicates with the first fluid supply unit 1A to which the first fluid F1 is supplied.

  The first microtubular channel 6 has a large-diameter portion 6f having a large channel diameter, a small-diameter portion 6g having a small channel diameter, and a tapered portion 6h that moderates the diameter change from the large-diameter portion 6f to the small-diameter portion 6g. Is provided.

  The large-diameter portion 6f is a flow path having a rectangular cross section in a direction orthogonal to the flow direction, and extends from the left end 6b to the right end 6c. The width and depth of the large-diameter portion 6f are preferably in the range of, for example, a width of 0.1 mm or more and 100 mm or less and a depth of 5 mm or less in order to ensure the uniformity of the temperature distribution of the fluid and the device strength. A range of 1 mm to 20 mm and a depth of 2 mm is more preferable. In other words, the shape of the large-diameter portion 16 is such that the pressure loss does not increase excessively, the flow path is not easily blocked, the flow path can be quickly controlled for heating and cooling, and the productivity can be improved. Any road shape may be used.

  The large-diameter portion 6f is a flow path having a rectangular cross section in a direction orthogonal to the flow direction, and extends from the left end 6b to the right end 6c. The width and depth of the large-diameter portion 6f are preferably set within a range of, for example, a width of 0.1 mm or more and 100 mm or less and a depth of 0.1 mm or more and 5 mm or less in order to ensure the uniformity of the temperature distribution of the fluid and the device strength. The range of 0.1 mm to 20 mm in width and 0.1 mm to 2 mm in depth is more preferable. Furthermore, the width of 0.1 mm or more and 20 mm or less and the depth of 0.1 mm or more and 1 mm or less are more preferable. That is, as the shape of the large-diameter portion 16, the pressure loss does not increase too much, the flow path is not easily blocked, the flow path can be quickly controlled for heating and cooling, and the flow rate of the fluid can be increased. Any flow channel shape may be used as long as the shearing force acts and molecular diffusion occurs in a state accompanied by a slight turbulent flow, thereby improving the mixing efficiency.

Moreover, as a cross-sectional area of the fluid which distribute | circulates the inside of the 1st micro tubular flow path 6f in a liquid-tight state, 0.01-500 mm < ² > is preferable and 0.01-40 mm < ² > is more preferable. Furthermore, 0.01-20 mm < ² > is more preferable.

  The small diameter portion 6g is also a channel formed in a rectangular cross section, and extends from the front of the right end 6f toward the right end 6c. The small-diameter portion 6g only needs to have a cross-sectional area smaller than at least the cross-sectional area of the large-diameter portion 16. For example, the width is 0.1 mm to 20 mm, the depth is 0.1 mm to 5 mm, and the width is 0.1 mm to 5 mm. Hereinafter, a depth range of 0.1 mm to 2 mm is more preferable. Furthermore, the width of 0.1 mm or more and 5 mm or less and the depth of 0.1 mm or more and 1 mm or less are more preferable. That is, as the shape of the small-diameter portion 17, the pressure loss does not increase excessively, the flow path is not easily blocked, the flow path can be quickly controlled for heating and cooling, the fluid flow rate can be increased, Any channel shape that can act as a force and molecular diffusion in a state accompanied by a slight turbulent flow can improve mixing efficiency.

As the cross-sectional area of the fluid flowing through the first micro-tubular flow channel 6g in a liquid-tight manner, preferably 0.01~100mm ^2, 0.01~10mm ² is more preferable. Furthermore, 0.01-5 mm <2> is more preferable.

  The speed of the fluid when flowing through the first microtubular channel 6g is preferably 0.1 m / second or more, more preferably 0.3 m / second or more because shearing force acting on the fluid increases. More preferably, it is 1.0 m / second or more and 3.0 m / second or more is particularly preferable. In particular, when mixing fluids having high viscosities or when mixing fluids having viscosities greatly different from each other, the flow rate is preferably 1.0 m / second or more.

