JP2007098237A - Manufacturing apparatus for substance and chemical reactor equipped with it - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To detect a leakage of fluids from the passage early and reliably in a micro-reactor. <P>SOLUTION: The chemical reactor 100 has a pump 108 capable of feeding the first solution 101 and the second solution 102 and a micro-reactor having a passage 103 mixing the first and second solutions to allow them to react. The rates of feeding the first and second solutions to the micro-reactor are controlled by a pump controller 113. The micro-reactor has the first base plate formed with the passage and the second base plate joined air-tightly to the first base plate. A leakage detection passage 105 is formed in the vicinity of the passage 103 formed in the first base plate. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a microreactor which is a substance manufacturing apparatus, and more particularly to a chemical reaction apparatus provided with a microreactor capable of detecting fluid leakage from a flow path.

  An example of a conventional apparatus for detecting fluid leakage is described in Patent Document 1. In the detection device described in this publication, in order to monitor the fluid in the pipe without directly contacting the fluid, a measurement pipe that is a part of the dielectric load of the measurement device is provided, and the fluctuation of the dielectric load in the measurement pipe section is detected. ing. At that time, the vibration frequency is measured using a resonance type electromagnetic sensing device, and the composition including the fluid pressure and the presence of air and other gases in the fluid is determined from the change in the measured frequency.

  Another method for detecting fluid leakage is described in US Pat. In the leak determination device described in this publication, the area obtained from the frequency spectrum of the acoustic signal received by the sensor is larger than the area obtained from a predetermined function so that a fluid leak can be determined even in the presence of noise. If the amount increases by a certain amount, it is determined that there is a leak. Further, Patent Document 3 describes that a microreactor is installed in a high-pressure vessel in order to prevent pressure leakage from the microreactor.

Japanese Patent Laid-Open No. 6-236696 Japanese Patent Laid-Open No. 9-43087 JP 2004-53545 A

  The devices described in Patent Documents 1 and 2 do not consider application to a microreactor, which is a small device, and thus there is a problem that the device becomes large when applied to a microreactor. In addition, in the microreactor flow path, the liquid and the reactants directly contact with each other in the minute flow path to cause a chemical reaction. Therefore, when an electromagnetic wave, ultrasonic wave, infrared light, ultraviolet light, or the like is applied, a reaction other than a predetermined reaction occurs. May occur, adversely affecting the reaction process and products.

  Further, even if the dielectric reaction described in Patent Document 1 is to be used, the fluid and the reactant in the microreactor do not necessarily have significant dielectric properties, and it may be assumed that they do not exhibit dielectric properties. Further, in the case where the entire microreactor is accommodated in a thermostat for temperature control, the thermostatic layer becomes a shield even when the leak determination method described in Patent Document 2 is used, and the leak sound of fluid leaking from the microreactor Is difficult to detect.

  The microreactor described in Patent Document 3 is effective in the case of a reaction under high pressure, but does not necessarily cause all reactions to occur under high pressure. Inevitably becomes a pressure vessel, and the apparatus becomes larger. Note that when the reaction system is micronized using a microreactor, properties different from the bulk may be exhibited. For example, even if it has corrosion resistance in the bulk, it may lose corrosion resistance in a micronized state. When such a material is used for a microreactor, it is difficult to detect corrosion that may occur inside the flow channel from outside the microreactor.

  The present invention has been made in view of the above problems of the prior art, and an object thereof is to detect leakage of fluid from a microreactor with a simple configuration. Another object of the present invention is to detect fluid leakage without changing the configuration of the reaction channel of the microreactor.

  A feature of the present invention that achieves the above object is that a first substrate having a flow path for mixing and circulating the first and second solutions, and a second substrate hermetically attached to the first substrate. In a manufacturing apparatus for a substance having a substrate, in the vicinity of a flow path formed on the first substrate, leakage detection for detecting leakage of the first and second solutions or their reaction product solutions from the flow path This is because a flow path is formed.

