JP4695570B2 - Mounting structure of microreactor temperature sensor to microreactor channel formation body - Google Patents

Description

The present invention relates to a structure for attaching a microreactor temperature sensor (hereinafter referred to as “temperature sensor” ) to a microreactor flow path forming body (hereinafter referred to as “flow path forming body” ) .

  A microchemical plant is a production facility that uses mixing, chemical reaction, separation, etc. in a microscale space, and has many advantages over conventional batch-type plants using large tanks and the like. For example, mixing of multiple fluids and chemical reactions can be performed with a small amount of sample in a short time, and if the production technology of products can be established at the laboratory level due to the small size of the device, it can be easily used for mass production by numbering up. It can be installed in equipment, can be applied to reactions involving dangers such as explosions, can be quickly adapted to the production of compounds that require high-mix low-volume production, and production volume can be easily adjusted to meet demand It can be done. For this reason, in the fields of chemical industry and pharmaceutical industry, it has been attracting attention as a suitable apparatus for producing materials and products by mixing or reacting fluids, and research and development has been actively conducted in recent years.

In microchemical plants, the reaction rate and the quality of the product can be improved by controlling the reaction temperature of the fluid. In order to control the reaction temperature, it is necessary to accurately measure the temperature of the fluid flowing through the micro flow path that is the reaction path. As a technique for measuring the temperature of a liquid flowing through a microchannel, for example, in Patent Document 1, a temperature sensor insertion port is provided in a microreaction main body part that forms a microchannel, and a liquid phase is obtained by the temperature sensor inserted therein. A microreactor configured to measure the temperature of is disclosed. Patent Document 2 discloses a microchannel device in which a temperature sensor is provided inside the microchannel.
JP 2004-321063 A JP 2006-130599 A

In the microreactor described in Patent Document 1, since the temperature sensor measures the heat of the reaction solution transmitted through the microreaction main body, there is a problem that the measurement temperature is inaccurate. In the microchannel device described in Patent Document 2, since the temperature sensor is provided in the microchannel, the accuracy of temperature measurement is improved, but the problem is that the liquid flow is disturbed by the temperature sensor and the flow is disturbed. there were. In particular, the flow path used in the microchemical plant has a cross-sectional area of several mm ² or less. A thermocouple sensor is used as the temperature measuring sensor, and its diameter is generally 0.5 mm (0.785 mm ² in cross-sectional area) or more. But in order to maintain the flow of while maintaining a laminar flow state, the use of the technique of Patent Document 2, there is a possibility that the turbulence temperature Dose capacitors becomes an obstacle.

  The present invention has been made in view of such problems, and can accurately measure the temperature of the fluid flowing in the flow path, and can prevent the flow from being disturbed. An object is to provide a temperature sensor mounting structure.

To achieve the above object, the present invention provides a mounting structure of the microreactor temperature sensor to the microreactor flow channel formation member (1,2,210) (3), fine channels (cross-sectional area of 1 mm ² or more and microreactor for temperature to measure 8 mm ² or less) of the channel (7,70) microreactor flow channel formation member forming a with (1,2,210), the temperature of the fluid flowing through the flow channel (7,70) A sensor (3),
In order to maintain the flow of the fluid in a state where the laminar flow is held on a part of the wall forming the microreactor flow path (7, 70) in which the flowing fluid undergoes a chemical reaction in a laminar flow , A substantially parallel recess (52, 521) is provided, and a temperature sensor (3) is provided in the recess (52, 521) so that the sheath (31) can flow while maintaining a stable laminar flow state. A part of the temperature measuring part (31a) composed of the bent part is exposed to the space in the flow path (7) or covered with an extremely thin sealing material (6a), and the sheath (31) is directly applied to the liquid. Or an extremely thin sealing material (6a) .

According to the present invention, since the temperature measuring part (31a) of the temperature sensor (3) is provided in the recess (52, 521), the flow of the fluid flowing through the flow path (7) is measured by the temperature sensor (3). hindered et is not the sensing portion (31a), it is never disturbed flow. Moreover, since the temperature measuring part (31a) of the temperature sensor (3) can directly contact the fluid flowing through the flow path (7, 70), the temperature of the fluid flowing through the flow path 7 can be accurately measured.