  The first microtubular channel 6 is a channel whose cross section in a direction orthogonal to the flow direction is rectangular, and extends from the left end 6b to the right end 6c. The width and depth of the first microtubular channel 6 are, for example, from 0.1 mm to 100 mm in width and from 0.1 mm to 5 mm in depth in order to ensure the uniformity of the temperature distribution of the fluid and the device strength. Preferably, the width is 0.1 mm to 10 mm, and the depth is 0.1 mm to 1 mm. A width of 0.1 mm to 20 mm and a depth of 0.1 mm to 2 mm are more preferable. Furthermore, the width of 0.1 mm or more and 2 mm or less and the depth of 0.1 mm or more and 0.5 mm or less are more preferable. That is, as the shape of the large-diameter portion 16, the pressure loss does not increase too much, the flow path is not easily blocked, the flow path can be quickly controlled for heating and cooling, and the flow rate of the fluid can be increased. Any flow channel shape may be used as long as the shearing force acts and molecular diffusion occurs in a state accompanied by a slight turbulent flow, thereby improving the mixing efficiency.

  In FIG. 3, three first microtubular channels 6 are arranged, but the number is not particularly limited. When arranging a plurality, the width and depth of each microtubular channel 6 may be the same or different. In addition, the inlet and outlet channel widths of the first microtubular channel 6 may be the same or different. A further illustration of the first plate is shown in FIG.

  The viscosity of the fluid flowing through the first microtubular channel is preferably 2000 mPa · s or less, and more preferably 1000 mPa · s or less. More preferably, it is 500 mPa · s or less.

  Next, the second plate 7 will be described in detail. As shown in FIG. 5, the second plate 7 has a rectangular and plate-like second microtubular flow path forming portion 7A.

  The second microtubular channel forming portion 7A has one second microtubular channel 8 on the upper surface 7a. The second microtubular channel 8 is formed in a groove shape from the lower end 7b of the second microtubular channel forming portion 7A toward the short direction (7c direction, Y direction in the figure). It is bent at right angles to the right end direction once near the center of the direction, and is open at the lower end 7b, the right end 7d, and the upper surface 7a. The opening at the lower end 7 b is the inlet 8 a of the second microtubular channel 8, and the opening at the right end 7 d is the outlet 8 b of the first microtubular channel 6. The inlet 8a communicates with the second fluid supply unit 2A to which the second fluid F1 is supplied.

  In the microtubular channel of the second plate used in the present invention, the fluid cross-sectional area flowing in a liquid-tight manner in the microtubular channel at the outlet is liquid-tight in the one microtubular channel in the inlet. The cross-sectional area is smaller than the cross-sectional area of the fluid flowing in a shape. By having such a structure, the second fluid F2 flows through the large-diameter inlet 8a at the inlet and flows into the small-diameter 8b. Each fluid second fluid F2 that has flowed into the small-diameter portion flows into the outlet 8b at a flow velocity larger than the flow velocity when flowing into the inlet, and flows into the mixing portion (S3 in FIG. 1). As a result, the mixing speed of the first fluid F1 and the second fluid F2 can be increased. In particular, it is particularly effective when at least one of the first fluid F1 and the second fluid F2 is a fluid that has low fluidity and is difficult to mix, that is, a high-viscosity fluid or a viscosity that differs greatly from each other. It can be demonstrated.

  The width and depth of the large-diameter portion are preferably in the range of, for example, a width of 0.1 mm or more and 100 mm or less and a depth of 0.1 mm or more and 5 mm or less in order to ensure uniformity of temperature distribution of the fluid and device strength. The range of 0.1 mm to 20 mm in width and 0.1 mm to 2 mm in depth is more preferable. That is, as the shape of the large diameter portion, the pressure loss does not become excessive, the flow path is not easily blocked, the flow path can be quickly controlled for heating / cooling, and the mixing performance can be improved. Any shape is acceptable.

Moreover, as a cross-sectional area of the fluid which distribute | circulates a large diameter part liquid-tightly, 0.01-500 mm < ² > is preferable and 0.01-40 mm < ² > is more preferable.

