JP2011104512A - System and method for cleaning micro flow passage - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a system and method for cleaning a micro flow passage. <P>SOLUTION: The system includes a chip 32 which forms a micro flow passage 34 producing a desired product from a raw material liquid in a state immersed in fluids 14 and 16 supplied to a housing 12, switching valves 28 and 38 interposed on a route immersed in the fluid, one being connected to the micro flow passage 34 side and the other being connected mutually switchably between the fluid side and a circulation side of the raw material liquid, a vacuum pump 50 depressurizing the inside of the housing 12 to produce bubbles in the micro flow passage 34, an ultrasonic vibrator 52 discharging the bubbles outside the micro flow passage 34 while irradiating the micro flow passage 34 with ultrasonic waves to clean the inside of the micro flow passage 34, and a control means for switching-controlling the connection of the switching valves 28 and 38 to the fluid side in cleaning the micro flow passage 54, and at the same time, activating the ultrasonic vibrator 52 and the vacuum pump 50. The system enables a stationary cleaning of the micro flow passage 34. <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

  The present invention relates to a microchannel cleaning system and a microchannel cleaning method, and more particularly to a microchannel that performs a reaction operation using a plurality of raw material liquids in a microchannel having an equivalent diameter of about 50 μm. The present invention also relates to a cleaning system and a cleaning method for performing a drying process of a micro-channel as required.

  A microchemical device generally called a microreactor performs unit operations or reaction operations such as mixing and separation for chemical reaction and substance production using phenomena in a micro space with a diameter of several μm to several hundred μm. (See Patent Document 1). This microreactor uses the phenomenon that the flow of the reaction fluid becomes laminar in the micro space, and actively forms a wide reaction interface, thereby improving the efficiency and speed of the reaction and mixing between the fluids. In recent years, it has attracted attention as an innovative technology that can be used. As this microreactor, a precise reaction / mixing system for a raw material liquid or the like using a microchannel formed by a fine processing technique such as etching has been proposed. In general, a plurality of such microreactors are provided in parallel to obtain a target product in a large amount in a short time (see Patent Document 2).

  However, such reaction and mixing in the micro space and the resulting product are likely to settle, adsorb, or crystallize in the micro flow channel, and easily contaminate the micro flow channel. Due to the contamination, the raw material throughput and metering accuracy cannot be maintained, and the advantages as a microreactor are impaired. Therefore, the microchannel is periodically cleaned and dried after cleaning.

  When cleaning the microchannel, remove the chip (microreactor) on which the microchannel has been formed from the device and clean it manually by rubbing with a brush or sponge, or immerse the removed chip in an ultrasonic cleaning tank. Then, the ultrasonic wave emitted from the ultrasonic vibrator is irradiated to remove contaminants in the microchannel. When the chips were then dried, they were dried by blowing nitrogen or dry air in a state where they were removed from the apparatus, or were put into a drying cabinet to evaporate moisture.

  As another cleaning method, the chip remains in the chip by stationary cleaning (so-called CIP cleaning) in which a fluid mixed with a detergent for removing contaminants is circulated through the microchannel while the chip is installed in the apparatus. Or a method of removing contaminants adhering to the flow path wall (see Patent Documents 3 and 4). In subsequent chip drying, nitrogen, dry air, or the like was supplied to the microchannel through a pipe to remove moisture.

JP 2005-97089 A JP 2008-80306 A JP 2006-272268 A JP 2007-326181 A

  However, when the chip is removed and the cleaning and drying operations are performed manually, the operation is complicated, and it is necessary to wash one by one and time is required. In particular, in a configuration having a plurality of chips as in Patent Document 2, all cleaning is performed. It becomes remarkable when doing. Further, in the cleaning process, there is a possibility that dirt with a size that is difficult to be seen by human eyes or dirt that has entered a gap that cannot be reached with a sponge cannot be removed by manual cleaning with a brush or sponge.

  On the other hand, when the microchannel is cleaned by CIP cleaning, since there is no work for removing the chip as described above, problems such as burden on the operator and work unevenness due to manual labor can be avoided. Since there is a risk of corrosion on the surface, the concentration of the chemical solution is limited, and therefore it takes a long time to pass the solution. In addition, since the micro-channel has a narrow channel diameter (for example, micron scale), it is difficult to circulate the fluid at high speed. Even if possible, a pump with high discharge pressure is required, or high-speed fluid flows. Deterioration of the inner wall surface due to erosion of the road was a problem. Further, even when the microchannel is removed and drying is performed in the drying cabinet, there is a problem that the wall surface of the microchannel may be deteriorated because the chip is heated to a high temperature.

  In addition, the invention described in Patent Document 3 has a method aiming to generate periodic laminar flow vortices (Karman vortices) in the microchannel and knock out the fouling adhering to the inner wall of the microchannel. However, when the diameter of the microchannel is 100 μm or less, it is difficult to generate a laminar vortex, and it is difficult to obtain a cleaning effect. Further, the invention described in Patent Document 4 is a method aiming at the effect of generating bubbles by electrolysis in the microchannel and stripping off the dirt attached to the inner wall of the microchannel by the bubbles. May cause corrosion of the microchannel, and it is not preferable to repeat this method.