Moreover, a temperature measuring part (31a) can be reliably fixed by joining a recessed part (52) and the temperature measuring part (31a) of a temperature sensor (3) with a sealing material (6a). By sealing the gap between the recess (52) and the temperature measuring part (31a) of the temperature sensor (3) with the sealing material (6a), it is possible to prevent the fluid from staying in the gap. By making the surface of the sealing material (6a) and the inner peripheral surface of the flow path (7) substantially flush, the fluid flowing through the flow path (7) can be kept stable without being disturbed. . At least a part of the temperature measuring section (31a) of the temperature sensor (3) is exposed to a space in the flow path (7, 70) so that the flowing fluid can be kept stable without being disturbed. Thus, the temperature of the fluid can be measured more accurately. The temperature sensor (3) is suitable for application to a microdevice by using a sheath (31) provided with a thermocouple element (32) therein as a thermocouple temperature sensor configured as a temperature measuring unit. By configuring the flow path forming body (1, 2, 210) with a synthetic resin such as polytetrafluoroethylene resin or adhesive fluororesin, the heat storage property can be reduced, and the temperature of the fluid flowing through the flow path (7, 70). Can be measured even more accurately. By providing the heat insulating means (4) around the flow path forming body (1, 2, 210), the fluid flowing in the flow path (7) has very little influence of heat radiation to the outside or heat reception from the outside. Become.

  In addition, the code | symbol in the bracket | parenthesis of each means described in the column of the means for solving a claim and a problem shows the correspondence with the specific means as described in embodiment mentioned later.

  According to the structure for attaching the temperature sensor to the flow path forming body of the present invention, the temperature of the fluid flowing through the flow path can be accurately measured, and the flow can be prevented from being disturbed.

[First Embodiment]
Hereinafter, a first embodiment of the present invention will be described with reference to the accompanying drawings. 1 is a partial front cross-sectional view of the temperature sensor microdevice of the first embodiment, FIG. 2 is a cross-sectional view taken along line AA in FIG. 1, FIG. 3 is a partial cross-sectional view of the first block, and FIG. Is a partial front sectional view of the second block, FIG. 5 is a partial sectional side view of the second block, FIG. 6 is a sectional view showing the structure of the temperature sensor, and FIG. 7 is a diagram showing the main part of the present invention. 3A is a partial front sectional view, FIG. 3B is a partial side sectional view, and FIG. 3C is a bottom view.

  As shown in FIGS. 1 and 2, the microsensor with temperature sensor 10 according to the first embodiment of the present invention includes a first block 1, a second block 2, a thermocouple temperature sensor 3, and a heat insulating member 4. . Each of these components will be described.

  As shown in FIG. 3, the first block 1 is made of a substantially cylindrical body made of a metal such as stainless steel, and has a pore having an inner diameter of about 0.7 mm penetrating along the central axis J1. 11 is provided. A convex portion 12 that is hollow so as to communicate with the pores 11 is provided at the center of one end surface of the first block 1. The other end surface of the first block 1 is provided with a long groove 13 formed along the diameter portion thereof. The long groove 13 has a first groove 51 having a semicircular arc shape with a cross-sectional radius of approximately 0.9 mm, and a first groove 51 having a substantially semicircular arc shape having a cross-sectional radius of approximately 0.5 mm. 2 grooves 52. The long groove 13 communicates with the pore 11 at the central portion in the longitudinal direction.

  As shown in FIG. 4, the second block 2 is formed of a substantially rectangular parallelepiped body made of a metal such as stainless steel like the first block 1, and the inside of the second block 2 is the center in the longitudinal direction of the second block 2. A fine hole 21 having a diameter of about 1.8 mm penetrating along the axis J2 and a cylindrical hole 22 opened from one surface parallel to the longitudinal direction of the second block 2 to the upper half position of the fine hole 21 are provided. Since the pore 21 and the cylindrical hole 22 communicate with each other, the inner circumferential cross section of the pore 21 has a semicircular arc shape at the communicating portion, as shown in FIG. Both ends of the pore 21 are an inlet port 23 and an outlet port 24 in which female threads for pipe attachment are formed. The cylindrical hole 22 has a size that allows the first block 1 to be inserted. The one surface parallel to the longitudinal direction of the second block 2 is an annular convex portion 25 communicating with the cylindrical hole 22.