  The cross-sectional area of the small-diameter portion may be a cross-sectional area that is at least smaller than the cross-sectional area of the large-diameter portion. For example, the width and depth of the small-diameter portion are preferably in the range of 0.1 mm to 20 mm in width and 5 mm in depth, in the range of 0.1 mm to 5 mm in width, and 0.1 mm to 2 mm in depth. That is, as the shape of the small diameter portion, the pressure loss does not become too large, the flow path is not easily blocked, the flow path heating and cooling can be quickly controlled, and the productivity can be improved. Is preferred.

  Moreover, as a cross-sectional area of the fluid which distribute | circulates a small diameter part liquid-tightly, 0.01-100 mm2 is preferable and 0.01-10 mm2 is more preferable.

  The speed of the fluid when flowing through the second microtubular channel 8b is preferably 0.1 m / second or more, more preferably 0.3 m / second or more because shearing force acting on the fluid increases. More preferably, it is 1.0 m / second or more and 3.0 m / second or more is particularly preferable. In particular, when mixing fluids having high viscosities or when mixing fluids having viscosities greatly different from each other, the flow rate is preferably 1.0 m / second or more.

  The viscosity of the fluid flowing through the second microtubular channel is preferably 2000 mPa · s or less, and more preferably 1000 mPa · s or less. More preferably, it is 500 mPa · s or less.

  Further, as shown in FIG. 5, the second plate is divided by a plurality of walls in which the outlet portion communicating with the mixing portion is installed in parallel with the fluid traveling direction, and a plurality of flow paths are formed. Surprisingly, for example, one channel may be used as illustrated in FIG. Here, the number of walls is, for example, 0 to 250, and more preferably 1 to 50. Further, the number of the second microtubular channels formed on the second plate may be one as shown in FIG. 5, or may be plural as shown in FIG.

  Since the micromixer of the present invention can easily increase the number of inlets of the microtubular channel of the second plate, it is also possible to obtain a mixed fluid of many kinds of fluids. When various kinds of fluids are allowed to flow through the micromixer of the present invention, for example, at least one first plate and at least two second plates are stacked, and the stacked portion is the second plate. A micromixer having a laminated part in which the inlet part of the microtubular channel included in the first plate is installed on a side surface different from the side where the inlet part of the microtubular channel included in is installed can be preferably exemplified. An example of such a micromixer is the micromixer shown in FIG.

  You may laminate | stack the temperature control plate which distribute | circulates the medium for heat exchange with the micro mixer of this invention. For example, FIG. 7 shows a micromixer in which a temperature control plate, a first plate, and a second plate are stacked.

As shown in FIG. 7, the temperature control plate 12 is provided with a temperature control flow path 13 having a concave groove shape on one surface 12 a at a predetermined interval. The cross-sectional area of the temperature control flow path 12 is not particularly limited as long as heat can be transferred to the reaction flow path, but is generally in the range of 0.02 to 500.0 (mm ² ). More preferably, it is 0.05-40.0 (mm < ² >). The number of the temperature control flow paths 6 can adopt an appropriate number in consideration of heat exchange efficiency, and is not particularly limited, but is, for example, 1 to 1000, preferably 10 to 100 per plate. It is. The width of the flow path is preferably in the range of, for example, 0.2 mm to 100 mm in width and 0.1 mm to 5 mm in depth, and more preferably in the range of 0.5 mm to 20 mm in width and 0.1 mm to 2 mm in depth. . In other words, the shape of the large-diameter portion 16 is such that the pressure loss does not increase excessively, the flow path is not easily blocked, the flow path can be quickly controlled for heating and cooling, and the productivity can be improved. Any road shape may be used.

  As shown in FIG. 7, the temperature control flow path 12 includes a plurality of main flow paths 13a arranged along the longitudinal direction of the temperature control plate 12, and upstream and downstream end portions of the main flow path 13a. You may provide the supply side flow path 13b and the discharge side flow path 13c which are connected.