  In the drying process after the washing process of any of the above methods, the momentum of the jet is strong near the inlet of the drying fluid, and there is an effect of removing moisture, but the momentum also decreases near the outlet, and the gas accompanied by moisture However, since it flows from the upstream of a microchannel, there existed a problem that the drying effect fell.

  Accordingly, the present invention focuses on the above problems and provides a microchannel cleaning system and a microchannel cleaning method that efficiently clean and dry the microchannel without damaging the microchannel. The purpose is to do.

  In order to achieve the above object, a micro-channel cleaning system according to the present invention is first formed at a merging position of a plurality of paths through which a raw material liquid is circulated, and the fluid supplied into the housing together with the paths. A microchannel that produces a desired product from the raw material liquid in the immersed state, and a microchannel that is interposed on the path immersed in the fluid, one connected to the microchannel side, the other connected to the fluid side and the raw material A switching valve connected to the liquid distribution side so as to be switchable with each other, a decompression means for decompressing the inside of the housing and generating bubbles in the microchannel, and irradiating the microchannel with ultrasonic waves An ultrasonic transducer for discharging the bubbles to the outside of the microchannel while cleaning the inside of the microchannel, and switching control of the switching valve to the fluid side at the time of cleaning the microchannel and the ultrasonic wave Oscillator and front And a control means for operating the pressure reducing means, characterized in that to enable cleaning in place of the microchannel.

Second, a plurality of the micro flow paths are arranged in the casing and connected in parallel to each other.
Third, it has fluid supply / discharge means connected to the casing and capable of switching between a state in which the fluid is supplied to the casing and a state in which the supplied fluid is discharged, and the control means The switching control of the fluid supply / discharge means is performed.

  Fourth, the casing includes a heating unit that heats the fluid supplied to the casing, and the control unit switches and controls the connection of the three-way valve to the fluid side after the cleaning, Control for operating the heating means for a predetermined time is performed.

  Fifth, the fluid supply / discharge means supplies the first fluid to the housing, discharges the first fluid and supplies the second fluid, and supplies the second fluid. It is possible to sequentially switch between the discharged state and the control means, through the fluid supply / discharge means, to supply the first fluid when the raw material liquid is passed, and to supply the second fluid at the time of cleaning. Control is performed to supply and discharge the second fluid after cleaning.

  On the other hand, in the microchannel cleaning method according to the present invention, firstly, the raw material liquid is formed in a joined position of a plurality of paths through which the raw material liquid flows and is immersed in the fluid supplied in the housing. A micro flow path for generating a desired product is formed so that a connection to the flow side of the raw material liquid and a connection to the fluid side can be alternately switched, and the connection of the micro flow path to the fluid side is switched. In addition, the inside of the casing is decompressed to generate bubbles in the microchannel, and the microchannel is irradiated with ultrasonic waves to discharge the bubbles outside the microchannel while washing the inside of the microchannel. In this way, the microchannel is subjected to stationary cleaning.

Third, after cleaning the inside of the micro flow path, the fluid supplied to the housing is discharged, and the inside of the housing is decompressed.
Fourth, after the microchannel is washed, the microchannel is switched to the distribution side, and then the fluid supplied to the casing is heated.

  Fifth, the second fluid for discharging the fluid from the housing and cleaning the microchannel when the microchannel is cleaned is supplied, and the second fluid is discharged after the cleaning. And

  According to the microchannel cleaning system and the cleaning method of the present invention, first, a chip (microreactor) having a microchannel is arranged in a casing in a state of being immersed in a fluid for temperature adjustment. . In this state, even if the microchannel is opened to the fluid side, the fluid hardly flows into the microchannel. However, by reducing the pressure in the casing and the casing that hermetically seals the fluid, air dissolved in the raw material liquid can be precipitated, and bubbles can be generated in the microchannel. Furthermore, since the kinetic energy is given to the bubbles by irradiating the ultrasonic waves to the microchannels, the bubbles are discharged out of the microchannels. Therefore, the fluid enters the microchannel instead of the released bubbles. Thereby, the wall surface of the microchannel is cleaned by the fluid and the irradiated ultrasonic wave. Since the bubbles are generated in the entire area of the microchannel, the fluid that replaces the bubbles reaches the entire microchannel. Therefore, it is possible to efficiently clean the inside of the microchannel by spreading the fluid over the entire microchannel. Since the opening to the raw material liquid side and the opening to the fluid side can be switched to each other, there is no need to remove the housing having the micro flow path. Therefore, it is possible not only to avoid the work burden such as the removal work of the housing, but also to perform the washing etc. in a fixed state, so that the distortion of the microchannel and the change of the surface shape of the microchannel are suppressed, A product of constant quality can be produced.

Secondly, by arranging a plurality of microchannels in parallel, a desired product can be generated in parallel to increase the generation efficiency.
Thirdly, the inside of the micro channel can be decompressed by opening the channel to the housing by decompressing the inside of the housing. Therefore, it is possible to evaporate the fluid remaining in the microchannel, and thereby the inside of the microchannel can be dried. Therefore, generation | occurrence | production of a drying nonuniformity can be suppressed and a drying operation can be performed efficiently.