  In this feature, the flow path may be formed in a meandering shape, and the leakage detection flow path may be formed of a plurality of flow paths in which branch portions extend between the meandering flow paths. The leakage detection channel may be formed from two serpentine channels sandwiching the serpentine channel. Furthermore, it has pressure detection means for detecting the pressure of the leakage detection flow path, and a pressure adjustment device for comparing the pressure with a predetermined value to determine the leakage of the solution. It is desirable to be able to maintain the path at negative pressure.

  In the above feature, a fluid may be enclosed in the leakage detection flow path, and a detection unit that detects at least one of a gas component, spatial thermal conductivity, and electrical conductivity of the fluid in the leakage detection flow path may be provided, Means capable of maintaining the leakage detection flow path at a negative pressure may be provided.

  Another feature of the present invention that achieves the above object is that the chemical reaction apparatus is capable of feeding the first and second solutions, and the amount of the first and second solutions fed by the pump. And a microreactor in which first and second solutions are supplied and a channel for mixing and reacting the first and second solutions is formed. The microreactor has the channel formed therein. A leakage detection flow path including a first substrate formed and a second substrate airtightly coupled to the first substrate, wherein a gas is sealed at a negative pressure in the vicinity of the flow path formed in the first substrate. The pressure detection means for detecting the pressure of the leakage detection flow path and the pressure detected by the pressure detection means are compared with a predetermined value, and leakage of the first and second solutions or their mixed reaction product solution is detected. And a pressure adjusting device for determination.

  According to the present invention, since the leakage detection flow path is provided in the vicinity of the flow path through which the reactant solution circulates, the leakage of the fluid from the flow path can be detected early and reliably with a simple configuration. .

  In the present invention, the microreactor 106 used in the chemical reaction apparatus 100 is provided with a working fluid channel 103 for detecting the state of the working fluid fine channel 103 of the microreactor 106 and the working fluid channel 103. Different monitoring flow paths 105 are formed. Then, the leakage of the fluid from the working fluid channel 103 is detected in a non-contact manner in the working fluid channel 103 by monitoring the monitoring channel 105.

  This specific leak detection system will be described below with reference to the drawings. FIG. 1 is a schematic view of an embodiment of a chemical reaction apparatus 100 according to the present invention, FIG. 2 is a top view of an X portion of a microreactor 106 included in the chemical reaction apparatus 100, and FIG. 3 is a chemistry shown in FIG. 2 is an exploded perspective view of a microreactor 106 included in a reaction apparatus 100. FIG. FIG. 4 is a flowchart showing a control flow when the chemical reaction apparatus 100 is operated.

  The chemical reaction apparatus 100 has a plate-like microreactor 106. In the microreactor 106, a fine channel 103 is formed in order to microreact the first solution containing the first substance and the second solution containing the second substance. The fine flow path 103 is branched into flow paths 103a and 103b so that the first and second reactant solutions 101 and 102 can be supplied to the fine flow path 103. Supply ports 115a and 115b are formed at the ends of the branched flow paths 103a and 103b, respectively. One end of tubes 109a and 109b is connected to each supply port 115a and 115b. A syringe 107a is connected to the other end of the tube 109a, and a syringe 107b is connected to the other end of the tube 109b. The syringes 107 a and 107 b are connected to a pump 108, and the pump 108 is controlled by a pump control device 113.

  In order to take out the reacted product from the microreactor 106, a discharge port 117 is formed at the end of the fine channel, and a tube 111 is connected to the discharge port 117. The end of the tube 111 is led to a solution reservoir 110, and the reaction product solution 104 is stored in the solution reservoir 110.

  Here, in the present invention, in order to detect leakage of the first and second reactant solutions 101 and 102 and the reaction product solution 104 from the microreactor 106, the microreactor 106 has a leak detection flow described in detail later. The path 105 was formed in the vicinity of the fine flow paths 103, 103a, and 103b. A port 116 is formed at one end of the leak detection flow path 105 and a port 118 is formed at the other end. Both ends of the tube 114 with the pressure adjusting device 112 interposed are ports 116 and 118, respectively. It is connected to the. The pressure adjusting device 112 is controlled by the pump control device 113.

