JP4541219B2 - Microdevice and control method thereof - Google Patents

Description

  The present invention has a plurality of main body forming members each formed with a flow path forming portion and constitutes a combination structure in which the plurality of main body forming members can be disassembled, and the plurality of main body forming members The present invention relates to a microdevice including a device main body in which a fluid flow path is formed by combining the flow path forming portions and a control method thereof.

  In conventional large batch reactors, in the reaction case where the mixing time of the raw material fluid to be brought into contact with the reaction affects the reaction yield and quality, from the viewpoint of reactivity, a large stirring blade or high pressure In many cases, a device for promoting mixing such as a mixer is attached.

  However, such measures increase the incidentalness of the apparatus, increase the cost of the apparatus itself, and increase the production efficiency per apparatus volume. Furthermore, in terms of temperature control, batch-type reactors are greatly used for temperature operations such as cooling and temperature rise due to a reduction in the heat transfer area per unit volume of the reaction fluid inherent in the batch reactor. Tends to require a long time, and the production efficiency per unit volume decreases.

  In response to such problems, chemical technology organizations and chemical industries around the world are exploring the possibility of technological improvements by applying microreactors having microchannels, so-called microreactors. Specifically, the microreactor is applied from the reverse concept to reduce the tendency to deteriorate in terms of mixing properties and temperature controllability that occurs in the chemical industry, which is referred to as scale-up. Expected to be markedly improved by the effects of this.

  Regarding a microreactor, for example, in Patent Document 1, in a chemical processing apparatus including a pressure vessel and a microreactor disposed in the pressure vessel, a first fluid is injected into the microreactor through a first supply path, and at the same time, By injecting into the internal volume of the pressure vessel through the pressure equalizing path branched from the supply channel, the internal pressure of the microreactor is increased and the pressure difference between the internal volume of the microreactor and the internal volume of the pressure vessel is the maximum of the microreactor. It is disclosed that the pressure limit is not exceeded. And according to this, it is described that the microreactor can be operated at a high pressure.

Patent Document 2 discloses a microreactor comprising a substrate having a fluid path, having a catalyst on the surface of the fluid path, and the substrate being exothermic. And according to this, it is described that a micro reactor for a fuel cell that can be sufficiently used for a portable device with high power consumption and that has high reaction efficiency can be provided.
JP 2004-105962 A JP 2003-331896 A

  In the field of microreactors, establishment of the idea of mass production from the viewpoint of industrialization in the future, simplification of maintenance management such as maintenance, and generalization to various reaction systems are expected.

  Among these, regarding the establishment of the idea of mass production, the idea called numbering up, which increases the number of devices in proportion to the desired production volume, is one of the major directions for mass production. . In addition, for simplified maintenance management and generalization to various reaction systems, the microreactor is configured as a single unit with a substrate with a reaction fluid flow path formed on the plate surface, and a large number of them are stacked. Is being considered. With such an apparatus configuration, workability in terms of maintenance such as cleaning after use is improved, maintenance management is simplified, and an optimum reaction fluid flow path is formed for the reaction system to be implemented. General purpose is achieved by selecting an appropriate substrate appropriately.

  By the way, when a substrate stacked microreactor is used, there is a problem that a product may not be obtained in an expected yield in a certain reaction system.

  When the corrosion of the microreactor over time was involved, or when the reaction fluid was a gas, it was extremely difficult to identify the fact. Was found to be a leakage of reaction fluid from the microreactor. In other words, the present inventors are not limited to a substrate-laminated microreactor processed with high accuracy, but the flow state due to the pressure, temperature, viscosity, etc. of the flowing reaction fluid, the phase state based on the reaction conditions, the substrate-like member It was found that the reaction fluid flowing through the reaction fluid flow channel leaks from the mating portion of the substrate-like member depending on the contact state between the substrate-like members based on the processing accuracy of the mating surfaces.

  The present invention has been made in view of the above points, and an object of the present invention is to provide a microdevice that regulates leakage of a circulating fluid flowing through a fluid flow channel from a device body and a control method thereof. is there.

The microdevice of the present invention that achieves the above object is as follows.
The plurality of main body forming members each having a flow path forming portion are formed, and the plurality of main body forming members constitute a combined structure that can be disassembled, and the flow path forming portions of the plurality of main body forming members A device body in which a fluid flow path is formed in combination,
Sealing fluid housing that forms a sealing fluid housing region that covers a linear member joining portion formed by at least one pair of the plurality of body forming members exposed outside the fluid flow path inside the device body. And
Is provided.

  According to the above configuration, if the sealing fluid is accommodated in the sealing fluid accommodating portion, and the magnitude relationship between the circulating fluid flowing through the fluid flow path and the pressure of the sealing fluid in the sealing fluid accommodating portion is controlled, the members are aligned. A sealing fluid atmosphere is formed so as to cover the portion, and the leakage of the circulating fluid in the fluid flow path from the member matching portion is regulated by the sealing fluid atmosphere.

  Here, in the present application, the microdevice means a microfluidic device such as a microreactor or a micromixer having a fluid flow path inside the device body.

And the control method of the microdevice of the present invention includes:
The plurality of main body forming members each having a flow path forming portion are formed, and the plurality of main body forming members constitute a combination structure that can be disassembled, and the flow path forming portions of the plurality of main body forming members Is a micro device having a device body in which a fluid flow path is formed inside,
The fluid channel from the member mating part to cover a linear member mating part formed by at least one pair of the plurality of body forming members exposed outside the fluid channel inside the device body. An atmosphere of a sealing fluid that restricts leakage of the circulating fluid is formed.

  If it carries out as mentioned above, while the sealing fluid atmosphere is formed so that a member matching part may be covered, the leakage of the circulation fluid of the fluid flow path from a member matching part is controlled by the sealing fluid atmosphere.

  According to the present invention, it is possible to form a sealing fluid atmosphere so as to cover the member mating portion, and it is possible to regulate leakage of the circulating fluid in the fluid flow path from the member mating portion by the sealing fluid atmosphere. it can.

  Hereinafter, embodiments of the present invention will be described.

  The microdevice of the present invention includes a device main body and a sealing fluid accommodating portion.

  The device main body includes a plurality of main body forming members each having a flow path forming portion. The device main body has a combination structure in which the plurality of main body forming members can be disassembled, and the fluid flow paths are formed by combining the flow path forming portions of the plurality of main body forming members. .

  The sealing fluid storage part forms a sealing fluid storage region for storing the sealing fluid. The sealing fluid accommodation region is a region that covers a linear member joining portion formed by at least a pair of the plurality of body forming members exposed outside the fluid flow path inside the device body.

  According to such a micro device, if the sealing fluid is accommodated in the sealing fluid accommodating part, and the magnitude relationship between the circulating fluid flowing through the fluid flow path and the pressure of the sealing fluid in the sealing fluid accommodating part is controlled, A sealing fluid atmosphere can be formed so as to cover the member mating portion, and leakage of the circulating fluid in the fluid flow path from the member mating portion can be regulated by the sealing fluid atmosphere.

  It is sufficient that the pressure of at least one of the circulating fluid in the fluid flow path and the sealing fluid in the sealing fluid storage portion is controlled. Therefore, both the pressure of the circulating fluid in the fluid flow path and the pressure of the sealing fluid in the sealing fluid storage portion may be controlled, or one of the pressures may be controlled.

  Here, as a specific configuration of the device main body, for example, a combination structure of a plurality of main body forming members is a combination structure of a plurality of block-shaped members or a stacked structure of a plurality of substrate-shaped members. be able to.

  When the device main body is composed of an overlapping structure of a plurality of substrate-like members, disassembly maintenance and assembly work can be easily performed. Moreover, since it is a superposition structure, a fluid flow path of many or a long distance can be comprised as a whole by forming a flow path formation part using each board-like member to the maximum.

  As a specific configuration of the sealing fluid storage unit, for example, a first configuration by a device body storage container formed so that a device body is stored and a sealing fluid storage region covers the device body, and a plurality of substrate-like members are stacked. Examples include a second configuration of a device main body configured with a mating structure formed so as to surround the outer periphery where the linear member mating portion is exposed.

  According to the first configuration, since the sealing fluid storage portion is configured by the device main body storage container, the structural separation between the sealing fluid storage region and the outside air can be reliably performed, and the pressure control of the sealing fluid is performed. Convenient. In addition, the conventional microdevice itself may be accommodated in a specific container, and can be configured without requiring a new device design. On the other hand, according to the second configuration, the sealing fluid storage portion is attached to a conventional microdevice configured by a superposed structure of a plurality of substrate-like members, or the microfluidic device is processed to provide the sealing fluid storage portion. What is necessary is just to form, and an apparatus can be comprised easily. Further, according to the second configuration, since the device configuration is compact, there is an advantage that the amount of sealing fluid stored in the sealing fluid storage region may be small. In either of the first and second configurations, there is an advantage that the conventional microdevice itself can be used as it is.