  As shown in FIGS. 1 and 6, the thermocouple temperature sensor 3 includes a sheath 31, a thermocouple element 32, a filling member 33, an adapter 34, a lead wire 35, and the like. The sheath 31 is made of an elongated pipe body made of stainless steel or ceramics. The diameter is about 0.5 mm, one end is configured as a closed end, and the other end is configured as an open end. The thermocouple element 32 is formed by joining one end of each of two strands 61 and 62 made of different kinds of metals, for example, a chromel strand and an aramel strand, at a junction point 63. Be placed. The filler 33 is made of ceramics such as alumina, etc., sufficiently achieves thermal contact between the closed end of the sheath 31 and the junction 63 of the thermocouple element 32, and the thermocouple element in the sheath 31. In order to ensure the mechanical retention of 32, the inner space of the sheath 31 is filled with a thermocouple element 32 embedded therein. Both strands 61 and 62 extend from the junction 63 in the sheath 31, pass through the open end, enter the adapter 34, and are connected to the lead wire 35. The lead wire 35 is connected to a control circuit (not shown), and temperature measurement is performed based on a voltage due to a dissimilar metal junction at a junction 63 generated according to the temperature.

  The heat insulating member 4 is made of asbestos, porous ceramics, and the like, and is provided so as to cover the first block 1 and the second block 2. A vacuum heat insulating device may be used.

  Next, a method of assembling the temperature sensor-equipped microdevice 10 including the above-described components will be described.

First, the sheath 31 is inserted from the one side 11 a of the pore 11 in the first block 1 to penetrate the first block 1. Next, a portion 31a of a certain length from the tip of the sheath 31 coming out from the other side 11b of the pore 11 is bent into an L shape. Next, the sheath 31 is pulled up, and the bent portion 31 a is embedded in the second groove 52 along the longitudinal direction of the second groove 52. Next, the first block 1 is placed in a state where the long groove 13 is on the upper side, the sealing material 6a is poured into the second groove 52 and the pores 11, and is dried for a predetermined time.

The sealing material 6 a fixes the bent portion 31 a of the sheath 31 to the second groove 52 and seals the gap between the second groove 52 and the bent portion 31 a of the sheath 31 and the second groove 52. Further, the sheath 31 in the pore 11 is fixed to the pore 11. The inside of the second groove 52 is finally in the following state. That is, as shown in FIG. 7, the surface of the sealing material 6a and the inner peripheral surface of the flow path 7 are substantially flush. Further, a part of the bent portion 31a of the sheath 31 is exposed to the space in the flow path 7 or is covered with an extremely thin sealing material 6a.

When the sealing material 6 a is solidified, the first block 1 is fitted into the cylindrical hole 22 of the second block 2. At this point, the flow path 7 is formed by the first groove 51 and the semicircular arc portion of the pore 21. The channel 7, the cross-sectional area in the present invention is 1 mm ² or more and corresponds to 8 mm ² or less of the flow path. Then, the boundary part of the 1st block 1 and the 2nd block 2 is welded with the sealing material 6b. Finally, the first block 1 and the second block 2 are covered with a heat insulating member 4. Through the above operation, the microsensor with temperature sensor 10 shown in FIGS.

  Next, a usage example of the microdevice with temperature sensor 10 will be described with reference to FIG. FIG. 8 is a schematic view of a reaction system using a microdevice with a temperature sensor. As shown in FIG. 8, the reaction system 20 includes a first liquid supply unit 71, a second liquid supply unit 72, a first temperature adjustment unit 73, a second temperature adjustment unit 74, a microdevice with temperature sensor 10, a microreactor 81, It consists of a controller 9 and pipes 75, 83 and 84.