  Fourth, it is possible to evaporate the fluid remaining in the microchannel by blocking the microchannel from the housing side and heating the fluid immersed in the microchannel. Can be dried. Therefore, since pressure reduction in the housing is not necessary, the process can be simplified and the cost can be reduced.

  Fifth, since the microchannel is cleaned using the second fluid, a fluid having a high cleaning effect and drying effect can be used at the time of cleaning, and the microchannel is efficiently cleaned. be able to.

It is a mimetic diagram of a washing system of a micro channel concerning this embodiment. It is a figure which shows the control flow of the washing | cleaning system of the micro flow path which concerns on this embodiment.

  Hereinafter, the present invention will be described in detail with reference to embodiments shown in the drawings. However, the components, types, combinations, shapes, relative arrangements, and the like described in this embodiment are merely illustrative examples and not intended to limit the scope of the present invention only unless otherwise specified. .

  FIG. 1 shows a microchannel cleaning system according to this embodiment. 1A is a perspective view of the entire micro-channel cleaning system, FIG. 1B is a channel when manufacturing a micro-channel product, and FIG. 1C is a micro-channel cleaning and drying time. The flow path of is shown. The cleaning system 10 according to the present embodiment is formed at a joining position of a plurality of paths through which the raw material liquid is circulated, and the paths are supplied to the fluid (first fluid 14 and second fluid 16) supplied into the housing 12. The microchannel 34 (chip 32) that generates a desired product from the raw material liquid in a state of being immersed together with the (piping 26, 30, 36, 39), and a path immersed in the fluid, one of which is interposed A switching valve (first three-way valve 28, second three-way valve 38) connected to the micro-channel 34 side and connected to the other side so as to be switchable between the fluid side and the raw material liquid flow side. ), Pressure reducing means (vacuum pump 50) for generating a bubble in the microchannel 34 by depressurizing the inside of the housing 12, and irradiating the microchannel 34 with ultrasonic waves to clean the inside of the microchannel 34 While the bubble is out of the microchannel 34 A control unit (not shown) for controlling the connection of the switching valve to the fluid side during the cleaning of the micro-channel 34 and operating the ultrasonic transducer 52 and the decompression unit when cleaning the micro-channel 34. The microchannel 34 can be cleaned in place. A plurality of the microchannels (chips 32) are arranged in the housing 12 and connected in parallel to each other.

  And it is connected to the housing 12 and can switch between a state in which the fluid (first fluid 14 and second fluid 16) is supplied to the housing 12 and a state in which the supplied fluid is discharged. The fluid supply / discharge means 18 is provided, and the control means 52 performs switching control of the fluid supply / discharge means 18.

  Further, the casing 12 has heating means (not shown) for heating the fluid (first fluid 14) supplied to the casing 12, and the control means 52 The connection of the one three-way valve 28 and the second three-way valve 38) is controlled to be switched to the fluid side, and the heating means (not shown) is operated for a predetermined time.

  Therefore, in the microchannel cleaning method according to the present embodiment, the fluid (the first fluid 14 and the second fluid 16) formed in the joining position of the plurality of paths through which the raw material liquid flows is supplied into the housing 12. The microchannel 34 for generating a desired product from the raw material liquid in a state immersed in the liquid) is formed so that the connection to the flow side of the raw material liquid and the connection to the fluid side can be switched alternately, The micro channel 34 is switched to the fluid side, the inside of the housing 12 is decompressed to generate bubbles in the micro channel 34, and the micro channel 34 is irradiated with ultrasonic waves to irradiate the micro channel 34. The micro-channel 34 is fixedly cleaned by discharging the bubbles to the outside of the micro-channel 34 while cleaning the inside. A plurality of the micro flow paths 34 are arranged in the housing 12 and connected in parallel to each other.

Then, after the inside of the micro flow path 34 is washed, the fluid supplied to the housing 12 is discharged, and the inside of the housing 12 is decompressed.
Further, after the microchannel 34 is washed, the microchannel 34 is switched to the flow side, and then the fluid (second fluid 16) supplied to the housing 12 is heated.

  The casing 12 is supplied with fluids (first fluid 14 and second fluid 16) for immersing the chip 32 in which the microchannels 34 are formed, and hermetically seals the inside so that the atmospheric pressure can be adjusted. It has a configuration. A supply port 12a for supplying the first fluid 14, a supply port 12b for supplying the second fluid, and a discharge port 12c for discharging the first fluid and the second fluid are provided in the upper part of the housing 12. Yes. A vacuum pump 50 serving as a decompression unit is attached to the housing 12. The vacuum pump is connected to the pressure gauge 50a, and operates so as to maintain the value when the pressure indicated by the pressure gauge 50a reaches a predetermined pressure. Here, it is assumed that the supply ports 12a and 12b and the discharge port 12c are configured to be closed when the vacuum pump 50 is operated so that the inside of the housing 12 can be hermetically sealed. Further, the casing 12 is provided with a temperature adjustment mechanism (not shown), and the temperature of the supplied fluid can be adjusted.