  FIG. 2 shows details of the flow paths 103, 103 a, 103 b, and 105 formed in the microreactor 106. In FIG. 1, the flow paths 103, 103 a, 103 b, and 105 are schematically shown, but in FIG. 2, the central portion X of the flow path 103 is shown enlarged. The other flow paths 103a and 103b have the same configuration.

FIG. 2A shows the case where the flow path 103 of the mixed solution in which the first and second reactant solutions 101 and 102 are mixed is formed in a meandering shape. A pair of leak detection flow paths 105 _l and 105 _r are linearly arranged outside the meandering width of the meandering flow path 103. And between two adjacent partial flow paths 103 _i , 103 _{i + 1} (i = 1, 2,...) In the meandering flow path 103, the two partial flow paths 103 _i , 103 _{i + 1} (i = 1, 2, ..)) Are provided in parallel with leak detection flow paths 105 _i (i = 1, 2,...). The leakage detection flow path 105 _i (i = 1, 2,...) Communicates with one leakage detection flow path 105 _l or 105 _r arranged outside the meandering flow path 103. Further, the leakage detection flow path 105 _i (i = 1, 2,...) Is arranged at a slight interval from the meandering flow path 103.

Another example of the leakage detection channel 105 is shown in FIG. Also in this figure, the mixed solution flow path 103 in which the first and second reactant solutions 101 and 102 are mixed is formed in a meandering manner. Then, the leakage detection flow path 105 is formed from first and second leakage detection flow paths 105 _l and 105 _r sandwiching the meandering flow path 103. That is, the first leakage detection flow path 105 _l is always located on the left side of the flow path 103 with respect to the flow direction of the mixed solution, and meanders in the same manner as the flow path 103, so that the second leakage detection flow path The path 105 _r is always located on the right side of the flow path 103 and meanders in the same manner as the flow path 103. The first and second leakage detection flow paths 105 _l and 105 _r are located in the vicinity of the flow path 103.

In this embodiment, the leakage detection flow path 105 provided in the vicinity of the flow path 103 is formed on the same plane as the flow path 103, but it is not always necessary to have the same plane, and the solution leaks from the flow path 103. If this can be detected, the flow path 103 and the leakage detection flow path 105 may be formed on different planes. Further, the leakage detection flow path 105 is composed of a left leakage detection flow path 105 _l and a right leakage detection flow path 105 _r , but the flow state inside the flow path 103 or the flow path 103 If the state can be detected, one of these leakage detection channels 105 _l and 105 _r can be omitted.

Further, if the time until leak detection is acceptable, the leak detection flow path 105 _i (i = 1, 2,...) Can be omitted in FIG. Furthermore, when a place where there is a risk of leakage is known in advance, it is not necessary to form the leakage detection flow path 105 over the entire flow path 103. For example, the corrosion of the flow path 103 is caused by the reaction of the mixed solution. Leakage detection flow path 105 may be formed only in a portion where it easily occurs. In any of these cases, the flow path structure of the leakage detection flow path 105 is simpler than in the present embodiment.

  The operation of the leak detection system having the microreactor 106 configured as described above will be described below. In order to detect the state of the flow path 103 or the internal state of the flow path 103, the pressure adjusting device 112 is used to create a negative pressure in the leakage detection flow path 105 by a predetermined amount. Thereafter, the pump control device 113 controls the pump 108 to send the first and second solutions 101 and 102 in the syringe 107. The first and second solutions 101 and 102 flow into the flow path 103 via the tube 109 connecting the syringe 107 and the microreactor 106.

  In the channel 103, the first and second solutions 101 and 102 are mixed and reacted to generate a reaction product solution 104. The generated reaction product solution 104 is sent to a solution reservoir 110 for recovering the product solution 104 via a tube 111 connecting the solution reservoir 110 and the microreactor 106.