  The 1st liquid supply part 71 is comprised so that the 1st liquid which is a to-be-reacted liquid can be pumped by a predetermined pressure. The 2nd liquid supply part 72 is comprised so that the 2nd liquid which is a to-be-reacted liquid can be pumped by predetermined pressure. The first temperature adjustment unit 73 includes means for heating or cooling the first liquid supplied from the first liquid supply unit 71 based on a control signal S <b> 2 from the controller 9. The second temperature adjustment unit 74 includes means for heating or cooling the second liquid supplied from the second liquid supply unit 72 based on the control signal S <b> 2 from the controller 9. The microreactor 81 includes a microchannel 82 formed so that the reaction proceeds in a state where the first liquid and the second liquid maintain a laminar flow. The controller 9 is configured to send a control signal S2 to the first temperature adjustment unit 73 and the second temperature adjustment unit 74 based on the temperature signal S1 obtained by the microdevice with temperature sensor 10.

  The operation of the reaction system 20 and the operation and effect of the temperature sensor microdevice 10 will be described. The first liquid supply section 71 and the second liquid supply section 72 simultaneously supply the first liquid and the second liquid to the temperature sensor microdevice 10 through the pipe 75, respectively. The pressure of each liquid at this time is set to such a magnitude that the first liquid and the second liquid can maintain a laminar flow state.

The temperature of the two-layer liquid of the first liquid and the second liquid flowing through the flow path 21 of the temperature sensor microdevice 10 is measured by the thermocouple temperature sensor 3. In the temperature sensor microdevice 10, since the surface of the sealing material 6a and the inner peripheral surface of the flow path 7 are substantially flush, there is little flow resistance or disturbance due to unevenness or the like, and the first liquid and the second liquid Can flow while maintaining a stable laminar flow state. Further, since a part of the bent portion 31a of the sheath 31 is exposed to the space in the flow path 7 or is covered with the ultrathin sealing material 6a, the sheath 31 is directly exposed to the liquid or is extremely thin. Since it contacts via the sealing material 6a, exact temperature measurement is possible.

  When the measured temperature is higher than the target temperature, the controller 9 reduces the temperature of the first liquid and the second liquid supplied from the first liquid supply unit 73 and the second liquid supply unit 74. The first temperature adjusting unit 73 and the second temperature adjusting unit 74 are controlled. On the contrary, when the measured temperature is lower than the target temperature, the controller 9 increases the temperatures of the first liquid and the second liquid supplied from the first liquid supply unit 73 and the second liquid supply unit 74. In addition, the first temperature adjusting unit 73 and the second temperature adjusting unit 74 are controlled. This control may be corrected based on the thermal conductivity of the first block 1 and the second block 2.

The first liquid and the second liquid that have come out of the temperature sensor microdevice 10 enter the microreactor 81 via the pipe 83. Thereafter, the first liquid and the second liquid cause the reaction to proceed while maintaining a laminar flow in the microchannel 82. Then, from the outlet port of the microreactor 81, the reacted liquid whose reaction has been completed is led out to the next step through the pipe 84. Since the 1st block 1 and the 2nd block 2 are coat | covered with the heat insulation member 4, the liquid which flows through the flow path 7 has very little influence of the thermal radiation to the outside or the heat receiving from the outside.
[Second Embodiment]
Next, a second embodiment of the present invention will be described. 9 is a partial front cross-sectional view of the microdevice with temperature sensor of the second embodiment, FIG. 10 is a view taken along the line BB in FIG. 9, and FIG. 11 is a main part of the microdevice with temperature sensor of the second embodiment. FIG. In these drawings, the same components as those of the temperature sensor-equipped microdevice 10 of the first embodiment are denoted by the same reference numerals, and description thereof is omitted.