  The fluid supply / discharge means 18 is connected to the housing 12, supplies the first fluid 14 from the supply port 12 a and stores the first fluid 14 in the housing 12, and discharges the first fluid 14. A state of discharging from the outlet 12c, a state of supplying the second fluid 16 from the supply port 12b and storing the second fluid 16 in the housing 12, and a state of discharging the second fluid 16 from the discharge port 12c Are operated in sequence by operating a valve or the like interposed in a pipe leading to the supply ports 12a and 12b and the discharge port 12c, and this switching is controlled by the control means 52. Here, the first fluid 14 is stored in the housing 12 when the raw material liquid is passed through the micro flow path 34, that is, in the manufacturing process described later of the desired product, and the second fluid 16 is stored in the micro flow. It is used in the later-described washing process and drying process of the path 34.

  The first fluid 14 adjusts the temperature of the microchannel 34 by immersing a chip 32 on which the microchannel 34 is formed in the manufacturing process described later. The first fluid 14 joins the raw material liquid in the microchannel 34. Temperature adjustment is performed by a temperature adjustment mechanism (not shown) so as to obtain an optimum temperature for obtaining a desired material. The second fluid 16 is introduced into the microchannel 34 at the time of cleaning the microchannel, and serves as a cleaning liquid for cleaning the inner wall of the microchannel 34.

  Therefore, the first fluid 14 and the second fluid 16 are made of a material that does not corrode the micro flow path 34 and the chip 32 forming the micro flow path 34, and water, oil, water vapor, or the like can be used. Further, the second fluid 16 may be mixed with a detergent, an alkaline solution, an enzyme agent, etc., in order to promote the cleaning effect. Further, the second fluid 16 may use a liquid that easily volatilizes within a range that does not damage the inner wall of the microchannel 34, such as an organic solvent such as alcohol or acetone, in order to promote a cleaning effect and a drying effect.

  In this embodiment, the raw material liquids (A1, A2, A3) are supplied from the supply tank 20, the pipe 22, the liquid feed pump 24, the pipe 26, the first three-way valve 28, the pipe 30, the micro flow path 34 (chip 32), The pipe 36, the second three-way valve 38, the pipe 39, the third three-way valve 40, the pipe 42, and the receiving tank 44 pass through the flow path in this order. Of these, the pipe 26, the first three-way valve 28, the pipe 30, the tip 32, the pipe 36, the second three-way valve 38, and the pipe 39 are immersed in the above-described fluids (the first fluid 14 and the second fluid 16). ing.

  In the present embodiment, three supply tanks 20 are arranged in parallel to form a flow path in which a liquid feed pump 24 and a first three-way valve 28 are connected in series, and these flow paths are mutually connected within a micro flow path 34. Join. Each of the supply tanks 20 is filled with a raw material liquid (A1, A2, A3) provided to obtain a desired product in the micro flow path 34, and the raw material liquid is supplied to the micro flow path 34 side by a liquid feed pump 24 through a pipe. To be supplied.

  The micro flow path 34 formed in the chip 32 is for joining two or more kinds of raw material liquids to generate a desired product. The micro flow path 34 is connected to the pipe 30 on the upstream side of the flow path of the raw material liquid, and is connected to the pipe 36 on the downstream side. In the present embodiment, a desired product formed by joining the three raw material liquids is discharged to the receiving tank 44 at the subsequent stage, and the product is stored in the receiving tank 44. Furthermore, in this embodiment, three chips 32 are arranged in parallel. Correspondingly, the pipe 30 is branched into three and connected to the upstream side of the microchannel, and the pipe 36 is formed so that three paths extending from the downstream side of the microchannel merge into one. Is done.

  In addition, the temperature of the microchannel 34 is adjusted by the first fluid 14 described above, and is maintained at an optimum temperature for obtaining a desired product by the first fluid 14 during the passage of the raw material liquid. Therefore, the micro flow path 34 joins the raw material liquids flowing from the pipe 30, generates a desired product while passing the joined raw material liquids through the micro flow path 34, and feeds the raw material liquid including the product to the pipe 36. Discharge.

  The chip 32 forming the microchannel 34 has, for example, a structure in which two plates are bonded to each other. A groove having a semicircular cross section is formed at a position opposite to each other on the bonding surface of the plate. By sticking the plates together in this state, a microchannel having a circular cross section is formed in the chip.

  In the manufacturing process in the microchannel 34, various unit operations and reaction operations are performed. For example, unit operations include mixing, separation, classification, filtration, heating, cooling, heat exchange, extraction, crystallization, dissolution, evaporation, distillation, absorption, adsorption, and reaction operations include inorganic and organic substances. Ion reaction, redox reaction, electric field reaction, nitrification reaction, combustion reaction, firing reaction, roasting reaction, halogenation reaction, sulfonation reaction, alkylation reaction, esterification reaction, fermentation reaction, thermal reaction, catalytic reaction , Radical reaction, polymerization reaction and the like. In order to perform these operations, materials such as ceramic, glass, silicone, and resin can be used as the material of the microchannel 34. If high heat conductivity is required for the microchannel 34, metal or the like can be used.