  In FIG. 7, the supply-side flow path 13b and the discharge-side flow path 13c are bent twice at right angles and open to the outside from the side surfaces 12d and 12e of the temperature control plate. As for the number of each temperature control channel 12, only the main channel 13a portion of the temperature control channel 12 is arranged, and the supply side channel 13b and the discharge side channel 13c are each composed of one. .

  In the laminate 11 configured as described above, the first fluid (F1) supplied in a pressurized state from the first fluid supply unit 1A into the case C is temporarily stored in the storage unit S1, and then stacked. The body 110 is divided into a plurality of first microtubular channels 6 provided in the body 110. Also, a plurality of second microtubules provided in the multilayer body 11 after being temporarily stored in the second fluid (F2) storage section S2 supplied in a pressurized state from the second fluid supply section 2A into the case C. Divided into flow paths 8.

  The 1st fluid (F1) which flowed into each 1st microtubular channel 6 of the 1st plate 5 leads to outlet 6e of the 1st microtubular channel 6, and is sent to mixing part S3. . In addition, the second fluid (F2) that has flowed into each second microtubular channel 8 of the second plate 7 is sent from the large diameter portion 9 to the small diameter portion 10 while increasing the flow velocity, and from the outlet 8b to the mixing portion. Sent to S3.

  The second fluid (F2) sent to the mixing unit S3 while increasing the flow rate is mixed with the second fluid (F2) sent to the mixing unit S3. At this time, since the speed of the second fluid (F2) is increased, the mixing efficiency in the mixing unit S3 is improved.

  The first fluid (F1) and the second fluid (F2) are mixed while generating turbulent flow in the mixing unit S3, and the obtained mixed fluid (F3) flows toward the mixed fluid delivery unit 5A. And it sends out from case C from sending part 5A.

  In the micromixer of the present invention, in addition to the above example, as shown in FIG. 8, one first plate for circulating E liquid and second liquid for circulating A liquid, B liquid, C liquid and D liquid respectively. 4 plates can be stacked to form a micromixer that mixes five types of solutions.

According to the above embodiment, the micromixer of the present invention can obtain the following effects.
(1) In the above-described embodiment, the micromixer 1 has a laminated portion in which the second plate is laminated on the first plate having the first microtubular channel, and the mixing portion. At least one of the second plate and the second plate has a single microtubular channel at the inlet, and a fluid cross-sectional area flowing in a liquid-tight manner in the microtubular channel at the outlet is The cross-sectional area is smaller than the cross-sectional area of fluid flowing in a liquid-tight manner in one microtubular channel in the section. By adopting such a configuration, the mixing efficiency of the first fluid and the second fluid can be increased, and even high viscosity fluids or different viscosity fluids having different viscosities can be mixed efficiently. it can.

  Hereinafter, the present invention will be described in more detail by way of examples. In the examples,% is based on weight unless otherwise specified.

<Reaction device used in Example 1>
In Example 1, the reaction device shown in FIG. 9 was used. In this device, the micromixer used was the micromixer shown in FIG. 1, and the micromixer 1 in which the lamination part had the lamination part shown in FIG. 7 was used.

  The micromixer 1 has one first plate 5 in which a first microtubular channel is formed by dry etching and a second plate 7 in which a second microtubular channel is also formed by etching. One plate, two temperature control plates 12 and plates 5, 7 and temperature control plates 12 are alternately stacked as shown in FIG. 7, and this stacked body is sandwiched between two cover plates. Yes. The material of the plate is SUS304. The plate thickness of the plates 5 and 7 is 0.4 mm. The temperature control plate 12 is 1.0 mm.

  The first microtubular channel 6 has a large diameter portion 6f of width 1.2 mm × depth 0.2 mm × length 38 mm, and a small diameter portion 6 g of width 0.4 mm × depth 0.2 mm × length 2 mm. did. The number of microtubular channels on the first plate 5 is ten.