  The action effect peculiar to the microdevice is achieved due to the narrow fluid flow path inside the device body. Therefore, from this viewpoint, the equivalent diameter of the cross section of the fluid flow path is preferably 2000 μm or less, more preferably 500 μm or less, and even more preferably 100 μm or less. Here, the equivalent diameter is a diameter of a perfect circle having the same area as the cross-sectional area of the channel. On the other hand, from the viewpoint of processing accuracy and productivity, it is preferable that the equivalent diameter of the cross section of the fluid flow path is 20 μm or more.

  The restriction of the leakage of the circulating fluid in the fluid flow path from the member matching section is performed by setting a sealing fluid atmosphere that regulates the leakage of the circulating fluid in the fluid flow path from the member matching section so as to cover the linear member matching section. Achieved by forming.

  The most effective method is to make the pressure of the sealing fluid in the sealing fluid atmosphere higher than the pressure of the circulating fluid in the fluid flow path. However, the pressure of the sealing fluid in the sealing fluid atmosphere is not necessarily higher than the pressure of the circulating fluid in the fluid flow path. If the pressure difference between the two is 1.5 MPa or less, the circulating fluid in the fluid flow path is temporarily Even if the pressure of the sealing fluid in the sealing fluid atmosphere is higher than the pressure of the above, the leakage of the circulating fluid from the member mating portion can be sufficiently restricted. Here, if the pressure difference between the two is larger than 1.5 MPa, if the pressure of the circulating fluid in the fluid flow path is higher than the pressure of the sealing fluid in the sealing fluid atmosphere, leakage of the circulating fluid from the device body On the other hand, in the opposite case, the flow of the sealing fluid into the device body is facilitated. From the above viewpoint, it is more effective if the pressure difference between the two is 0.5 MPa or less.

  The leakage of the circulating fluid from the member mating portion becomes particularly significant when the circulating fluid pressure in the fluid flow path is set high. Therefore, when the pressure of the circulating fluid in the fluid flow path is set to 5.0 MPa or more, a particularly remarkable effect according to the present invention can be obtained.

  In addition to forming a sealing fluid atmosphere for restricting the leakage of the circulating fluid, the sealing fluid may be circulated. In this way, even if a harmful circulation fluid leaks, safety can be ensured by the dilution effect. Moreover, when performing pressure control of the sealing fluid, the pressure operation can be stably performed.

  In this case, the temperature of the device body may be adjusted using the circulating fluid as a heat medium. If it does in this way, in addition to regulation of the leakage of the circulation fluid from a member fitting part, temperature regulation of a device main part can be performed with sealing fluid.

  The sealing fluid in the sealing fluid atmosphere may be a reaction inert gas. In this way, since the sealing fluid is a reaction-inactive gas, it is possible to prevent the circulating fluid from contacting and reacting with the sealing fluid. Here, the reaction-inert gas sealing fluid is any of a rare gas such as helium and argon, nitrogen, carbon dioxide, and a mixture thereof.

  The microdevice having the above configuration is not particularly limited in use, such as a microreactor or a micromixer.

  Hereinafter, an example of a microreactor as an embodiment of the present invention will be described in detail with reference to the drawings.

(Embodiment 1)
FIG. 1 shows a microreactor system (microdevice system) S according to the first embodiment.

  The microreactor system S includes a microreactor (microdevice) 100 and an incidental part such as a reaction fluid supply system.

  The microreactor 100 includes a reactor main body (device main body) 10 and a reactor main body storage container (device main body storage container) 201 that stores the reactor main body (device main body). Therefore, the microreactor 100 is related to the first configuration.

  The reactor main body 10 is of a substrate laminated type, and has first and second substrate-like members (main body forming members) 11 and 12 having the same outer shape that constitute an overlapping structure (combined structure) that can be disassembled vertically. is doing.

  A through-hole is formed in the first substrate member 11. The through hole is formed in the reaction fluid inflow portion 161.

  A through hole is formed in the second substrate member 12, and the through hole and the through hole of the first substrate member 11 are formed on the upper surface side, that is, on the mating surface side with the first substrate member 11. A groove is formed so as to communicate with each other. The through hole of the second substrate member 12 is formed in the reaction fluid outflow portion 162.

  The reactor main body 10 is laminated such that these first and second substrate-like members 11 and 12 are overlapped with each other with their mating surfaces in contact with each other, and clip means such as joint fastening with bolts and nuts, etc. (Not shown) are integrated. And the concave groove of the 2nd substrate-like member 12 and the lower surface part of the 1st substrate-like member 11 corresponding to this are each constituted by channel formation part 17, and the 1st and 2nd substrate-like member 11, The reaction fluid flow paths 18 are formed inside the reactor main body 10 by being combined by overlapping the 12. Further, on the side surface of the reactor main body 10, a linear member matching portion 19 of the first substrate-like member 11 and the second substrate-like member 12 overlapped is formed so as to extend along the outer periphery. The linear member matching portion 19 is exposed outside the reaction fluid flow path 18 inside the reactor main body 10.

  According to the reactor main body 10 configured by superposing the first and second substrate members 11 and 12 as described above, the disassembly maintenance and the assembly work can be easily performed. If the flow path forming portion 17 is formed by making the most of 12, the reaction fluid flow paths 18 having a large number or a long distance can be configured as a whole. The reactor body 10 has the same configuration as that of a conventional substrate-stacked microreactor itself.

  The material forming each of the first and second substrate-like members 11 and 12 of the reactor body 10 is not particularly limited, and a wide range of metal materials, ceramic materials, resin materials, and the like can be used. Among them, from the viewpoint of heat resistance and chemical resistance to the reaction fluid that is a circulating fluid, those that are rich in dimensional stability and that do not cause changes in the processing accuracy of the mating surfaces of the first and second substrate members 11, 12 are preferable. Further, from the viewpoint of handling in industrial operation, those that are less likely to be damaged by contact between members are preferable. Specifically, the material is preferably a high-hardness metal material or ceramic material having a Vickers hardness (conforming to JIS Z 2244) of 80 HV or more, for example, austenitic steel typified by SUS304 or SUS316, or SUS430. Ferritic steel, ferrite and austenitic duplex stainless steel represented by SUS329, metal materials such as Hastelloy 276C, Ni alloy, metallic materials such as titanium alloy represented by pure titanium and 6-4 titanium alloy, heat resistant hard glass And ceramic materials such as quartz glass, alumina, silicon carbide, silicon nitride, and aluminum nitride. However, a metal material is preferable when pressure resistance is required depending on use conditions. Further, the first and second substrate-like members 11 and 12 may be formed of the same material or may be formed of different materials.

  The shape of each of the first and second substrate members 11 and 12 is not particularly limited, and examples thereof include a rectangular plate shape and a disk shape. In general, the outer diameter is about 10 to 200 mm and the thickness is about 0.5 to 10 mm. Furthermore, the arithmetic average roughness Ra (conforming to JIS B 0601) of the mating surfaces is 0.1 μm or less, and the maximum height Ry (conforming to JIS B 0601) is 1.0 μm or less. Further, the surface waviness (conforming to JIS B 0601) is 20 μm or less.

  The reaction fluid channel 18 has a shape with a width of 20 to 2000 μm (preferably 500 μm or less, more preferably 100 μm or less) in terms of an equivalent diameter in the channel cross-sectional area. The cross-sectional shape of the reaction fluid channel 18 is not particularly limited, and examples thereof include a semicircular shape, a semielliptical shape, a square shape, a rectangular shape, a trapezoidal shape, a parallelogram shape, a star shape, and an indefinite shape. A concave groove having a semicircular cross section or a semielliptical cross section is formed so as to correspond to each of the first and second substrate-like members 11 and 12, and the cross sectional shape is a circular or elliptical reaction. The fluid flow path 18 may be formed. Further, the shape of the trajectory extending in the length direction of the reaction fluid channel 18 is not particularly limited, although a linear shape is illustrated in FIG. 1. For example, in addition to the linear shape, A circular shape, a meandering shape, a helical shape, etc. can be mentioned. From the viewpoint of reactivity and workability, the cross-sectional shape of the reaction fluid channel 18 is preferably circular, semi-circular, elliptical, semi-elliptical, square, or rectangular, and the locus extending in the length direction of the reaction fluid channel 18. As the shape, a linear shape, a circular shape, or a meandering shape is preferable. The reaction fluid channel 18 does not necessarily have a constant cross-sectional shape along the length direction, and does not necessarily have a regular trajectory formed in the length direction. In addition, the reaction fluid channel 18 may be a single channel or a combined channel or a division channel depending on the purpose of the reaction. Further, the reaction fluid channel 18 may be provided with a catalyst, an adsorbent, or the like.