  The first three-way valve 28 serving as a switching valve is interposed on a path (pipe 26, pipe 30) through which the raw material liquid (A1, A2, A3) flows, and one is connected to the pipe 30 and the other is pipe 26. And an opening 28a opened in the housing 12 so as to be switchable with each other. That is, one is connected to the chip 32 side, and the other is connected to the supply tank 20 side (raw material liquid distribution side) and the inside of the housing 12 (fluid side) in a mutually switchable state. Therefore, when the first three-way valve 28 is connected (opened) to the supply tank 20 side, the raw material liquid can be passed from the supply tank 20 and connected to the inside of the housing 12 (opened). In this case, the fluid (second fluid 16) supplied to the housing 12 can be circulated to the chip 32 side as will be described later. The liquid feed pump 24 is linked to the first three-way valve 28 to be connected, and the operation is stopped when the first three-way valve 28 is connected (opened) to the inside of the housing 12. .

  The second three-way valve 38 serving as another switching valve is interposed on a path (pipe 36, pipe 39) through which the raw material liquid (B) flows, passes through the chip 32, and passes through the manufacturing process ( B) is discharged to the receiving tank 44 side, or the second fluid 16 is supplied to the chip 32 side as will be described later. One of the second three-way valves 38 is connected to the pipe 36, and the other is connected to the pipe 39 and the opening 38 a opened in the housing 12 in a state where the two can be switched to each other. That is, one is connected to the chip 32 side, and the other is connected in a state that can be switched between the receiving tank 44 side and the inside of the housing. The second three-way valve 38 is linked to the first three-way valve 28. When the first three-way valve 28 is connected (opened) to the supply tank 20 side, the second three-way valve 38 is connected (opened) to the receiving tank 44 side. When the three-way valve 28 is connected (opened) to the inside of the housing 12, it is connected (opened) to the inside of the housing 12.

  The third three-way valve 40 is disposed downstream of the second three-way valve 38 in the flow path, and discharges the raw material liquid (B) to the receiving tank 44 side, or waste liquid after the cleaning process (second fluid 16 Alternatively, the raw material liquid) is discharged to the waste liquid tank 48. The third three-way valve 40 is connected so as to be switchable between a pipe 42 that connects one side to the pipe 39 and a pipe 42 that connects the other side to the receiving tank 44 and a pipe 43 that connects to the waste liquid tank. The third three-way valve 40 is interlocked with the second three-way valve 38. When the second three-way valve 38 is connected (opened) to the receiving tank 44 side, the third three-way valve 40 is connected (opened) to the receiving tank 44 side. When the three-way valve 38 is connected (opened) to the inside of the housing 12, it is connected (opened) to the waste liquid tank 48 side.

The on-off valve 46 is interposed in the pipe 43 and is normally closed, but is opened by control of a control means (not shown) immediately after a later-described cleaning process or at the time of a drying process.
Therefore, when the first three-way valve 28 is connected to the supply tank 20 side, the second three-way valve 38 and the third three-way valve 40 are connected to the receiving tank 44 side. Therefore, the raw material liquid stored in the supply tank 20 passes through the first three-way valve 28, is introduced into the chip 32 (micro flow path 34), and joins to generate a desired product. The contained raw material liquid is discharged from the chip 32 (micro flow path 34) and supplied to the receiving tank 44 via the second three-way valve 38 and the third three-way valve 40. On the other hand, when the first three-way valve 28 is connected to the inside of the housing 12, the second three-way valve 38 is connected to the inside of the housing 12, and the third three-way valve 40 is connected to the waste liquid tank 48 side. However, as long as the above-described on-off valve 46 is closed, the fluid (second fluid 16) in the housing 12 does not flow out to the waste liquid tank 48.

  The heating means (not shown) is used in the drying process of the microchannel 34. The driving of the heating unit (not shown) is controlled by a control unit (not shown), and heats the fluid (first fluid 14) supplied into the housing 12 to heat the inside of the microchannel 34.

  The control means (not shown) is an application installed in a PC (not shown), for example, and is a fluid supply / discharge means 18, a vacuum pump 50, a first three-way valve 28, a second three-way valve 38, a third The three-way valve 40, the on-off valve 46, and a heating means (not shown) are connected, and the operation thereof is controlled by a key operation, a program, or the like to clean and dry the micro flow path 34.

  FIG. 2 shows a flowchart of the microchannel cleaning system of the present embodiment. In the present embodiment, a first cleaning step 56 for cleaning the microchannel 34 by introducing the second fluid 16 into the microchannel 34 and a step after the first cleaning step 56, The second fluid 16 is a step after the first drying step 60 and the first cleaning step 56 in which the microchannel 34 is dried by discharging the second fluid 16 and depressurizing the inside of the housing 12. A second drying step 62 for drying the micro flow path 34 by heating the liquid, and a second cleaning step for cleaning (or washing) the micro flow path 34 by irradiating only the ultrasonic wave while passing the raw material liquid. 58. Therefore, the control means (not shown) selects one of the above processes corresponding to the usage state of the microchannel 34 to wash or dry the microchannel 34. Here, the first drying process 60 or the second drying process 62 is performed after the first cleaning process 56 because the second fluid 16 remaining in the microchannel 34 after cleaning and the raw material liquid are mixed. This is to avoid the possibility that unnecessary components are generated in the micro flow path 34.

  Control means (not shown) drives each component so as to pass through each stage from stage 101 (production end) to stage 123 (production restart). Here, in the stage 101, the first fluid 14 is stored in the housing 12, and the first fluid 14 is in a state where the chip 32 is immersed.