  In the second plate 7, the cross-sectional dimension of the large-diameter portion 8a of the microtubular channel is 1.2 mm wide × 0.2 mm deep × 20 mm long. The small diameter portion 8b of the small tubular channel has a width of 0.4 mm, a depth of 0.2 mm, and a length of 2 mm, and the number of microtubular channels is ten. The cross-sectional dimension of the flow path of the temperature control plate 12 is width 1.2 × depth 0.5 × length (L1) 40 mm.

  In Example 1, the mixing efficiency of the first fluid and the second fluid was evaluated by synthesizing urethane acrylate using the reaction device shown in FIG. In FIG. 9, the outlet of the tank 61 for containing the first fluid and the inlet of the plunger pump 63 are connected via a pipe through which the first fluid passes, and the tank for containing the second fluid. The outlet of 62 and the inlet of the plunger pump 64 are connected via a pipe through which the second fluid passes. From the outlet of the plunger pump 63 and the outlet of the plunger pump 64, piping through which the first fluid or the second fluid passes through the plunger pump 63 or the plunger pump 64, respectively, extends. It is connected to the inlet of the micromixer 1.

  Further, the pipe connected to the outlet of the micromixer 1 is connected to the reaction line 1 including the chemical reaction microreactor 65 or 66 and the receiving container 68 via the connector 67, and the chemical reaction microreactor 65 or 66 and the receiving container. 69 is connected to reaction line 2 comprising 69.

The first fluid and the second fluid are mixed in the micromixer 1 to form a mixed fluid.
The mixed fluid is distributed to the reaction line 1 and the reaction line 2 according to the time when the mixed fluid is formed.

  The distributed mixed solution reacts while flowing through the reaction line 1 or the reaction line 2 and is cooled. The reaction is performed in the microreactor 65 and the cooling is performed in the microreactor 66.

  The microreactor 65 or 66 is the microreactor shown in FIG. 10, and the stacked portion for performing the reaction has the structure shown in FIG.

  The microreactor 65 will be described with reference to FIG. α is a fluid mixture of the first fluid and the second fluid. β is a reactant of the mixed fluid. γ is a heat exchange medium. The microreactor 65 is formed by alternately laminating three temperature control plates having five temperature control channels 6 formed by etching as well as two process plates having five reaction channels 4 formed by dry etching. Yes. The material of the process plate 2 and the temperature control plate 3 is SUS304, and the plate thickness is 1 mm. The cross-sectional dimensions of the reaction channel 4 and the temperature control channel 6 are both width 1.2 mm × depth 0.5 mm. The length of the reaction channel 4 is 40 mm. The length (L1) of the temperature control flow path 6 is 40 mm. The microreactor 65 is heated so that the temperature of the mixed fluid and the reaction product of the mixed fluid is 160 ° C.

  The microreactor 66 will be described with reference to FIG. α is a fluid mixture of the first fluid and the second fluid. β is a reactant of the mixed fluid. γ is a heat exchange medium. The microreactor 65 is formed by alternately laminating three temperature control plates having five temperature control channels 6 formed by etching as well as two process plates having five reaction channels 4 formed by dry etching. Yes. The material of the process plate 2 and the temperature control plate 3 is SUS304, and the plate thickness is 1 mm. The cross-sectional dimensions of the reaction channel 4 and the temperature control channel 6 are both width 1.2 mm × depth 0.5 mm. The length of the reaction channel 4 is 40 mm. The length (L1) of the temperature control flow path 6 is 40 mm. The microreactor 65 is cooled so that the temperature of the mixed fluid and the reaction product of the mixed fluid becomes 70 ° C.

  The reaction product obtained through the lines 1 and 2 is discharged to a receiving container 68 or 69 through a pipe connected to the outlet.