As shown in FIGS. 9 and 10, the microdevice with temperature sensor 20 of the second embodiment includes a flow path forming body block 210, a thermocouple type temperature sensor 3, and a heat insulating member 4. The flow path forming body block 210 is a substantially rectangular parallelepiped shaped body integrally molded from polytetrafluoroethylene resin or adhesive fluororesin. Inside thereof, there are provided pores 211 having a diameter of about 1.8 mm that penetrate along the central axis J3 in the longitudinal direction of the flow path forming block 210. Both ends of the pore 211 are an inlet port 231 and an outlet port 241 for pipe attachment, respectively. A flow path 70 is formed by the pores 211. Passage 70, the cross-sectional area in the present invention is 1 mm ² or more and corresponds to 8 mm ² or less of the flow path.

  A groove 521 formed so as to overlap the pore 211 is provided at the center in the longitudinal direction of the pore 211. The groove 521 has a substantially semicircular arc shape with a cross-sectional radius of about 0.5 mm. The bent portion 31 a of the sheath 31 is embedded in the groove 521. A part of the surface of the bent portion 31 a is exposed to the space in the flow path 70.

  Next, with reference to FIGS. 12 and 13, a manufacturing method of the microdevice with temperature sensor 20 will be described. FIG. 12 is a view showing a mold apparatus for manufacturing the microdevice with temperature sensor of the second embodiment, and FIG. 13 is a view showing a manufacturing procedure of the microdevice with temperature sensor of the second embodiment.

  As shown in FIG. 12, the mold tool 40 includes a first molding part 41, a second molding part 42, and two substantially round bar members 43, 43. The 1st molding part 41 and the 2nd molding part 42 are provided with the cavity for shape | molding the upper half part and lower half part of the microdevice 20 with a temperature sensor, respectively. On the upper surface of the first molding portion 41, a pore 41h having a size that allows the sheath 31 to be inserted, and a resin introduction hole 41n to which the resin injection nozzle 441 in the resin supply portion 44 is connected are formed. The two substantially round bar members 43 and 43 are both processed into the same shape, and each include a large-diameter portion 43a and a small-diameter portion 43b. The 1st molding part 41 and the 2nd molding part 42 are provided with semicircular grooves 41m and 42m provided with a diameter substantially the same as the outer diameter of large diameter parts 43a and 43a of substantially round bar member 43, respectively. The first molding portion 41 and the second molding portion 42 can be locked (sealed) with substantially round bar members 43 and 43 sandwiched therebetween.

  The microdevice 20 with temperature sensor is manufactured as follows. First, as shown in FIG. 13A, the sheath 31 whose tip is bent in an L shape is inserted into the pore 41 h of the first molding portion 41. Next, as shown in FIG. 13B, the large-diameter portions 43a and 43a of the substantially round bar member 43 are placed in the semicircular grooves 42m and 42m of the second molding portion 42, respectively. At this time, the end surfaces of the small-diameter portions 43b of both substantially round bar members 43 are brought into contact with each other. Next, as shown in FIG. 13C, the first molding part 41 is overlaid on the second molding part 42 to lock both molding parts. At this time, the bent portion 31 a of the sheath 31 is placed parallel to the longitudinal direction of the substantially round bar member 43 and on the small-diameter portion 43 b.

  Next, the melted polytetrafluoroethylene or adhesive fluororesin is pumped from the resin introduction hole 41 into the cavity through the resin injection nozzle 441 from the resin supply unit 44. As shown in FIG. 13D, when the inside of the mold is filled with polytetrafluoroethylene or adhesive fluororesin and cooled for a predetermined time, the two substantially round bar members 43 and 43 are pulled out. Furthermore, the first molding part is removed from the second molding part when it is cooled for a predetermined time. Through the above operation, the flow path forming block 210 to which the temperature sensor 3 is attached is completed. Finally, by covering the periphery of the flow path forming block 210 with the heat insulating member 4, the microdevice 20 with temperature sensor shown in FIGS.

  The usage example of the microdevice with temperature sensor 20 is almost the same as that in the first embodiment. By replacing the microdevice with temperature sensor 10 in FIG. Similar effects can be obtained. In the case of the second embodiment, since the flow path forming block 210 is made of synthetic resin such as polytetrafluoroethylene or adhesive fluororesin and has particularly low heat storage, the temperature of the liquid flowing through the flow path 7 is further increased. It becomes possible to measure accurately.