  The first and second substrate-like members 11 and 12 are merely brought into contact with each other so that they can be disassembled in order to simplify the operation such as maintenance. For this reason, if uneven weight distribution is generated in that portion, local floating can occur, and a leakage flow path from the reaction fluid flow path 18 to the outside of the reactor body 10 is formed, which impairs practical use, and the flow of the reaction fluid. Since the normal reaction operation cannot be performed due to abnormalities in heat transfer, reaction time, etc., careful attention is required during assembly.

  The reactor main body storage container 201 is formed in an internal space in which the reactor main body 10 can be stored and a space region covering the reactor main body 10 is formed, that is, a box having an inner volume larger than the volume of the reactor main body 10. . A space region covering the reactor main body 10 is a sealed fluid storage region 21, and thus the reactor main body storage container 201 constitutes a sealed fluid storage unit. The reactor main body storage container 201 is configured to be openable and closable for the reactor main body 10 to be taken in and out, and in the closed state, the internal sealed fluid storage region 21 is sealed.

  According to the sealing fluid storage portion configured by such a reactor main body storage container 201, the structural isolation between the sealing fluid storage region 21 and the outside air can be reliably performed, which is convenient when controlling the pressure of the sealing fluid. It is. Further, the conventional microreactor itself may be accommodated in a specific container, and can be configured without requiring a new device design.

  The reactor main body container 201 is formed with a pair of through holes through which the coupling pipes 22 detachably connected to the reactor main body are inserted. One of these through-holes is configured as a supply pipe connection 23 and the other as a recovery pipe connection 24.

  The reactor main body storage container 201 is formed with a pair of through holes in the upper and lower sides that communicate with the sealing fluid storage region 21. Of these through-holes, the upper side is configured as a sealing fluid inflow portion 25 and the lower side is configured as a sealing fluid outflow portion 26.

  Examples of the material forming the reactor main body container 201 include the same materials as the material forming the reactor main body 10.

  The shape of the reactor main body container 201 is not particularly limited, and examples thereof include a cubic shape, a rectangular parallelepiped shape, and a cylindrical shape. The container dimensions are not particularly limited as long as the sealed fluid accommodation region 21 is formed.

  A reaction fluid supply pipe 42 extending from the reaction fluid supply source 41 is connected to the supply pipe connection portion 23 of the reactor main body container 201. The reaction fluid supply pipe 42 is provided with a reaction fluid supplier 43 for circulating the reaction fluid, and a reaction fluid pressure gauge 44 for detecting the pressure of the reaction fluid is attached.

  The reaction fluid supply source 41 is, for example, a reaction fluid storage tank that stores the reaction fluid or a micromixer that mixes a plurality of raw material fluids and sends out the reaction fluid.

  The reaction fluid supplier 43 is not particularly limited, and a suitable one is selected depending on the type of reaction fluid. Specifically, when the reaction fluid is a gas, for example, a compressor or a blower is used. When the reaction fluid is a liquid, for example, a liquid feeder is used. For example, a centrifugal pump, diffuser pump, spiral mixed flow pump, mixed flow pump, axial flow pump, gear pump, screw pump, cam pump, vane pump, piston pump, plunger pump, diaphragm pump, vortex pump, viscosity pump , Bubble pumps, jet pumps, electromagnetic pumps and the like. Of these, a type in which no pulsating flow is generated is preferable. The reason is that, when different reaction fluids are mixed in the reactor main body 10, if pulsating flow occurs, not only the performance of uniformly mixing cannot be obtained, but also a reduction in performance is predicted in terms of heat transfer.

  A reaction fluid recovery pipe 51 extends from the recovery pipe connection part 24 of the reactor main body container 201 and is connected to the reaction fluid recovery tank 52. A reaction fluid pressure regulator 53 for adjusting the pressure of the reaction fluid is interposed in the reaction fluid recovery pipe 51. A reaction fluid pressure gauge 44 is electrically connected to the reaction fluid pressure regulator 53. The reaction fluid pressure regulator 53 is configured to be capable of inputting a set pressure and incorporates an arithmetic element, and opens and closes the flow path based on the set pressure information and the pressure information detected by the reaction fluid pressure gauge 44. To do.

  The reaction fluid pressure regulator 53 is, for example, a pressure reducing valve device or a back pressure valve device.

  A sealing fluid supply pipe 62 extending from the sealing fluid storage tank 61 is connected to the sealing fluid inflow portion 25 of the reactor main body container 201. The sealing fluid supply pipe 62 is provided with a sealing fluid supplier 63 for circulating the sealing fluid, and a sealing fluid pressure gauge 64 for detecting the pressure of the sealing fluid is attached.

  The sealing fluid supplier 63 is not particularly limited, and a suitable one is selected depending on the type of the sealing fluid. Specifically, when the sealing fluid is a gas, for example, a compressor or a blower is used. Further, when the sealing fluid is a liquid, for example, a liquid feeder or the like is used. For example, a centrifugal pump, diffuser pump, spiral mixed flow pump, mixed flow pump, axial flow pump, gear pump, screw pump, cam pump, vane pump, piston pump, plunger pump, diaphragm pump, vortex pump, viscosity pump , Bubble pumps, jet pumps, electromagnetic pumps and the like. In addition, when the sealing fluid is either gas or liquid, a pressure tank in which the sealing fluid storage tank 61 and the sealing fluid supplier 63 are integrated may be used.

  A sealed fluid recovery pipe 71 extends from the sealed fluid outflow portion 26 of the reactor main body container 201 and is connected to the sealed fluid recovery tank 72. A sealing fluid pressure regulator 73 that adjusts the pressure of the sealing fluid is interposed in the sealing fluid recovery pipe 71. A sealing fluid pressure gauge 64 is electrically connected to the sealing fluid pressure regulator 73. The sealing fluid pressure regulator 73 is configured to be capable of inputting a set pressure and incorporates an arithmetic element, and the flow path is based on the set pressure information and the pressure information detected by the sealing fluid pressure gauge 64. Open and close.

  The sealing fluid pressure regulator 73 is, for example, a pressure reducing valve device or a back pressure valve device.

  Next, the operation of the microreactor system S will be described.

  When the microreactor system S is operated, the reaction fluid supplier 43 sequentially supplies the reaction fluid from the reaction fluid supply source 41 through the reaction fluid supply pipe 42 to the supply pipe connection portion 23, the coupling tube 22, and the reaction fluid inflow portion 161. Then, it is continuously supplied to the reaction fluid flow path 18 of the reactor body 10. The reaction fluid pressure gauge 44 sends the detected pressure information of the reaction fluid to the reaction fluid pressure regulator 53. Here, the reaction fluid is not particularly limited, and maintains fluidity other than solid phase such as gas phase, liquid phase, gas-liquid mixed phase, emulsified phase, solid-liquid mixed phase (slurry), and supercritical fluid. It may be of any property.

  In the reactor main body 10, the reaction fluid flows in the reaction fluid channel 18 and the reaction proceeds to generate a product reaction fluid. The reaction fluid of the product is sent to the reaction fluid recovery pipe 51 via the reaction fluid outlet 162, the coupling pipe 22, and the recovery pipe connection 24 in order, and then the reaction fluid recovery tank via the reaction fluid pressure regulator 53. 52 is collected. Here, the reaction performed in the reactor body 10 is not particularly limited, and examples thereof include a catalytic reaction, an ion exchange reaction, an electrochemical reaction, a radical reaction, and a supercritical reaction.

  On the other hand, the sealing fluid supplier 63 supplies the sealing fluid from the sealing fluid storage tank 61 via the sealing fluid supply pipe 62 and the sealing fluid inflow portion 25 to the sealing fluid in the reactor main body container 201. Supply to the storage area 21. Further, the sealing fluid pressure gauge 64 sends pressure information of the sealing fluid to the sealing fluid pressure regulator 73. Here, the sealing fluid is not particularly limited, and has properties such as a gas phase, a liquid phase, a gas-liquid mixed phase, an emulsified phase, and a solid-liquid mixed phase (slurry) that maintain fluidity other than the solid phase. Anything is acceptable.