  Here, when the first and second solutions 101 and 102 are being fed, the pressure adjusting device 112 measures the pressure in the leak detection flow path 105 using a pressure measuring means (not shown). Since the leak detection flow path 105 is maintained at a predetermined negative pressure, if fluid leaks from the flow path 103 to the leak detection flow path 105, the first and second solutions 101 and 102, the reaction product solution 104, or substances contained in the first and second solutions 101 and 102 and the reaction product solution 104 are vaporized, and the pressure in the leak detection flow path 105 increases.

  Therefore, when the pressure in the leak detection channel 105 does not change, it can be seen that no fluid leaks from the channel 103. Conversely, when the pressure in the leak detection flow path 105 changes, it is known that fluid is leaking from the flow path 103. That is, if the pressure in the leak detection flow path 105 is measured using the pressure adjusting device 112, the state inside the flow path 103 or the state of the flow path 103 can be detected.

  In the above embodiment, a syringe pump is used as the pump 108. However, as long as the reactant solution in the syringe 107 can be introduced into the substance production apparatus 106, the syringe may be manually pushed. The first and second solutions 101 and 102 are introduced into the microreactor 106 using the syringe 107 and the pump 108, but if the first and second solutions 101 and 102 can be introduced into the microreactor 106, A plunger pump, a diaphragm pump, or a screw pump may be used. Moreover, you may utilize a water head difference.

  The tubes 109 and 111 are made of a material that does not adversely influence the reaction, such as stainless steel, silicon, glass, hastelloy, or silicon resin. Alternatively, corrosion resistance is improved by using stainless steel or silicon whose surface is coated with glass lining, Ni, Au, Ag, or the like, or silicon whose surface is oxidized.

  When the state detection system shown in FIG. 1 is started up or when experimental conditions are changed, the microreactor 106 may be washed to change the first and second solutions 101 and 102. In this case, it is desirable to add a recovery mechanism for recovering each solution as waste liquid from the inside of the syringe 107, the tubes 109 and 111, and the microreactor 106. In this case, the state detection system can be further enhanced.

  In order to control the flow path 103 to a predetermined temperature, for example, it is desirable to use a thermostatic chamber that can accommodate the entire microreactor 106. Alternatively, the microreactor 106 may be sandwiched between Peltier elements or a plate whose temperature is controlled by cooling or heating fluid. A temperature control flow path may be formed in the microreactor 106 to allow a temperature-controlled fluid to flow.

  In the above embodiment, the two types of solutions of the first and second solutions 101 and 102 are mixed in the flow path formed in the microreactor 106, but three or more types of solutions may be mixed. Further, the flow path may have a multilayer structure. Specifically, in addition to a mechanism for mixing and reacting the first and second solutions 101 and 102 to the microreactor 106 and discharging the product solution 104 as a product solution 104, for example, a plurality of solutions are introduced and the flow path 103 is set. A mechanism for obtaining the first solution 101 and the second solution 102, a product solution 104 and several solutions introduced into the microreactor 106, mixed in the flow path 103, and discharged as another reaction product solution, A mechanism for purifying a substance by extraction or distillation from the product solution 104 or the like may be provided.

  When the flow path is formed in the microreactor 106, a pair of substrates is used, a groove is formed on one substrate by a micromachining technique, and another flat substrate is overlapped and bonded. Alternatively, a flow path is formed on one substrate by micromachining technology, and the other substrate is overlaid and then screwed. When the flow path is formed in this way, the substrates can be easily disassembled after the microreactor 106 is used.

  For the microreactor 106, stainless steel, silicon, gold, glass, hastelloy, or silicon resin that does not adversely influence the reaction is used. Alternatively, the corrosion resistance is improved using glass lining, metal coated with Ni, Au, Ag, or the like, or silicon whose surface is oxidized.

  The width of the channel 103 formed in the microreactor 106 is set to be smaller than the diameter of the vortex lump formed as a result of stirring in the batch method. Specifically, it is 1 mm or less. When the channel 103 is made fine, the mixing efficiency is improved. However, if the flow path 103 is too fine, the flow rate, that is, the generation amount decreases, which is not practical. In addition, since there is a high possibility that the flow path 103 is blocked due to contamination of impurities or crystallization due to reaction, the width of the flow path 103 is determined according to the type of reaction and the purpose of use.