<Device used in Example 2>
In Example 2, a device to which the tank 61 for storing the first fluid, the tank 62 for storing the second fluid, the plunger pump, and the micromixer 2 was used was used. Specifically, the outlet of the tank 61 into which the first fluid is placed and the inlet of the plunger pump 63 are connected via a pipe through which the first fluid passes, and the second fluid is put in. The outlet of the tank 62 and the inlet of the plunger pump 64 are connected via a pipe through which the second fluid passes. From the outlet of the plunger pump 63 and the outlet of the plunger pump 64, piping through which the first fluid or the second fluid passes through the plunger pump 63 or the plunger pump 64, respectively, extends. It is connected to the inlet of the micromixer 2.

  In the micromixer 2, the first fluid and the second fluid are mixed to form a mixed fluid. The mixed fluid is discharged to a receiving container through a pipe connected to the micromixer 1 or 2.

  The micromixer 2 has a structure in which the temperature control plate 12 is omitted in FIG. Specifically, one first plate 5 on which the first microtubular channel is formed by dry etching and one second plate 7 on which the second microtubular channel is also formed by etching are used. Is sandwiched between two cover plates. The material of the plate is SUS304. The plate thickness of the plates 5 and 7 is 0.4 mm.

  The large diameter portion 6f of the first microtubular channel 6 of the first plate 5 has a width of 1.2 mm × a depth of 0.2 mm × a length of 38 mm, and the small diameter portion 6g has a width of 0.4 mm × depth of 0.1 mm. It was 2 mm × length 2 mm. The number of microtubular channels on the first plate 5 is ten. In the second plate 7, the cross-sectional dimension of the large-diameter portion 8a of the microtubular channel is 1.2 mm wide × 0.2 mm deep × 20 mm long. The small diameter portion 8b of the small tubular channel has a width of 0.4 mm, a depth of 0.2 mm, and a length of 2 mm, and the number of microtubular channels is one.

Example 1
A urethane acrylate was synthesized using an isocyanate compound adjusted to a viscosity of 2 mPa · s as the first fluid and a polyfunctional acrylate adjusted to a viscosity of 300 mPa · s as the second fluid. As the adjustment, a heating medium was sent to the temperature control plate 12, and the temperature of each fluid was set to 60 ° C.

  The above compound was circulated at a flow rate of 100 g / min with the plunger pumps 63 and 64 and circulated through the micromixer 1 to obtain a mixed fluid. The obtained mixed fluid was divided into an early stage and a late stage, and the connectors were operated to send them to the microreactors 65 and 66, respectively. In each microreactor, the reaction was allowed to proceed at 160 ° C. under a residence time of 50 seconds. Urethane acrylates obtained using the microreactors 65 and 66 are abbreviated as urethane acrylate (1-1) and urethane acrylate (1-2), respectively. As a result of gel permeation chromatography (GPC) analysis, the area ratio [%] of urethane acrylate in urethane acrylate (1-1) and urethane acrylate (1-2) and the area ratio [%] of residual acrylate were 95. The values were the same as 5 [%] and 1.3 [%]. From this, it can be considered that the micromixer 1 is uniformly mixed.

  In Example 1, the flow rate of the first fluid at the outlet of the microtubular channel in the mixing part of the micromixer of the present invention was 0.42 m / s, and the velocity of the second fluid was 1.66 m / s. It was.

Example 2
Water having a viscosity of 1 mPa · s and a water tank having a viscosity of 30 mPa · s were passed through a device having a micromixer by a plunger pump at a flow rate of 10 g / min. As a result, it was confirmed that mixing was possible without pulsation.

  In Example 2, both the flow velocity of the first fluid and the velocity of the second fluid at the outlet of the microtubular channel in the mixing portion of the micromixer of the present invention were 1.04 m / s.

Comparative Example 1
A heterogeneous fluid mixing experiment was conducted in the same manner as in Example 2 except that a Y-shaped micromixer was used instead of the micromixer 2. The flow path through which the first fluid provided in the Y-shaped micromixer is 0.4 mm wide × 0.2 mm deep × 15 mm long. The flow path through which the second fluid flows is similarly 0.4 mm wide × 0.2 mm deep × 15 mm long. The flow path through which the mixed solution flows is 0.8 mm wide × 0.2 depth × 15 mm long. Since the plate forming the flow path is made of the same material as the micromixer 1, the roughness of the flow path wall surface is the same as that of the micromixer 1.