  When the sealing fluid supply unit 63 is continuously operated, the sealing fluid flows through the sealing fluid storage region 21 in the reactor main body storage container 201. The sealing fluid that has circulated through the sealing fluid storage region 21 is sent to the sealing fluid recovery pipe 71 via the sealing fluid outflow portion 26, and the sealing fluid recovery tank via the sealing fluid pressure regulator 73. 72 is collected. Further, when the sealing fluid supply 63 is stopped when the sealing fluid reaches the set pressure of the sealing fluid pressure regulator 73, the sealing fluid does not flow in the reactor main body container 201, and the sealing fluid The housing area 21 is hermetically sealed.

  Through all the above processes, the reaction fluid pressure regulator 53 opens and closes the flow path so that the pressure of the reaction fluid detected by the reaction fluid pressure gauge 44 is maintained at the set pressure. Further, the sealing fluid pressure regulator 73 opens and closes the flow path so that the pressure of the sealing fluid detected by the sealing fluid pressure gauge 64 is maintained at the set pressure. That is, the reaction fluid pressure regulator 53 and the sealing fluid pressure regulator 73 constitute a pressure control unit.

  Next, a method for controlling the microreactor 100 using the microreactor system S will be described.

  As a control method, a method of setting the set pressure of the sealing fluid pressure regulator 73 higher than the set pressure of the reaction fluid pressure regulator 53 and setting the pressure of the sealing fluid higher than the pressure of the reaction fluid, or the reaction fluid There is a method of setting the set pressure of the pressure regulator 53 and the set pressure of the sealing fluid pressure regulator 73 close to each other to reduce the pressure difference between the reaction fluid and the sealing fluid.

  At this time, the first control for maintaining the respective pressures of the reaction fluid and the sealing fluid at the respective set pressures while continuously supplying both the supply of the reaction fluid and the supply of the sealing fluid and circulating them. Even if the method is adopted, the reaction fluid is continuously supplied and circulated, while the sealing fluid is supplied until the pressure reaches the set pressure, and the sealing fluid is sealed at the set pressure without flowing. The second control method may be employed in which the state of hermetically sealing in the fluid containing region 21 is maintained and the pressure of the reaction fluid is maintained at the set pressure.

  In this way, the sealing fluid atmosphere can be formed so as to cover the member mating portion 19 of the reactor main body 10, and the reaction of the reaction fluid flow path 18 from the member mating portion 19 by the sealing fluid atmosphere. Fluid leakage can be regulated. In particular, when the reaction fluid is harmful, it is possible to ensure safety by regulating the leakage of the reaction fluid.

  In addition, according to the first control method, even if a harmful reaction fluid leaks, safety can be ensured by the dilution effect. In addition, when pressure control of the sealing fluid is performed, the pressure operation can be stably performed.

  More specifically, the set pressure of the reaction fluid pressure regulator 53 and the set pressure of the sealing fluid pressure regulator 73 are set so that the pressure difference between the reaction fluid and the sealing fluid is 1.5 MPa or less. It is preferable that the pressure be 0.5 MPa or less. In addition, when the pressure difference between the reaction fluid and the sealing fluid is 1.5 MPa or less, the latter pressure may be set lower than the former pressure. From the viewpoint of ensuring the above, it is preferable to set the latter pressure to be higher than the former pressure.

  Further, the leakage of the reaction fluid from the member mating portion 19 becomes particularly significant when the pressure of the reaction fluid in the reaction fluid channel 18 is set high. Therefore, when the set pressure of the reaction fluid in the reaction fluid channel 18 is set to 5.0 MPa or more or when used in a supercritical state, it is possible to obtain a remarkable effect of restricting the leakage of the reaction fluid.

  Furthermore, in the first control method, the sealing fluid may be circulated and the temperature of the reactor main body 10 may be adjusted using the sealing fluid as a heat medium. In this way, an additional function is given to the sealing fluid in addition to the regulation of leakage of the reaction fluid. In this case, a temperature sensor is attached to the reactor main body 10, a heater is attached to the sealing fluid supply pipe 62, the temperature sensor and the heater are electrically connected to the temperature control unit, and the temperature control unit is a temperature sensor. Based on the detected temperature information of the reactor main body 10, the heater may be ON / OFF controlled to adjust the temperature of the sealing fluid. Here, examples of the sealing fluid suitable for the heat medium include silicon oil, ester oil, water, water vapor, air, chlorofluorocarbon, and alternative chlorofluorocarbon.

  In both the first and second control methods, a reaction inert gas may be used as the sealing fluid. In this way, the sealing fluid can be prevented from contacting and reacting with the sealing fluid, and a dangerous reaction having explosive properties can be carried out in an explosion-proof manner. Can achieve innovative effects. Here, the reaction-inert gas sealing fluid is any of a rare gas such as helium and argon, nitrogen, carbon dioxide, and a mixture thereof.

(Embodiment 2)
2 and 3 show a microreactor system (microdevice system) S according to the second embodiment.

  The microreactor system S includes a microreactor (microdevice) 100 and an incidental part such as a reaction fluid supply system. In addition, the part of the same name as the thing of Embodiment 1 is shown with the same code | symbol.

  The microreactor 100 includes a reactor main body (device main body) 10, a sealing fluid storage unit 202 attached to the outside thereof, and a main body temperature controller 30 attached to the reactor main body 10. Therefore, the microreactor 100 is related to the second configuration described above.

  The reactor main body 10 is of a substrate laminated type, and has first and second substrate-like members (main body forming members) 11 and 12 having the same outer shape that constitute an overlapping structure (combined structure) that can be disassembled vertically. is doing. 2 and 3, the first and second substrate-like members 11 and 12 are formed in a disc shape, but the present invention is not limited to this.

  The first substrate member 11 has a pair of through holes. One of these through holes is configured as a reaction fluid inflow portion 161 and the other is formed as a reaction fluid outflow portion 162. Further, the first substrate member 11 is formed with a concave groove on the lower surface side, that is, the mating surface side with the second substrate member 12 so as to communicate the reaction fluid inflow portion 161 and the reaction fluid outflow portion 162. ing.

  On the other hand, the second substrate member 12 is a flat plate.

  The reactor main body 10 is laminated such that these first and second substrate-like members 11 and 12 are overlapped with each other with their mating surfaces in contact with each other, and clip means such as joint fastening with bolts and nuts, etc. (Not shown) are integrated. And the concave groove of the 1st substrate-like member 11 and the upper surface part of the 2nd substrate-like member 12 corresponding to this are each constituted by channel formation part 17, and the 1st and 2nd substrate-like member 11, The reaction fluid flow paths 18 are formed inside the reactor main body 10 by being combined by overlapping the 12. Further, on the side surface of the reactor main body 10, a linear member matching portion 19 of the first substrate-like member 11 and the second substrate-like member 12 overlapped is formed so as to extend along the outer periphery. The linear member matching portion 19 is exposed outside the reaction fluid flow path 18 inside the reactor main body 10.

  According to the reactor main body 10 configured by superposing the first and second substrate members 11 and 12 as described above, the disassembly maintenance and the assembly work can be easily performed. If the flow path forming portion 17 is formed by making the most of 12, the reaction fluid flow paths 18 having a large number or a long distance can be configured as a whole. The reactor body 10 has the same configuration as that of a conventional substrate-stacked microreactor itself.

  The sealing fluid storage portion 202 is formed in an annular shape that can be externally fitted so as to surround the outer periphery of the reactor main body 10, and is formed in a substantially U-shaped cross section that opens to the inside over the entire periphery. The sealing fluid storage unit 202 is detachably attached to the reactor main body 10 so as to cover the member matching part 19 with an inner opening, and thereby, the sealing that covers the outer periphery of the member matching part 19 over the entire circumference. A fluid containing region 21 is formed. The contact portion between the sealing fluid storage unit 202 and the reactor main body 10 may be subjected to a sealing process such as sandwiching a sealing material so that the sealing fluid storage region 21 is sealed.

  According to such a configuration, it is only necessary to attach the sealing fluid storage portion 202 to the conventional microreactor itself configured by a superposition structure of a plurality of substrate-like members, and thus the apparatus can be easily configured. it can. Further, since the device configuration is compact, the amount of sealing fluid stored in the sealing fluid storage region 21 may be small.

  A pair of through holes are formed in the side surface of the sealing fluid storage unit 202. One of the through holes is configured as a sealing fluid inflow portion 25 and the other is formed as a sealing fluid outflow portion 26.

  Examples of the material forming the sealing fluid storage unit 202 include the same materials as the material forming the reactor body 10.