  In the above embodiment, the shape of the flow path 103 in which the first and second solutions 101 and 102 are mixed is Y-shaped, but the flow path shape in which the first and second solutions 101 and 102 can be mixed is used. If so, it may be T-shaped. Alternatively, a nozzle that discharges the second solution 102 may be disposed on the wall surface of the flow path through which the first solution 101 flows, and the second reactant solution 102 is placed on the bottom surface of the flow path through which the first solution 101 flows. You may arrange the nozzle to discharge. In addition, the first and second solutions 101 and 102 may be exchanged for introduction.

  In the above embodiment, the shape of the flow path after the first and second solutions 101 and 102 are mixed is a straight line. However, the flow path may be meandered or may be spiral. The selection of these shapes is determined in consideration of the rate at which the reaction product solution is produced from the mixed first and second solutions 101 and 102.

  In the above embodiment, the flow path 103 and the tubes 109 and 111 are connected on the upper surface side of the microreactor 106, but may be connected on the lower surface side or side surface side of the microreactor 106. Although the leak detection flow path 105 and the pressure adjusting device 112 are connected on the side surface of the microreactor 106, they may be connected on the upper surface side or the lower surface side of the microreactor 106. These connection positions are selectively selected according to the specific configuration of the chemical reaction apparatus 100.

  FIG. 3 is an exploded perspective view of the microreactor 106 configured to be disassembled. The decomposition type microreactor 106 shown in FIG. 1A is configured by superposing two first and second substrates 301 and 303 having substantially the same outer shape. In the first substrate 301, the flow path 103 and the leakage detection flow path 105 are formed by a micro processing technique or the like. A sealant 302a made of ethylene tetrafluoride resin is embedded as packing around the flow paths 103 and 105 on the first substrate 301.

  A through hole is formed in the second substrate 303 in accordance with the shape of the flow path 103 formed in the first substrate 301, and the first and second solutions 101 and 102 are transferred to the flow path 103 in the through hole. Supply ports 115a and 115b for connecting the tube 109 to be introduced are attached. A discharge port 117 to which a tube 111 that discharges the reaction product solution 104 generated in the flow path 103 to the outside of the microreactor 106 is connected to a through hole on the downstream side of the flow path 103. In the second substrate 303, ports 116 and 118 for connecting the leak detection flow path 105 and the pressure adjustment device 112 are also formed at positions corresponding to the leak detection flow path 105 of the first substrate 303. .

  FIG. 3B shows an example of the microreactor 106 using a third substrate 302b as an intermediate substrate instead of the sealing material 302a surrounding the flow channel 103 and the leakage detection flow channel 105. The microreactor 106 is configured by laminating an intermediate substrate 302b between two first and second substrates 301 and 303 having substantially the same outer shape. In the first substrate 301, the flow path 103 and the leakage detection flow path 105 are formed by micromachining technology. The leak detection flow path 105 extends to the short side of the first substrate 301, and ports 116 and 118 for connecting the leak detection flow path 105 and the pressure adjusting device 112 are formed at the end thereof. .

  A through hole is formed in the second substrate 303, and the tube 109 for introducing the first and second solutions 101 and 102 into the microreactor 106 and the reaction product solution 104 are discharged into the through hole. Supply ports 115a and 115b and a discharge port 117 for connecting the tubes 111 are attached. The sheet 302b as an intermediate substrate is a soft material, for example, a sheet of tetrafluoroethylene resin. In the sheet 302b, through holes 304a to 304c are formed at the same positions as the through holes formed in the second substrate 303.