  First, the case where the 1st washing | cleaning process 56 is performed is demonstrated. In order to execute the stage 102 (cooling / heating medium exchange in the casing), the presence or absence is input by a key operation or the like in a control means (not shown). Next, in order to execute the stage 103, the control means (not shown) operates the fluid supply / discharge means 18, discharges the first fluid 14 stored in the casing 12, and discharges the second fluid 16 to the casing. The first three-way valve 28 and the second three-way valve 38 are connected to the inside of the housing 12 and the third three-way valve 40 is connected to the waste liquid tank side to execute the stage 104 (three-way valve opening). To do. As a result, the flow path of the raw material liquid is blocked, the upstream side and the downstream side of the flow path of the raw material liquid are opened to the second fluid 16 in the micro flow path 34, and the cleaning liquid is supplied by the stage 105 (supplying the cleaning liquid into the housing) The second fluid 16 flows into the microchannel 34 from the opening 28a and the opening 38a.

  However, inflow of the second fluid 16 is insufficient in this state. Therefore, in order to execute the stage 106 (decompression in the casing), the control means (not shown) operates the vacuum pump 50 to depressurize the casing 12. Then, the second fluid 16, the raw material liquid remaining in the microchannel, and the air dissolved in the second fluid 16 flowing into the microchannel are deposited to form bubbles. Further, in order to execute the stage 107 (in-chip cleaning), a control means (not shown) operates the ultrasonic vibrator 52 for a predetermined time while the vacuum pump 50 is operated, and ultrasonic waves are applied to the chip 32 (microchannel 54). Irradiate. Then, the air bubbles generated in the micro flow path 34 are released into the housing 12 through the openings 28a and 38a, and the second fluid 16 stored in the housing 12 in such a manner that the bubbles are exchanged. It flows into the microchannel 34 from the opening 28a and the opening 38a. At this time, even if the microchannel 34 has an inner diameter of about 50 μm, it is difficult to generate bubbles in the microchannel 34 and irradiate ultrasonic waves to discharge the bubbles outside the microchannel 34. Does not occur. Therefore, the inner wall of the microchannel 34 is cleaned by the inflowing second fluid 16 and the irradiated ultrasonic waves.

  When the cleaning is completed, the control means (not shown) for the stage 108 (return pressure in the casing) stops the operation of the ultrasonic vibrator 52 and the vacuum pump 50 to return the inside of the casing 12 to the atmospheric pressure, and the stage 109 ( The on-off valve 46 is driven to discharge the waste matter and the second fluid 16 peeled off from the inner wall of the micro flow path 34. At this time, the second fluid 16 at a higher water level than the openings 28a, 38a opened to the inside of the housing 12 of the first three-way valve 28 and the second three-way valve 38 is discharged via the on-off valve 46, The second fluid 16 below the water level remains in the housing 12 as it is. Therefore, the control means (not shown) drives the fluid supply / discharge means 18 to discharge the second fluid 16 remaining in the housing 12 from the discharge port 12c, whereby the first cleaning step 56 is completed.

  Next, it is determined whether or not the first drying step 60 and the second drying step 62 are performed in the stage 111 (in-chip drying). If neither drying step is performed, the stage 121 (three-way valve closed) is determined. Thus, the control means (not shown) switches the first three-way valve 28 and the second three-way valve 38 to open to the supply tank 20 side, and switches the third three-way valve 40 to open to the receiving tank 44 side. To control and close the on-off valve 46. Then, the control means (not shown) drives the fluid supply / discharge means 18 to supply the first fluid 14 serving as the cooling / heating medium into the casing by the stage 122 (cooling / heating medium injection into the casing). Further, the control means (not shown) operates the temperature adjusting mechanism (not shown) by adjusting the temperature of the first fluid 14 to a predetermined temperature by the stage 117 (cooling / heating medium temperature adjustment), and the stage 123 (resuming production). ), The liquid feed pump 24 is operated, and the raw material liquid is passed through the microchannel 34.

  Next, the case where it is determined that the drying process is performed in the stage 111 (in-chip drying) will be described. In the stage 112 (chip temperature control), the first drying process (without temperature control) or the second drying process (with temperature control) is determined. At this time, all of the fluid (second fluid 16) in the housing 12 is discharged by the stage 109 (cleaning waste liquid discharge), and the first three-way valve 28 and the second three-way valve 38 are the housing. 12 is opened, the third three-way valve 40 is opened to the waste tank 48 side, and the open / close valve 46 is opened.

  First, the case where the 1st drying process 60 is selected is demonstrated. In the stage 118 (decompression in the casing), the control means (not shown) closes the on-off valve 46 and operates the vacuum pump 50 for a predetermined period of time to depressurize the interior of the casing 12 and the micro flow path 34 for a predetermined period of time. Then, in the stage 119 (drying in the chip), the second fluid 16 and the like remaining in the microchannel 34 are evaporated, and thereby the inside of the microchannel 32 can be dried. In the stage 120 (returning pressure in the casing), the control means (not shown) stops the operation of the vacuum pump 50 to return the pressure in the casing 12 to atmospheric pressure, and proceeds to the stage 121 (three-way valve closed) described above. To do.