  A reaction fluid supply pipe 42 extending from the reaction fluid supply source 41 is connected to the reaction fluid inflow portion 161 of the reactor body 10. The reaction fluid supply pipe 42 is provided with a reaction fluid supplier 43 for circulating the reaction fluid, and a reaction fluid pressure gauge 44 for detecting the pressure of the reaction fluid is attached.

  A reaction fluid recovery pipe 51 extends from the reaction fluid outlet 162 of the reactor body 10 and is connected to the reaction fluid recovery tank 52. A reaction fluid pressure regulator 53 for adjusting the pressure of the reaction fluid is interposed in the reaction fluid recovery pipe 51. A reaction fluid pressure gauge 44 is electrically connected to the reaction fluid pressure regulator 53. The reaction fluid pressure regulator 53 is configured to be capable of inputting a set pressure and incorporates an arithmetic element, and opens and closes the flow path based on the set pressure information and the pressure information detected by the reaction fluid pressure gauge 44. To do.

  A sealing fluid supply pipe 62 extending from the sealing fluid storage tank 61 is connected to the sealing fluid inflow portion 25 of the sealing fluid storage portion 202. The sealing fluid supply pipe 62 is provided with a sealing fluid supplier 63 for circulating the sealing fluid, and a sealing fluid pressure gauge 64 for detecting the pressure of the sealing fluid is attached.

  A sealing fluid recovery pipe 71 extends from the sealing fluid outflow portion 26 of the sealing fluid storage portion 202 and is connected to the sealing fluid recovery tank 72. A sealing fluid pressure regulator 73 that adjusts the pressure of the sealing fluid is interposed in the sealing fluid recovery pipe 71. A sealing fluid pressure gauge 64 is electrically connected to the sealing fluid pressure regulator 73. The sealing fluid pressure regulator 73 is configured to be capable of inputting a set pressure and incorporates an arithmetic element. The sealing fluid pressure regulator 73 is configured to flow through the flow path based on the set pressure information and the pressure information detected by the reaction fluid pressure gauge 64. Open and close.

  The main body temperature controller 30 is formed in a plate shape having the same outer shape as the first and second substrate members 11 and 12 of the reactor main body 10 by a heat generating material, and is laminated on the second substrate member 12 on the lower side. It is provided as follows.

  An output controller 32 connected to the power supply unit 31 is electrically connected to the main body temperature controller 30. The output controller 32 is electrically connected to a temperature measuring unit 33 including a temperature sensor 33 a attached to the second substrate member 12. The output controller 32 is configured to be able to input a set temperature and incorporates an arithmetic element, and controls energization to the main body temperature controller 30 based on the set temperature information and the temperature information from the temperature measurement unit 33. To do.

  Next, the operation of the microreactor system S will be described.

  When the microreactor system S operates, the reaction fluid supplier 43 causes the reaction fluid to flow from the reaction fluid supply source 41 through the reaction fluid supply pipe and through the reaction fluid inflow portion 161 to the reaction fluid flow path 18 of the reactor main body 10. To supply continuously. The reaction fluid pressure gauge 44 sends the detected pressure information of the reaction fluid to the reaction fluid pressure regulator 53.

  In the reactor main body 10, the reaction fluid flows in the reaction fluid channel 18 and the reaction proceeds to generate a product reaction fluid. The product reaction fluid is sent to the reaction fluid recovery pipe 51 via the reaction fluid outlet 162 and is recovered to the reaction fluid recovery tank 52 via the reaction fluid pressure regulator 53.

  On the other hand, the sealing fluid supplier 63 seals the sealing fluid from the sealing fluid storage tank 61 via the sealing fluid supply pipe 62 and the sealing fluid inflow portion 25 to seal the sealing fluid storage portion 202. The fluid is supplied to the fluid containing area 21. Further, the sealing fluid pressure gauge 64 sends pressure information of the sealing fluid to the sealing fluid pressure regulator 73.

  When the sealing fluid supplier 63 is continuously operated, the sealing fluid flows through the sealing fluid storage region 21 in the sealing fluid storage unit 202. The sealing fluid that has circulated through the sealing fluid storage region 21 is sent to the sealing fluid recovery pipe 71 via the sealing fluid outflow portion 26, and the sealing fluid recovery tank via the sealing fluid pressure regulator 73. 72 is collected. Further, when the sealing fluid supply unit 63 is stopped when the sealing fluid reaches the set pressure of the sealing fluid pressure regulator 73, the sealing fluid is not circulated in the sealing fluid storage unit 202. The fluid containing region 21 is hermetically sealed.

  Through all the above processes, the reaction fluid pressure regulator 53 opens and closes the flow path so that the pressure of the reaction fluid detected by the reaction fluid pressure gauge 44 is maintained at the set pressure. Further, the sealing fluid pressure regulator 73 opens and closes the flow path so that the pressure of the sealing fluid detected by the sealing fluid pressure gauge 64 is maintained at the set pressure. That is, the reaction fluid pressure regulator 53 and the sealing fluid pressure regulator 73 constitute a pressure control unit.

  Regarding temperature control of the reactor main body 10, the temperature measurement unit 33 detects the temperature of the reactor main body 10 with the temperature sensor 33 a and sends the temperature information to the output controller 32. The output controller 32 performs ON / OFF control of energization to the main body temperature controller 30 so that the temperature of the reactor main body 10 is maintained at the set temperature.

  The detailed configuration, control method, and operational effects of the reactor body 10 and the like are the same as those in the first embodiment.

  FIG. 4 shows a modification of the microreactor system S according to the second embodiment. In addition, the part of the same name as the thing of Embodiment 1 is shown with the same code | symbol.

  In the microreactor 100 of the microreactor system S, only the sealing fluid inflow portion 25 is formed on the side surface of the sealing fluid storage portion 202.

  A sealing fluid supply pipe 62 extending from the sealing fluid storage tank 61 is connected to the sealing fluid inflow portion 25 of the sealing fluid storage portion 202. The sealing fluid supply pipe 62 is provided with a sealing fluid pressure regulator 73 and a sealing fluid supplier 63 in order from the upstream side, and a sealing fluid pressure gauge 64 is attached. A sealing fluid pressure gauge 64 is electrically connected to the sealing fluid pressure regulator 73.

  The sealing fluid supplier 63 passes the sealing fluid from the sealing fluid storage tank 61 through the sealing fluid supply pipe 62 and sequentially passes through the sealing fluid pressure regulator 73 and the sealing fluid inflow portion 25. It supplies to the sealing fluid accommodation area | region 21 of the sealing fluid accommodating part 202. FIG. Further, the sealing fluid pressure gauge 64 sends pressure information of the sealing fluid to the sealing fluid pressure regulator 73. When the sealing fluid reaches the set pressure of the sealing fluid pressure regulator 73, the sealing fluid pressure regulator 73 closes the flow path, and the sealing fluid does not circulate in the sealing fluid storage unit 202. The housing area 21 is hermetically sealed. That is, in the microreactor system S of this modified example, only the second control method can be performed.

  Other configurations, operations, and the like are the same as those of the microreactor system S according to the second embodiment.

(Embodiment 3)
5 and 6 show a microreactor system (microdevice system) S according to the third embodiment.

  The microreactor system S includes a microreactor (microdevice) 100 and an incidental part such as a reaction fluid supply system. In addition, the part of the same name as the thing of Embodiment 1 is shown with the same code | symbol.

  The microreactor 100 is composed of only the reactor main body (device main body) 10. The microreactor 100 has the second configuration described above.

  The reactor main body 10 is of a substrate laminated type, and has first and second substrate-like members (main body forming members) 11 and 12 having the same outer shape that constitute an overlapping structure (combined structure) that can be disassembled vertically. is doing. 5 and 6, the first and second substrate-like members 11 and 12 are formed in an elongated rectangular shape, but the present invention is not limited to this.

  The first substrate member 11 has a pair of through holes. One of these through holes is configured as a reaction fluid inflow portion 161 and the other is formed as a reaction fluid outflow portion 162. The first substrate member 11 is formed with a concave groove on the lower surface side, that is, the mating surface side with the second substrate member 12 so as to communicate the reaction fluid inflow portion 161 and the reaction fluid outflow portion 162. .

  An annular groove 27 is formed in the second substrate member 12 on the upper surface side, that is, on the mating surface side with the first substrate member 11 so as to surround the flow path forming portion 17. The second substrate-like member 12 is formed with a pair of through holes that penetrate the annular groove 27 from the lower surface side. One of the through holes is configured as a sealing fluid inflow portion 25 and the other is formed as a sealing fluid outflow portion 26.