  By the way, in the microreactor 106 shown in the above embodiment, the state of the flow channel 103 or the internal state of the flow channel 103 is detected from the change in the pressure in the leakage detection flow channel 105. Therefore, the flow path 103 and the leak detection flow path 105 are kept airtight. In this embodiment, hard materials such as stainless steel, silicon, gold, glass, and hastelloy are used for the first and second substrates 301 and 303 of the microreactor 106 so that the microreactor 106 can withstand repeated use so as to be disassembled. . When these hard materials are used for the substrates 301 and 303, the contact surface pressure of the substrate and its uniformity are determined by the roughness of the substrate surface. If the surface roughness of the substrate is large, it becomes difficult to maintain sufficient airtightness, and the first and second solutions 101 and 102 and the reaction product solution 104 leak from the flow path 103 to the leak detection flow path 105. To do.

  In order to improve the airtightness, in the embodiment shown in FIG. 3A, a soft material sealing material 302a such as tetrafluoroethylene resin is applied to the substrate 301 on which the flow paths 103 and 105 are manufactured by the micro processing technique. It is mated. The sealing material 302 a may be fitted to the bottom surface side of the second substrate 303. In the embodiment shown in FIG. 3B, the first and second substrate-sized sheets 302b covering the flow path 103 and the leakage detection flow path 105 are provided between the first and second substrates 301 and 303. It is sandwiched.

  FIG. 4 is a flowchart showing the control algorithm of the leak detection system shown in the above embodiments. At the start of production (step 401), in the chemical reaction device 100 shown in FIG. 1, the pressure regulator 112 controls the inside of the leak detection flow path 105 to a predetermined negative pressure (step 402). Thereafter, the pump control device 113 drives the pump 108 to send the first and second solutions 101 and 102 into the flow path 103 (step 403).

  The pressure adjustment device 112 measures the pressure in the leak detection flow path 105 (step 404), and refers to the pressure conditions in the leak detection flow path 105 stored in the storage means (not shown), and the first and second solutions 101, It is determined whether or not the liquid 102 is continuously fed to the flow path 103 (step 405). When it is determined that the pressure in the leak detection flow path 105 has not changed in comparison with the pressure conditions in the leak detection flow path 105, the solution does not leak from the flow path 103, so the first and second solutions 101 and 102 are continuously fed (step 403). Steps 403 to 405 are repeated until a predetermined amount of the first and second solutions 101 and 102 are fed.

  Here, strictly speaking, the pressure condition in the leak detection channel 105 is the first and second solutions 101 and 102, or the reaction product solution 104 itself, or the first and second solutions 101 and 102 and the reaction. At least one of the highly volatile solute and the solvent contained in the product solution 104 is determined by the amount leaked into the leak detection flow path 105 and the vapor pressure of the substance at the set pressure in the leak detection flow path 105. It is difficult to predict the amount of vaporized material that leaks into the leak detection flow path 105. However, since the leak detection flow path 105 is maintained at a predetermined negative pressure, the substances in the solutions 101, 102, and 104 flowing in the flow path 103 are immediately vaporized, and the pressure in the leak detection flow path 105 is Increases rapidly. Therefore, the pressure condition in the leak detection flow path 105 depends on the performance of the pressure adjustment device 112.

  When the pressure adjustment device 112 determines that the pressure in the leakage detection flow path 105 has changed, the fluid is leaking from the flow path 103, so the leakage information is fed back to the pump control device 113 and the pump 108 is stopped. (Step 406). The liquid feeding of the first and second solutions 101 and 102 is finished, and the production is forcibly finished (step 407). At the end of the forced production, the first and second solutions 101 and 102 and the reaction product solution 104 remain in the flow path 103 and the leakage detection flow path 105. However, even in that case, a solution with unknown components is not mixed with the reaction product solution 104. Further, since the change in pressure occurs instantaneously with the leakage of the solutions 101, 102, 104, the amount of leakage of the solutions 101, 102, 104 to the outside of the microreactor 106 can be minimized.

  In order to prevent the solution of unknown components from being mixed with the reaction product solution 104, a waste liquid reservoir for storing the waste liquid is provided in addition to the solution reservoir 110 for storing the reaction product solution 104. If it is determined that the pressure in the leakage detection flow path 105 has changed, the pressure change is fed back to the pump control device 113. At the same time, the storage destination of the reaction product solution 104 is switched from the solution reservoir 110 to the waste fluid reservoir. The entire amount of the first and second solutions 101 and 102 is sent to the waste liquid reservoir. At least one of the solutions 101, 102, and 104 remains in both the flow path 103 and the leakage detection flow path 105. However, there is no possibility that a solution with unknown components is mixed in the reaction product solution 104.