  And the case where the 2nd drying process 62 is selected is demonstrated. In the stage 113 (three-way valve closing), the control means (not shown) closes the inside of the housing 12 of the first three-way valve 28 and the second three-way valve 38 to open the supply tank 20 side, and the third three-way The valve 40 and the on-off valve 46 are left as they are. As a result, the micro flow path 34 is isolated from the inside of the housing 12. Then, in the stage 114 (heating medium supply into the casing), the control means (not shown) operates the fluid supply / discharge means 18 to supply the first fluid 14 into the casing 12 and the stage 115 (heating medium supply). In the temperature adjustment, the control means (not shown) operates the heating means (not shown) for a predetermined time to heat the first fluid 14. Then, the chip 32 is heated by the first fluid 14, and thereby the microchannel 34 is also heated for a predetermined time. Thereby, in the stage 116 (drying in the chip), the second fluid 16 and the like remaining in the microchannel 34 is vaporized and discharged to the outside through the on-off valve, whereby the microchannel 34 can be dried. . After the microchannel 34 is dried, the operation of the heating means (not shown) is stopped and the process proceeds to the stage 117 (cooling / heating medium temperature adjustment).

  On the other hand, when the second cleaning step 58 (both washing) is performed, the first fluid 14 as the cooling / heating medium is not discharged in the stage 102 (cooling / heating medium exchange in the casing). At this time, the raw material liquid remains in the microchannel 34.

  In the stage 110 (in-chip cleaning), the control means (not shown) operates the ultrasonic vibrator 52 to clean the inside of the micro flow path 34 with the ultrasonic wave and the raw material liquid. At this time, the first three-way valve 28 and the second three-way valve 38 are opened to the supply tank 20 side, and the third three-way valve 40 is opened to the waste liquid tank 48 side by a control means (not shown) and opened and closed. The valve 46 is in a closed state. Then, in the stage 110a (cleaning waste liquid discharge), the control means (not shown) opens the on-off valve 46 and operates the liquid feed pump 24, thereby causing the raw material liquid used for cleaning in the micro flow path 54 and the micro liquid by cleaning. Deposits peeled off from the inner wall of the flow path 34 are discharged to a waste liquid tank 48. After the discharge, the on-off valve 46 is closed and the third three-way valve 40 is opened to the receiving tank 44 side to proceed to the stage 123 (production restart).

  In the present embodiment, the first fluid 14 is used for adjusting the temperature of the microchannel 34 in the manufacturing process, and the second fluid 16 is used for the cleaning process and the drying process. However, the first fluid 14 is used for the cleaning process and the drying process. If the fluid supply / discharge means 18 can be used in the process, the fluid supply / discharge means 18 performs a mutual operation between the state in which the fluid (first fluid 14) is supplied into the housing 12 and the state in which the fluid is discharged. It may be configured to be switchable between. In the present embodiment, since the manufacturing process is performed under atmospheric pressure, the pressure in the housing 12 and the microchannel 34 when the vacuum pump 50 is operated is not particularly limited as long as the atmospheric pressure is equal to or lower than the atmospheric pressure. In this embodiment, the first fluid 14 is heated by heating means (not shown) to heat the micro flow path 34. However, a direct microwave oscillator (not shown) operated by the control means (not shown) is used. You may attach directly to the chip | tip 32, and you may heat the 2nd fluid 16 at the time of washing | cleaning, and may adjust it to the optimal temperature for washing | cleaning.

  As described above, according to the microchannel cleaning system 10 and the cleaning method according to the present embodiment, first, the chip 32 (microreactor) having the microchannel 34 has a fluid (first The first fluid 14 and the second fluid 16) are disposed in the housing 12 in a state of being immersed in the fluid. In this state, even if the microchannel 34 is opened to the fluid side, the fluid hardly flows into the microchannel 34. However, by depressurizing the housing 12 and the inside of the housing 12 that hermetically seals the fluid, air dissolved in the raw material liquid can be precipitated, and bubbles can be generated in the microchannel 34. Furthermore, since the kinetic energy is given to the bubbles by irradiating the micro flow path 34 with ultrasonic waves, the bubbles are discharged out of the micro flow path 34. Therefore, the fluid enters the microchannel 34 instead of the released bubbles. Thereby, the wall surface of the micro flow path 34 is cleaned by the fluid and the irradiated ultrasonic wave. Since the bubbles are generated in the entire area of the micro flow path 34, the fluid that replaces the bubbles spreads over the entire micro flow path 34. Therefore, it is possible to efficiently clean the inside of the microchannel 34 by spreading the fluid over the entire microchannel 34. Since opening to the raw material liquid side (supply tank 20 side) and opening to the fluid side (inside the casing 12) can be switched to each other, it is not necessary to remove the casing 12 having the micro flow path 34. . Therefore, it is possible not only to avoid the work load such as the removal work of the housing 12, but also to perform the cleaning etc. in a fixed state, thereby suppressing the distortion of the micro flow path 34 and the change in the surface shape of the micro flow path. Thus, a product with a certain quality can be produced.