  The reactor main body 10 is laminated such that the first and second substrate-like members 11 and 12 are overlapped with each other with their mating surfaces in contact with each other, and clip means such as joint fastening with bolts and nuts. (Not shown) are integrated. And the concave groove of the 1st substrate-like member 11 and the upper surface part of the 2nd substrate-like member 12 corresponding to this are each constituted by channel formation part 17, and the 1st and 2nd substrate-like member 11, The reaction fluid flow paths 18 are formed inside the reactor main body 10 by being combined by overlapping the 12.

  According to the reactor main body 10 configured by superposing the first and second substrate members 11 and 12 as described above, the disassembly maintenance and the assembly work can be easily performed. If the flow path forming portion 17 is formed by making the most of 12, the reaction fluid flow paths 18 having a large number or a long distance can be configured as a whole. The reactor body 10 has the same configuration as that of a conventional substrate-stacked microreactor itself.

  Further, the annular groove 27 of the second substrate member 12 and the corresponding lower surface portion of the first substrate member 11 are combined by overlapping the first and second substrate members 11, 12, The inner side edge of the annular groove 27 is in contact with the lower surface of the first substrate member 11 to form a linear member matching portion 19, and the sealing fluid containing region 21 is formed so as to cover the member matching portion 19. Forming. That is, the second substrate-like member 12 also constitutes a sealing fluid storage part. The linear member matching portion 19 is exposed outside the reaction fluid flow path 18 inside the reactor main body 10.

  According to such a configuration, it is only necessary to process the conventional microreactor itself configured by a superposed structure of a plurality of substrate-like members to form the sealing fluid storage portion 202, thereby facilitating the apparatus. Can be configured. Further, since the device configuration is compact, the amount of sealing fluid stored in the sealing fluid storage region 21 may be small.

  A reaction fluid supply pipe 42 extending from the reaction fluid supply source 41 is connected to the reaction fluid inflow portion 161 of the first substrate member 11 of the reactor body 10. The reaction fluid supply pipe 42 is provided with a reaction fluid supplier 43 for circulating the reaction fluid, and a reaction fluid pressure gauge 44 for detecting the pressure of the reaction fluid is attached.

  A reaction fluid recovery pipe 51 extends from the reaction fluid outflow portion 162 of the first substrate member 11 of the reactor body 10 and is connected to the reaction fluid recovery tank 52. A reaction fluid pressure regulator 53 for adjusting the pressure of the reaction fluid is interposed in the reaction fluid recovery pipe 51. A reaction fluid pressure gauge 44 is electrically connected to the reaction fluid pressure regulator 53. The reaction fluid pressure regulator 53 is configured to be capable of inputting a set pressure and incorporates an arithmetic element, and opens and closes the flow path based on the set pressure information and the pressure information detected by the reaction fluid pressure gauge 44. To do.

  A sealing fluid supply pipe 62 extending from the sealing fluid storage tank 61 is connected to the sealing fluid inflow portion 25 of the second substrate member 12 of the reactor body 10. The sealing fluid supply pipe 62 is provided with a sealing fluid supplier 63 for circulating the sealing fluid, and a sealing fluid pressure gauge 64 for detecting the pressure of the sealing fluid is attached.

  A sealed fluid recovery pipe 71 extends from the sealed fluid outflow portion 26 of the second substrate member 12 of the reactor body 10 and is connected to the sealed fluid recovery tank 72. A sealing fluid pressure regulator 73 that adjusts the pressure of the sealing fluid is interposed in the sealing fluid recovery pipe 71. A sealing fluid pressure gauge 64 is electrically connected to the sealing fluid pressure regulator 73. The sealing fluid pressure regulator 73 is configured to be capable of inputting a set pressure and incorporates an arithmetic element, and the flow path is based on the set pressure information and the pressure information detected by the sealing fluid pressure gauge 64. Open and close.

  Next, the operation of the microreactor system S will be described.

  When the microreactor system S is operated, the reaction fluid supplier 43 causes the reaction fluid to flow from the reaction fluid supply source 41 through the reaction fluid supply pipe and through the reaction fluid inflow portion 161 to the reaction fluid flow path 18 of the reactor body 10. To supply continuously. The reaction fluid pressure gauge 44 sends the detected pressure information of the reaction fluid to the reaction fluid pressure regulator 53.

  In the reactor main body 10, the reaction fluid flows in the reaction fluid channel 18 and the reaction proceeds to generate a product reaction fluid. The product reaction fluid is sent to the reaction fluid recovery pipe 51 via the reaction fluid outlet 162 and is recovered to the reaction fluid recovery tank 52 via the reaction fluid pressure regulator 53.

  On the other hand, the sealing fluid supply unit 63 supplies the sealing fluid from the sealing fluid storage tank 61 via the sealing fluid supply pipe 62 and the sealing fluid inflow portion 25 to the sealing fluid accommodation region of the reactor body 10. 21. Further, the sealing fluid pressure gauge 64 sends pressure information of the sealing fluid to the sealing fluid pressure regulator 73.

  When the sealing fluid supplier 63 is continuously operated, the sealing fluid flows in the sealing fluid accommodation region 21 in the reactor main body 10. The sealing fluid that has circulated through the sealing fluid storage region 21 is sent to the sealing fluid recovery pipe 71 via the sealing fluid outflow portion 26, and the sealing fluid recovery tank via the sealing fluid pressure regulator 73. 72 is collected. Further, when the sealing fluid supply 63 is stopped when the sealing fluid reaches the set pressure of the sealing fluid pressure regulator 73, the sealing fluid is not circulated in the reactor main body 10, and the sealing fluid accommodation region 21 is hermetically sealed.

  Through all the above processes, the reaction fluid pressure regulator 53 opens and closes the flow path so that the pressure of the reaction fluid detected by the reaction fluid pressure gauge 44 is maintained at the set pressure. Further, the sealing fluid pressure regulator 73 opens and closes the flow path so that the pressure of the sealing fluid detected by the sealing fluid pressure gauge 64 is maintained at the set pressure. That is, the reaction fluid pressure regulator 53 and the sealing fluid pressure regulator 73 constitute a pressure control unit.

  The detailed configuration, control method, and operational effects of the reactor body 10 and the like are the same as those in the first embodiment.

(Embodiment 4)
FIG. 7 shows a microreactor system (microdevice system) S according to the fourth embodiment.

  The microreactor system S includes a microreactor (microdevice) 100 and an incidental part such as a reaction fluid supply system. In addition, the part of the same name as the thing of Embodiment 1 is shown with the same code | symbol.

  The microreactor 100 includes a reactor main body (device main body) 10 and a reactor main body accommodating portion 204 that accommodates it. Therefore, the microreactor 100 is related to the second configuration described above.

  The reactor main body 10 is a substrate stack type, and has first to fifth substrate-like members (main body forming members) 11 to 15 having the same outer shape that constitute an overlapping structure (combined structure) that can be disassembled vertically. is doing.

  A through-hole is formed in the first substrate member 11. The through hole is formed in the reaction fluid inflow portion 161.

  A through hole is formed in the second substrate member 12, and the through hole and the through hole of the first substrate member 11 are formed on the upper surface side, that is, on the mating surface side with the first substrate member 11. A groove is formed so as to communicate with each other.

  Similarly to the second substrate member 12, each of the third to fifth substrate members 13, 14, and 15 is formed with a through hole and a concave groove. Further, a through hole of the fifth substrate member 15 is formed in the reaction fluid outflow portion 162.

  The reactor main body 10 includes these first to fifth substrate-like members 11 to 15 which are stacked in such a manner that the mating surfaces are in contact with each other and are stacked one on top of the other in order, and clip means such as fastening with bolts and nuts (non-fixed). It is the structure integrated by (illustration). And the concave groove of the 2nd substrate-like member 12 and the lower surface part of the 1st substrate-like member 11 corresponding to this are each constituted by channel formation part 17, and the 1st and 2nd substrate-like member 11, The reaction fluid flow paths 18 are formed by being combined by overlapping 12. Similarly, in each of the third to fifth substrate members 13, 14, 15, the concave groove and the lower surface portion of the upper substrate member corresponding thereto form the reaction fluid flow path 18. As a result, a reaction fluid flow path 18 is formed in the reactor body 10 so as to communicate vertically from the reaction fluid inflow portion 161 of the first substrate member 11 to the reaction fluid outflow portion 162 of the fifth substrate member 15. Yes. Further, on the side surface of the reactor main body 10, four linear member alignment portions 19 extending in parallel with each other are formed so as to extend along the outer periphery by the superimposed first to fifth substrate-like members 11 to 15. Has been. These linear member matching portions 19 are exposed outside the reaction fluid flow path 18 inside the reactor main body 10.