  As a result of the experiment, it was confirmed that intermittent flow was observed in water having a low viscosity, and stable flow was difficult. In other words, the Y-shaped mixer is designed so that the fluids intersect with each other, so when two types of fluids with different viscosities are passed through the fluidic channels, the low-viscosity fluid has a higher flow rate, It can be presumed that intermittent feeding occurs because the fluid with high viscosity has a low flow velocity.

Comparative Example 2
Other than using the micromixer used in the example of JP-T 9-512742 instead of the micromixer 1 and circulating each with a plunger pump so that the flow rate when flowing is 12.5 g / min. Produced urethane acrylate (2′-1) and urethane acrylate (2′-2) in the same manner as in Example 1. The cross-sectional dimensions of the microtubular channels of the first and second plates of the micromixer used in the embodiment of JP-T 9-512742 are width 0.4 mm × depth 0.2 mm × length 38 mm. The number of microtubular channels is ten. The number of stacked layers is one each.

  The urethane acrylate area ratio [%] in the obtained urethane acrylate (2′-1) and urethane acrylate (2′-2) is 92 [%] and 77 [%], respectively, and the area of the remaining acrylate. The ratio [%] was 2.7 [%] and 18.8 [%], respectively, and the area ratios were different. From this result, it was concluded that urethane acrylates having different physical properties were produced and uniform mixing was not performed. Moreover, although it tried to distribute | circulate at 100 g / min, pressure loss became 10 Mpa or more, distribution was difficult and urethane acrylate was not obtained.

  In Comparative Example 2, the flow rate of the first fluid at the outlet of the microtubular channel was 0.05 m / s, and the velocity of the second fluid was 0.21 m / s.

C: Case of the micromixer C1: Left end of the case C C2: Lower right end of the case C C3: Lower left end of the case C C4: Upper end of the case C F1: First fluid F2: Second fluid F3: First Mixed fluid of fluid and second fluid H1: Heat medium S1: Reservoir for temporarily storing first fluid (F1) S2: Reservoir for temporarily storing second fluid (F2) S3: Mixer 1A: First 1 fluid supply section 1B: opening formed at the left end of case C 1C: connector connected to opening 2B 2A: second fluid supply section 2B: opening formed at the lower right end of case C 2C: opening Connector 3A connected to section 2B: Heat medium supply section for supplying heating medium H1 into case C 3B: Opening formed at lower left end of case C 3C: Connector connected to opening 3B 4A: Heat medium Sending part 4B: Upper part of case C Opening portion formed at the right end 4C: Connector connected to the opening portion 4B 5: First plate 5A: Delivery portion including the opening portion 5B and the connector 5C 5B: Opening portion formed at the right end portion of the case C 5C: Connector connected to the opening 5B 6: First microtubular channel 6A: First microtubular channel forming part 6a: Upper surface of the first microtubular channel forming part 6A 6b: First microtubular flow Left end 6c: Right end of first microtubular flow path forming portion 6A 6d: Inlet of first microtubular flow path 6e: Outlet of first microtubular flow path 6f: First 6g: Small diameter portion of the first microtubular flow path 6h: Tapered portion of the first microtubular flow path 7: Second plate 7A: Second microtubular flow Path forming part 7a: Upper surface of second microtubular channel forming part 7A 7b: Second microtubular channel Lower end 7c of forming part 7c: End in the short direction from lower end 7b of second microtubular flow path forming part 7A 7d: Right end of second microtubular flow path forming part 7A 8: Second 8a: inlet of the second microtubular channel 8b: outlet of the first microtubular channel 6 12: temperature control plate 12a: surface of the temperature control plate 12 13: surface of the temperature control plate 12 Temperature control flow channel 13a having a concave groove shape provided in 12a: Main flow channel 13b arranged along the longitudinal direction of temperature control plate 12 13b: Supply flow channel 13c communicating with main flow channel 13a 13c: Main flow channel 13a 61: Tank for storing the first fluid 62: Tank for storing the second fluid 63: Plunger pump 64: Plunger pump 65: Tube reactor 66: Tube reactor 67: Connector 68: Receiving container 9: receiving vessel 110: laminate