Secondly, by arranging a plurality of microchannels 34 in parallel, a desired product can be generated in parallel and the generation efficiency can be increased.
Thirdly, the inside of the micro flow path 34 that opens the flow path to the housing 12 can be decompressed by depressurizing the inside of the housing 12. Therefore, it is possible to evaporate the fluid remaining in the microchannel 34, and thereby the inside of the microchannel 34 can be dried. Therefore, generation | occurrence | production of a drying nonuniformity can be suppressed and a drying operation can be performed efficiently.

  Fourth, it is possible to evaporate the fluid remaining in the microchannel 34 by blocking the microchannel 34 from the housing 12 side and heating the fluid that immerses the microchannel 34. The inside of the microchannel 34 can be dried. Therefore, since the decompression in the housing 12 is unnecessary, the process can be simplified and the cost can be suppressed.

  Fifth, since the microchannel 34 is cleaned using the second fluid, a fluid having a high cleaning effect and a high drying effect can be used at the time of cleaning, and the microchannel 34 is efficiently cleaned. It can be performed.

  The present invention can be used as a microchannel cleaning system and a cleaning method capable of reliably cleaning the microchannel without damaging the microchannel.

DESCRIPTION OF SYMBOLS 10 ......... Cleaning system, 12 ......... Case, 12a ......... Supply port, 12b ......... Supply port, 12c ...... Discharge port, 14 ...... First fluid, 16 ......... Second 18 ......... Fluid supply / discharge means, 20 ......... Supply tank, 22 ......... Piping, 24 ......... Feed pump, 26 ......... Piping, 28 ......... First three-way valve, 28a ......... Opening, 30 ......... Piping, 32 ......... Chip, 34 ......... Microchannel, 36 ......... Piping, 38 ......... Second three-way valve, 38a ......... Opening, 39 ......... Piping, 40 ...... Third three-way valve, 42 ......... Piping, 43 ......... Piping, 44 ......... Receiving tank, 46 ......... On-off valve, 48 ......... Waste liquid tank, 50 ... ...... Vacuum pump, 50a ......... Pressure gauge, 52 ......... Ultrasonic vibrator, 56 ......... First cleaning step, 58 ......... Second cleaning step, 60 ... First drying step, 62 ......... second drying step.

Claims (10)

A micro-channel that is formed at a merging position of a plurality of paths through which the raw material liquid is circulated, and generates a desired product from the raw material liquid in a state of being immersed together with the path in a fluid supplied in a housing;
A switching valve interposed on the path immersed in the fluid, one connected to the micro-channel side, and the other connected to be switchable between the fluid side and the flow side of the raw material liquid;
Decompression means for decompressing the inside of the housing to generate bubbles in the microchannel;
An ultrasonic transducer that emits the bubbles to the outside of the microchannel while irradiating the microchannel with ultrasonic waves to clean the inside of the microchannel;
Controlling the switching of the switching valve to the fluid side at the time of cleaning the micro flow path, and a control means for operating the ultrasonic transducer and the pressure reducing means, and allowing the micro flow path to be cleaned in place A microchannel cleaning system characterized by the above.   The microchannel cleaning system according to claim 1, wherein a plurality of the microchannels are arranged in the casing and connected in parallel to each other. A fluid supply / discharge means connected to the housing and capable of switching between a state in which the fluid is supplied to the housing and a state in which the supplied fluid is discharged;
The micro flow path cleaning system according to claim 1, wherein the control unit performs switching control of the fluid supply / discharge unit. The case has a heating means for heating the fluid supplied to the case,
3. The microchannel according to claim 1, wherein the control unit performs switching control of the connection of the three-way valve to the fluid side after the cleaning, and performs control for operating the heating unit for a predetermined time. Cleaning system. The fluid supply / discharge means includes a state in which the first fluid is supplied to the housing, a state in which the first fluid is discharged and a second fluid is supplied, and a state in which the second fluid is discharged, Can be switched in order,
The control means supplies the first fluid when the raw material liquid is passed through the fluid supply / discharge means, supplies the second fluid at the time of the cleaning, and discharges the second fluid after the cleaning. The microchannel cleaning system according to any one of claims 1 to 4, wherein control is performed. A micro-channel that is formed at a joining position of a plurality of paths through which the raw material liquid flows and that generates a desired product from the raw material liquid in a state of being immersed in a fluid supplied in the housing, to the flow side of the raw material liquid And the connection to the fluid side can be alternately switched,
Switch the connection of the microchannel to the fluid side and depressurize the housing to generate bubbles in the microchannel,
A microchannel characterized in that the microchannel is subjected to stationary cleaning by irradiating the microchannel with ultrasonic waves to discharge the bubbles outside the microchannel while cleaning the inside of the microchannel. Cleaning method.   The method for cleaning a microchannel according to claim 6, wherein a plurality of the microchannels are arranged in the housing and connected in parallel to each other.   The method for cleaning a microchannel according to claim 6 or 7, wherein after cleaning the inside of the microchannel, the fluid supplied to the casing is discharged and the inside of the casing is decompressed.   The method for cleaning a microchannel according to claim 6 or 7, wherein after the microchannel is cleaned, the fluid supplied to the housing is heated after the microchannel is switched to the distribution side. . 6. The second fluid for discharging the fluid from the housing and cleaning the microchannel when the microchannel is cleaned is supplied, and the second fluid is discharged after cleaning. The method for cleaning a microchannel according to any one of items 1 to 9.

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