  As mentioned above, although embodiment of this invention was described, embodiment disclosed above is an illustration to the last, Comprising: The scope of the present invention is not limited to this embodiment. The scope of the present invention is defined by the terms of the claims, and is intended to include any modifications within the scope and meaning equivalent to the terms of the claims. For example, the cross-sectional shape of the flow paths 7 and 70 is not limited to the circular shape shown here, and may be a square, for example. Further, in the first embodiment, the first block 1 and the second block 2 serving as the flow path forming body are not made of metal, but are made of synthetic resin such as polytetrafluoroethylene or adhesive fluororesin as in the second embodiment. However, a suitable commercially available adhesive may be used as the bonding material instead of the silver candy.

It is a front fragmentary sectional view of the microdevice with a temperature sensor for microreactors . It is an AA arrow line view of FIG. It is 3 surface partial sectional drawing of a 1st block. It is a front fragmentary sectional view of the 2nd block. It is side surface partial sectional drawing of a 2nd block. It is sectional drawing which shows the structure of the temperature sensor for microreactors . It is a figure which shows the principal part of this invention. It is the schematic of the reaction system using the microdevice with a temperature sensor for microreactors . It is a front fragmentary sectional view of the microdevice with a temperature sensor for microreactors of a 2nd embodiment. It is a BB line arrow directional view of FIG. It is a figure which shows the principal part of the microdevice with a temperature sensor for microreactors of 2nd Embodiment. It is a figure which shows the metal mold | die instrument for manufacturing the microdevice with a temperature sensor for microreactors of 2nd Embodiment. It is a figure which shows the manufacture procedure of the microdevice with a temperature sensor for microreactors of 2nd Embodiment.

Explanation of symbols

1 First block ( microreactor flow path forming body)
2 Second block ( microreactor channel forming body)
3 Thermocouple type temperature sensor (temperature sensor for microreactor )
4 Insulation member (insulation means)
6a, 6b Sealing material 7 Channel 31 Sheath 31a Bent part of sheath (temperature measuring part)
32 Thermocouple element 52 Concavity 70 Channel 210 Microreactor channel formation body 521 Concavity

Claims (4)

The microreactor temperature sensor (3) is attached to the microreactor channel forming body (1, 2, 210), and has a fine channel (cross-sectional area of 1 mm ² or more and 8 mm ² or less) (7, 70). And a microreactor channel forming body (1, 2, 210) formed with a microreactor temperature sensor (3) for measuring the temperature of the fluid flowing through the channel (7, 70),
In order to maintain the flow of the fluid in a state where the laminar flow is held on a part of the wall forming the microreactor flow path (7, 70) in which the flowing fluid undergoes a chemical reaction in a laminar flow, A substantially parallel recess (52, 521) is provided, and a temperature sensor (3) is provided in the recess (52, 521) so that the sheath (31) can flow while maintaining a stable laminar flow state. A part of the temperature measuring part (31a) composed of the bent part is exposed to the space in the flow path (7) or covered with an extremely thin sealing material (6a), and the sheath (31) is directly applied to the liquid. A structure for attaching a microreactor temperature sensor to a microreactor flow path forming body, wherein the microreactor flow path forming body is configured to be in contact with each other via an ultrathin sealing material (6a).   The structure for attaching a temperature sensor for a microreactor to a microreactor channel forming body according to claim 1, wherein the recess (52) and the temperature measuring part (31a) of the temperature sensor (3) are joined together by a sealing material (6a).   The microreactor to the microreactor channel forming body according to claim 1 or 2, wherein a gap between the recess (52) and the temperature measuring part (31a) of the temperature sensor (3) is sealed with a sealing material (6a). Temperature sensor mounting structure.   The surface of the sealing material (6a) and the inner peripheral surface of the flow path (7) are substantially flush with each other so that the flowing fluid can be kept stable without being disturbed. A structure for attaching a temperature sensor for a microreactor to the microreactor channel forming body described.

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