  According to the reactor main body 10 configured by superimposing such first to fifth substrate-like members 11 to 15, disassembly maintenance and assembling work can be easily performed, and each substrate-like member 11 to 11 can be performed. If the flow path forming portion 17 is formed by making the most of 15, the reaction fluid flow paths 18 having a large number or a long distance can be configured as a whole. The reactor body 10 has the same configuration as the conventional substrate stacked microreactor itself.

  The reactor main body accommodating portion 204 is formed with a main body accommodating recess opened on the upper surface side for accommodating the reactor main body 10. The main body accommodating recess is formed so that the inner diameter of the open end portion is fitted to the upper portion of the first substrate-like member 11 of the reactor main body 10, and the inner diameter of the bottom portion is that of the fifth substrate-like member 15. The lower part is formed to fit. The main body accommodating recess is formed such that the inner diameter of the intermediate portion corresponding to the lower part of the first substrate-like part to the upper part of the fifth substrate-like part is larger than the outer diameter of the reactor main body 10. Then, the reactor main body 10 is accommodated in the reactor main body accommodating portion 204, so that the sealed fluid accommodating region 21 covering the four linear member mating portions 19 on the outer periphery of the intermediate portion of the reactor main body 10 therebetween. Is to be formed. That is, the reactor main body storage unit 204 constitutes a sealed fluid storage unit. Note that the contact portion between the open end portion of the reactor main body accommodating portion 204 and the reactor main body 10 may be subjected to a sealing process such as sandwiching a sealing material so that the sealing fluid accommodating region 21 is sealed. Good.

  According to such a configuration, it is only necessary to combine the reactor main body storage unit 204 with a conventional microreactor itself configured by a superposition structure of a plurality of substrate-like members, and thus the apparatus can be easily configured. it can. Further, since the device configuration is compact, the amount of sealing fluid stored in the sealing fluid storage region 21 may be small.

  In the reactor main body accommodating portion 204, a pair of upper and lower through holes reaching the main body accommodating recess from the side surface are formed at a plurality of locations. Of these through-holes, the upper side is configured as a sealing fluid inflow portion 25 and the lower side is configured as a sealing fluid outflow portion 26. The reactor main body accommodating portion 204 is formed with a connection channel 28 penetrating from the main body accommodating concave portion to the bottom surface corresponding to the reaction fluid outflow portion 162 of the fifth substrate member 15 of the reactor main body 10.

  Examples of the material for forming the reactor main body accommodating portion 204 include the same materials as those for forming the reactor main body 10.

  A reaction fluid supply pipe 42 extending from the reaction fluid supply source 41 is connected to the reaction fluid inflow portion 161 of the first substrate member 11 of the reactor body 10. The reaction fluid supply pipe 42 is provided with a reaction fluid supplier 43 for circulating the reaction fluid, and a reaction fluid pressure gauge 44 for detecting the pressure of the reaction fluid is attached.

  A reaction fluid recovery pipe 51 extends from the reaction fluid outflow portion 162 of the first substrate-like member 11 of the reactor body 10 via the connection flow path 28 and is connected to the reaction fluid recovery tank 52. A reaction fluid pressure regulator 53 for adjusting the pressure of the reaction fluid is interposed in the reaction fluid recovery pipe 51. A reaction fluid pressure gauge 44 is electrically connected to the reaction fluid pressure regulator 53. The reaction fluid pressure regulator 53 is configured to be capable of inputting a set pressure and incorporates an arithmetic element, and opens and closes the flow path based on the set pressure information and the pressure information detected by the reaction fluid pressure gauge 44. To do.

  A sealing fluid supply pipe 62 extending from the sealing fluid storage tank 61 is connected to each sealing fluid inflow portion 25 of the reactor main body accommodating portion 204. The sealing fluid supply pipe 62 is provided with a sealing fluid supplier 63 for circulating the sealing fluid, and a sealing fluid pressure gauge 64 for detecting the pressure of the sealing fluid is attached.

  A sealed fluid recovery pipe 71 extends from each sealed fluid outflow portion 26 of the reactor main body accommodating portion 204 and is connected to the sealed fluid recovery tank 72. A sealing fluid pressure regulator 73 that adjusts the pressure of the sealing fluid is interposed in the sealing fluid recovery pipe 71. A sealing fluid pressure gauge 64 is electrically connected to the sealing fluid pressure regulator 73. The sealing fluid pressure regulator 73 is configured to be capable of inputting a set pressure and incorporates an arithmetic element, and the flow path is based on the set pressure information and the pressure information detected by the sealing fluid pressure gauge 64. Open and close.

  Next, the operation of the microreactor system S will be described.

  When the microreactor system S is operated, the reaction fluid supplier 43 causes the reaction fluid to flow from the reaction fluid supply source 41 through the reaction fluid supply pipe and through the reaction fluid inflow portion 161 to the reaction fluid flow path 18 of the reactor body 10. To supply continuously. The reaction fluid pressure gauge 44 sends the detected pressure information of the reaction fluid to the reaction fluid pressure regulator 53.

  In the reactor main body 10, the reaction fluid flows in the reaction fluid channel 18 and the reaction proceeds to generate a product reaction fluid. The product reaction fluid is sent to the reaction fluid recovery pipe 51 via the reaction fluid outlet 162 and the connection flow path 28 in order, and is recovered to the reaction fluid recovery tank 52 via the reaction fluid pressure regulator 53. .

  On the other hand, the sealing fluid supplier 63 seals the sealing fluid from the sealing fluid storage tank 61 via the sealing fluid supply pipe 62 and the sealing fluid inflow portion 25 to seal the sealing fluid storage portion 202. The fluid is supplied to the fluid containing area 21. Further, the sealing fluid pressure gauge 64 sends pressure information of the sealing fluid to the sealing fluid pressure regulator 73.

  When the sealing fluid supplier 63 is continuously operated, the sealing fluid flows through the sealing fluid storage region 21 in the reactor main body storage unit 204. The sealing fluid that has circulated through the sealing fluid storage region 21 is sent to the sealing fluid recovery pipe 71 via the sealing fluid outflow portion 26, and the sealing fluid recovery tank via the sealing fluid pressure regulator 73. 72 is collected. Further, when the sealing fluid supply 63 is stopped when the sealing fluid reaches the set pressure of the sealing fluid pressure regulator 73, the sealing fluid is not circulated in the reactor main body accommodating portion 204. The housing area 21 is hermetically sealed.

  Through all the above processes, the reaction fluid pressure regulator 53 opens and closes the flow path so that the pressure of the reaction fluid detected by the reaction fluid pressure gauge 44 is maintained at the set pressure. Further, the sealing fluid pressure regulator 73 opens and closes the flow path so that the pressure of the sealing fluid detected by the sealing fluid pressure gauge 64 is maintained at the set pressure. That is, the reaction fluid pressure regulator 53 and the sealing fluid pressure regulator 73 constitute a pressure control unit.

  The detailed configuration, control method, and operational effects of the reactor body 10 and the like are the same as those in the first embodiment.

(Other embodiments)
In the first to fourth embodiments, the microreactor 100 is used. However, the microreactor 100 is not particularly limited thereto, and other microdevices such as a micromixer may be used.

  In the first to fourth embodiments, the sealing fluid is circulated from the sealing fluid storage tank 61 to the sealing fluid recovery tank 72. However, the present invention is not limited to this, and the sealing fluid circulation flow is not limited thereto. It is good also as a structure which circulates sealing fluid to a path.

  Moreover, in the said Embodiment 1-4, although the pressure control part was comprised by the reaction fluid pressure regulator 53 and the sealing fluid pressure regulator 73, it is not limited to this in particular, A single reactor control part is used. A pressure control unit may be configured to control the pressure of the reaction fluid and / or the pressure of the sealing fluid.

  Moreover, in the said Embodiment 1-4, although it is the structure which can distribute | circulate sealing fluid to the sealing fluid accommodation area | region 21, and can also seal sealing fluid in the sealing fluid accommodation area | region 21, it is the said implementation. As in the modification of the second embodiment, the first, third, and fourth embodiments may be configured such that only the sealing fluid inflow portion 25 is provided and only the latter can be performed.

(Configuration of test equipment)
The microdevice used for the test is of a type in which the device body is housed in a device body housing container.