  However, when the channel 103 is corroded or when the remaining solution 101 or 102 is about to be exhausted, and when the channel 103 further corrodes, the solution 101, 102, 104 may leak.

  In the above embodiment, the leak detection flow path 105 is maintained at a predetermined negative pressure using the pressure adjusting device 112, but may be a predetermined positive pressure. For example, the inside of the leak detection flow path 105 is filled with an inert gas that does not easily react with the solutions 101, 102, 104 such as helium or argon, and the leak detection flow path 105 is filled with a predetermined pressure using the pressure adjustment device 112. Hold at pressure. And it may be made to detect that a fluid leaks from channel 103 and a pressure changes. Conversely, a substance that immediately reacts with the solutions 101, 102, and 104 is sealed in advance in the leak detection flow path 105, and is maintained at a predetermined pressure using the pressure adjustment device 112. In this case, the leakage of fluid from the flow path 103 can be detected by measuring the change in pressure caused by the reaction with impurities.

  However, when the microreactor 106 is configured by superimposing and screwing the first substrate having the flow path created by the microfabrication technology and the second substrate, the inside of the leak detection flow path 105 is positively pressurized. Then, the applied pressure acts so as to increase the gap of the microreactor 106. Therefore, it is preferable to keep the pressure in the leak detection flow path 105 at a negative pressure.

  When the solutions 101, 102, and 104 leak to some extent from the flow path 103, the leakage can be determined even if the pump control device 113 directly measures a change in pressure in the flow path 103. In this case, it is difficult to grasp a minute leak. Therefore, if the leakage detection flow path 105 is provided and the pressure adjusting device 112 maintains the pressure in the flow path 105 at a predetermined negative pressure, the leakage of the solution from the flow path 103 can be detected with higher accuracy.

  In the above embodiment, leakage of the solution is detected by guiding it to the leakage detection channel 105. At this time, when the solution contains a highly volatile solute and solvent, or when the solution is easily vaporized, the pressure It is also possible to detect the leakage of the solution using a gas detector instead of the adjustment device 112.

  In the above embodiment, the leakage of the solution from the flow path 103 to the leak detection flow path 105 may be detected using a spatial thermal conductivity measurement device instead of the pressure adjustment device 112. In general, since the thermal conductivity is higher in the order of gas, liquid, solid, and metal, when the solution contains liquid, solid, and metal, the leakage of the solution from the flow path 103 changes the thermal conductivity. Can be monitored accurately. A substance that easily reacts with the solutions 101, 102, 104 or the components in the solutions 101, 102, 104 is enclosed in the leak detection channel 105 in advance, and the spatial thermal conductivity change due to the reaction is measured using a spatial thermal conductivity measuring device. It is also possible to detect the leakage of the solution from the flow path 103 by measuring.

  In the above embodiment, the leakage of the solution from the flow path 103 to the leakage detector 105 may be detected using an electrical conductivity measurement device instead of the pressure adjustment device 112. Since the electrical conductivity is large for metals and ions, when the solution contains metals or ions, leakage of the solution can be accurately monitored from the change in electrical conductivity. When the substance generated by the reaction is a metal or ion, the leakage of the reaction product from the flow path 103 can be accurately detected from the change in electrical conductivity.

  When the first and second solutions 101 and 102 or the reaction product solution 104 are colored, the microreactor 106 is made colorless and transparent or colorless and transparent such as glass or silicon resin that is resistant to the colored solution. It is made of a close material. In this case, the leakage of the solution from the flow path 103 to the leak detection flow path 105 is detected without using a pressure adjusting device, a gas detector, a spatial thermal conductivity measurement apparatus, an electrical conductivity measurement apparatus, or the like. It can be easily judged from the color change. Even if the solutions 101, 102, and 104 themselves are not colored, the solution 101, 102, and 104 may react with the liquid enclosed in the leak detection flow path 105 and develop a color so long as the liquid in the leak detection flow path 105 is not colored. The leakage of the solution from the channel 103 can be easily detected from the color change due to the reaction.