Claims (6)

A first plate having a first micro-tubular flow channel which first fluid is formed in a groove shape that leads to the fluid supply channel flows, is formed in a groove shape that leads to the fluid supply path in which the second fluid flows A laminated portion in which a second plate having a second microtubular channel is laminated;
A mixing section that communicates with the outlet of the first microtubular channel and the outlet of the second microtubular channel and that mixes the first fluid and the second fluid;
A micromixer having
The first plate has an inlet portion of a microtubular channel that leads to a fluid supply path and an outlet portion of the microtubular channel that leads to a mixing portion, and the inlet portion and the outlet portion are side portions of the first plate. In addition, the cross-sectional area of the fluid that flows in a liquid-tight manner in the microtubular channel at the outlet portion is smaller than the cross-sectional area of the fluid that flows in a liquid-tight manner in the microtubular channel at the inlet portion. A plate having
The first microtubular channel has a large-diameter portion with a large channel diameter at the inlet, a small-diameter portion with a small channel diameter at the outlet, and a tapered portion that moderates the diameter change from the large-diameter portion to the small-diameter portion. And
The cross-sectional area of the fluid that flows in a liquid-tight manner in the microtubular channel at the inlet of the first plate is 0.01 to 40 mm ² , and the fluid break that flows in the liquid-tight manner in the microtubular channel at the outlet is The area is 0.01 to 10 mm ² ;
The second plate has an inlet part of the microtubular channel that leads to the fluid supply path and an outlet part of the microtubular channel that leads to the mixing part, and the inlet part and the outlet part are side parts of the second plate. The microtubular channel at the inlet is a single channel, and the fluid cross-sectional area flowing in a liquid-tight manner in the microtubular channel at the outlet is a single channel at the inlet. A plate having a cross-sectional area smaller than a fluid cross-sectional area flowing in a liquid-tight manner in a microtubular channel,
The second microtubular channel is formed on the second plate surface in the middle of the large diameter portion having a large flow channel diameter at the inlet portion, the small diameter portion having a small flow channel diameter at the outlet portion, and the small diameter portion from the large diameter portion to the small diameter portion. It has a bent part that bends at right angles,
The fluid cross-sectional area that flows in a liquid-tight manner in one microtubular channel at the entrance of the second plate is 0.01 to 40 mm ² , and the fluid cross-sectional area in the microtubule in the outlet is fluid-tight. The fluid cross-sectional area is 0.01 to 10 mm ² ,
The area of the cross section leading to the outlet of the first microtubular channel and the outlet of the second microtubular channel of the mixing section is equal to the cross-sectional area of the outlet of the first microtubular channel and the second microtubular channel. A micromixer characterized by being 4 to 100 times the total cross-sectional area of the outlet .   A laminated portion in which at least one first plate and at least two second plates are laminated, wherein the laminated portion is different from a side surface on which an inlet portion of a microtubular channel included in the second plate is installed; The micromixer according to claim 1, further comprising a laminated portion in which an inlet portion of a microtubular channel included in the first plate is provided on a side surface.   The micromixer according to claim 1 or 2, wherein a temperature control plate having a heat exchange medium flow path through which the heat exchange medium flows is further laminated in the laminated portion. A method for producing a mixed fluid, wherein a mixed fluid is produced by mixing two or more kinds of fluids using the micromixer according to claim 1. The method for producing a mixed fluid according to claim 4, wherein the two or more fluids have different viscosities, the first fluid is a low-viscosity fluid, and the second fluid is a high-viscosity fluid. The method for producing a mixed fluid according to claim 5, wherein the difference in viscosity between the two or more fluids is 10 times or more.

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