  The device body is composed of a pair of circular substrate-like members, one of which is formed with a groove as a flow path forming part having a width of 1 mm, a depth of 0.5 mm, and a length of 1 m, and the other one of A pair of through holes constituting the fluid inflow portion and the fluid outflow portion are formed so as to correspond to both ends of the concave groove of the circular substrate member. The device body is configured by superposing these pair of circular substrate members, passing the bolts through the eight bolt insertion holes formed in the center and outer periphery, and tightening the nuts with a tightening strength of 0.5 N · m. did.

  The device main body container is a pressure-holding container having a volume of 600 ml in which a through hole forming a sealing fluid inflow portion is formed.

  The micro device extends from the ion exchange water storage tank and is connected to the fluid inflow portion of the device body through a metal pipe with a plunger pump and a pressure gauge interposed therein and connected to the fluid inflow portion of the device body. A metal pipe with a pressure regulator interposed is drawn into the device body container and connected to the fluid outflow part of the device body, and further extends from the nitrogen gas tank and is provided with a pressure sensor and a pressure regulator. Is connected to the sealing fluid inflow portion of the device main body container.

(Test method)
The water tests of the following tests 1 to 6 were performed, and the liquid leakage rate was calculated from the balance of the liquid feeding amount and the recovered liquid amount for each. Further, the presence or absence of liquid leakage was confirmed by observation of the appearance of the device body.

-Test 1
A nitrogen gas atmosphere of 1.4 MPa was set in the device main body container, and 0.0 MPa ion exchange water was passed through the fluid flow path of the device main body at a flow rate of 0.1 mL / min for 12 hours. Here, the pressure in the device main body container and the pressure of the ion exchange water are both gauge pressures (hereinafter the same).

-Test 2-
The inside of the device main body container was a 1.4 MPa nitrogen gas atmosphere, and 1.0 MPa ion exchange water was passed through the fluid flow path of the device main body at a flow rate of 0.1 mL / min for 12 hours.

-Test 3-
The inside of the device main body container was a 1.4 MPa nitrogen gas atmosphere, and 1.5 MPa ion exchange water was passed through the fluid flow path of the device main body at a flow rate of 0.1 mL / min for 12 hours.

-Test 4-
The inside of the device main body container was set to 0.0 MPa, and 0.0 MPa ion exchange water was passed through the fluid flow path of the device main body at a flow rate of 0.1 mL / min for 12 hours.

-Test 5-
The inside of the device main body container was set to 0.0 MPa, and 1.5 MPa ion exchange water was passed through the fluid flow path of the device main body at a flow rate of 0.1 mL / min for 12 hours.

-Test 6
The inside of the device main body container was set to 0.0 MPa, and 3.0 MPa ion exchange water was passed through the fluid flow path of the device main body at a flow rate of 0.1 mL / min for 12 hours.

-Test 7-
The inside of the device main body container was set to 0.0 MPa, and 5.0 MPa ion exchange water was passed through the fluid flow path of the device main body at a flow rate of 0.1 mL / min for 12 hours.

-Reference test-
The inside of the device main body container was set to 0.0 MPa, and 9.0 MPa ion exchange water was passed through the fluid flow path of the device main body at a flow rate of 0.1 mL / min. However, the fluid leakage rate of 5.3% was confirmed in the intermediate course 2 hours after the start of water flow, so the test was stopped.

(Test results)
The test results are shown in Table 1.

  According to Table 1, in tests 1 and 2 where the pressure of the sealing fluid (nitrogen gas) is higher than the pressure of the circulating fluid (ion exchange water), the fluid leakage rate is 0.0%, and the appearance Observation shows that no liquid leakage was confirmed, that is, no liquid leakage occurred. This is considered to be because the circulating fluid did not resist the sealing fluid with higher pressure and was sealed in the device body.

  In Test 4 in which there is no pressure difference between the sealing fluid and the circulating fluid, the fluid leakage rate is 0.2%, and it is understood that liquid leakage is not confirmed by external observation, that is, the liquid leakage is extremely small. This means that if at least the sealing fluid and the circulating fluid have the same pressure, liquid leakage can be suppressed to a very low level.

  In Tests 3, 5 and 6 where the pressure of the sealing fluid is lower than the pressure of the circulating fluid, the fluid leakage rate is 0.8 to 1.0%, and liquid appearance is confirmed by appearance observation. Obviously, liquid leakage occurred. This is considered to be because the circulating fluid leaked outside the device body against the sealing fluid having a lower pressure. However, this level of liquid leakage is sufficiently acceptable for practical use in comparison with Test 7 in which the pressure of ion-exchanged water, which is a circulating fluid, is 5.0 MPa, and a reference test in which 9.0 MPa is used. . Therefore, even if the pressure of the sealing fluid is lower than the pressure of the circulating fluid, if the pressure difference is 3.0 MPa or less and 1.5 MPa or less in consideration of safety, the leakage of the circulating fluid Is considered to be sufficiently low.

  As described above, the present invention includes a plurality of main body forming members each having a flow path forming portion formed therein, and constitutes a combination structure in which the plurality of main body forming members can be disassembled. It is useful for a microdevice including a device body in which a flow path forming portion of a plurality of main body forming members is combined to form a fluid flow path therein and a control method thereof.

1 is a diagram illustrating a configuration of a microreactor system according to a first embodiment. It is a figure which shows the structure of the microreactor system which concerns on Embodiment 2. FIG. 6 is a top view of the microreactor of Embodiment 2. FIG. It is a figure which shows the structure of the modification of the microreactor system which concerns on Embodiment 2. FIG. It is a figure which shows the structure of the microreactor system which concerns on Embodiment 3. FIG. It is a top view of the microreactor of Embodiment 3. It is a figure which shows the structure of the microreactor system which concerns on Embodiment 4. FIG.

Explanation of symbols

100 microreactor (microdevice)
10 Reactor body (device body)
11-15 First to fifth substrate-like members (main body forming members)
17 channel formation part 18 reaction fluid channel 19 member matching part 201 reactor main body container (sealing fluid container, device main body container)
202 Sealing fluid container 204 Reactor body container (sealing fluid container)
21 Sealing fluid storage area

Claims (12)

The plurality of main body forming members each having a flow path forming portion are formed, and the plurality of main body forming members constitute a combination structure that can be disassembled by an overlapping structure of a plurality of substrate-like members. A device main body in which a fluid flow path is formed by combining the flow path forming portions of the main body forming member;
Covering a linear member joining portion formed by surrounding at least a pair of the plurality of body forming members formed so as to surround the outer periphery of the device body and exposed outside the fluid flow path inside the device body. A sealing fluid storage portion forming a sealing fluid storage region;
With micro device. The microdevice according to claim 1, wherein a material of the device body is a metal material and / or a ceramic material having a Vickers hardness of 80 HV or more. 2. The microdevice according to claim 1, wherein the arithmetic average roughness Ra of the overlapping surface of the substrate-like member is 0.1 μm or less and the maximum height Ry is 1.0 μm or less. The microdevice according to claim 1, wherein the surface waviness of the overlapping surface of the substrate-like member is 20 μm or less.   The microdevice according to claim 1, wherein the fluid flow path inside the device body has an equivalent diameter of 2000 μm or less of a cross section of the flow path. The plurality of main body forming members each having a flow path forming portion are formed, and the plurality of main body forming members constitute a combination structure that can be disassembled by an overlapping structure of a plurality of substrate-like members. A control method of a microdevice including a device body in which a fluid flow path is formed by combining the flow path forming portions of the main body forming member,
A linear member joining portion formed by at least one pair of the plurality of body forming members exposed outside the fluid flow path inside the device body is formed so as to surround the outer periphery of the device body. A method for controlling a microdevice, wherein a sealing fluid atmosphere that restricts leakage of a circulating fluid in the fluid flow path from the member mating portion is formed by covering with a sealing fluid storage portion .   The method for controlling a microdevice according to claim 6, wherein the pressure of the sealing fluid in the sealing fluid atmosphere is made higher than the pressure of the circulating fluid in the fluid flow path.   The method for controlling a micro device according to claim 6, wherein a pressure difference between the circulating fluid in the fluid flow path and the sealing fluid in the sealing fluid atmosphere is 1.5 MPa or less.   The method for controlling a micro device according to claim 6, wherein the pressure of the circulating fluid in the fluid flow path is set to 5.0 MPa or more.   The method for controlling a micro device according to claim 6, wherein the sealing fluid in the sealing fluid atmosphere is circulated.   The method for controlling a micro device according to claim 10, wherein the temperature of the device body is adjusted using the sealing fluid as a heat medium.   The method for controlling a micro device according to claim 6, wherein the sealing fluid in the sealing fluid atmosphere is a reaction inert gas.

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