  In the above embodiment, the chemical reaction apparatus has only one microreactor 106, but it goes without saying that two or more microreactors may be provided. Further, the newly added microreactor may be one used in a normal batch method. When a plurality of microreactors are provided, they may be arranged in series, or only specific microreactors among a plurality of microreactors arranged in parallel may be arranged in the series. Two types of microreactors may be connected to a specific microreactor.

  In the above embodiment, the first solution 101 and the second solution 102 are used as starting solutions, but at least one of the first solution 101 and the second solution 102 is generated by a reaction generated by another microreactor. It may be a product solution. Further, at least one of the first and second solutions 101 and 102 may be a target product solution of another microreactor.

It is a schematic diagram of one Example of the leak detection system which concerns on this invention. It is a top view of the microreactor used for the leak detection system shown in FIG. It is a disassembled perspective view of the microreactor used for the leak detection system shown in FIG. It is a control flowchart of the leak detection system shown in FIG.

Explanation of symbols

DESCRIPTION OF SYMBOLS 100 ... Chemical reaction apparatus, 101 ... 1st solution, 102 ... 2nd solution, 103 ... Flow path, 104 ... Reaction product solution, 105 ... Leak detection flow path, 106 ... Micro reactor (substance manufacturing apparatus), 107 ... Syringe, 108 ... Pump, 109 ... Tube, 110 ... Solution reservoir, 111 ... Tube, 112 ... Pressure adjustment device, 113 ... Pump control device, 114 ... Tube, 115a, 115b ... Supply port, 116 ... Port, 117 ... Discharge Port 118, 301... First substrate 302a... Sealing material 302b... Sheet (intermediate substrate) 303.

Claims (7)

  In an apparatus for producing a substance, comprising: a first substrate on which a flow path for mixing and flowing a first and second solution is formed; and a second substrate airtightly attached to the first substrate. In the vicinity of the flow path formed on the first substrate, a leakage detection flow path for detecting leakage of the first and second solutions or the reaction product solution from the flow path is formed. Manufacturing equipment for substances to be used.   2. The flow path according to claim 1, wherein the flow path is formed in a meandering shape, and the leakage detection flow path is formed by a plurality of flow paths having branch portions extending between the meandering flow paths. Substance manufacturing equipment.   2. The substance manufacturing apparatus according to claim 1, wherein the flow path is formed in a meandering shape, and the leakage detection flow path is formed from two meandering flow paths sandwiching the meandering flow path.   Pressure detection means for detecting the pressure of the leakage detection flow path, and a pressure adjustment device for comparing the pressure with a predetermined value to determine the leakage of the solution. The apparatus for producing a substance according to any one of claims 1 to 3, wherein the path can be maintained at a negative pressure.   A fluid is sealed in the leak detection flow path, and a detection means is provided for detecting at least one of a gaseous component, spatial thermal conductivity, and electrical conductivity of the fluid in the leak detection flow path. Item 2. The apparatus for producing a substance according to Item 1.   6. The substance manufacturing apparatus according to claim 5, wherein means for maintaining the leak detection flow path at a negative pressure is provided.   A pump capable of feeding the first and second solutions, a pump control device for controlling the amount of the first and second solutions fed by the pump, and the first and second solutions are supplied. And a microreactor having a channel for mixing and reacting the first and second solutions, and the microreactor is hermetically coupled to the first substrate having the channel and the first substrate. A leakage detection flow path having a negative pressure sealed in the vicinity of the flow path formed in the first substrate, and a pressure detection means for detecting the pressure of the leakage detection flow path, A chemical reaction device characterized by comprising a pressure adjusting device for comparing the pressure detected by the pressure detection means with a predetermined value and judging leakage of the first and second solutions or their mixed reaction product solution. .

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