JP2006272268A - Method of cleaning microchemical device - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To remove fouling in a micro passage efficiently during operation or stopping of a unit operation or reaction operations. <P>SOLUTION: A cleaning method is for a microchemical device 30 which causes two raw-material fluids A and B to pass through fluid supplying passages 34A and 34B, respectively, and join in a single micro passage 32 of an equivalent diameter of ≤1 mm and carries out reaction operations or a unit operation. The method comprises causing a cleaning fluid to pass through the micro passage 32 to generate a laminar flow vortex within the micro passage 32 so as to clean the micro passage 32. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a cleaning method for a microchemical device, and more particularly, to a cleaning method for a microchemical device in which a reaction operation or a unit operation is performed using a plurality of raw material fluids in a fine microchannel having an equivalent diameter of 1 mm or less. .

  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. It is. This microreactor utilizes the phenomenon that the flow of the reaction fluid becomes laminar in the microspace, and actively forms a wide reaction interface to make the reaction and mixing between fluids more efficient or faster. In recent years, it has been attracting attention as an innovative technology that can be integrated into the market. As this microreactor, a precise reaction / mixing system for a chemical solution or the like using a microchannel formed by a microfabrication technique such as etching has been proposed.

  However, the reaction and mixing in such a micro space and the product resulting therefrom are settled, adsorbed or crystallized in the micro channel, and the micro channel is likely to be contaminated. Due to the fouling, the raw material throughput and metering accuracy cannot be maintained, and the advantages of the microreactor are impaired.

  As means for solving this, conventionally, it is a general chemical apparatus cleaning method: 1) physical cleaning method (use of shearing force of flow, use of friction with solids), 2) chemical cleaning ( Use of chemical reaction, use of dissolving power) is used. Furthermore, when performing a cleaning operation of the microchemical device, the microchemical device is often disassembled and manually performed.

Patent Document 1 discloses a microreactor cleaning method. This microreactor is provided with a valve and a throttle means upstream or downstream of the microreactor. A method has been proposed in which the inside of the microchannel is pressurized to a predetermined pressure that is equal to or lower than the pressure limit of the channel by closing the valve and the throttle means, and then the pressure is removed and washed. By this method, it is said that the contamination in the microchannel can be removed by the shearing force on the inner wall surface of the microchannel, which accompanies a rapid change in the flow velocity.
JP 2005-501696 A

  However, the microchannel formed in the microchemical device often has a complicated structure or shape because an operation for introducing and joining a plurality of fluids or an operation for separating them is performed. FIG. 11 is a conceptual diagram showing a conventional Y-shaped channel 1. As shown in FIG. 11, in particular, the contamination 2 tends to remain in a portion where the flow velocity is slow, a branch portion of the flow path, an inner wall surface, or the like. For this reason, for example, there is a problem that it is difficult to remove the polluted stagnant by simply pressurizing the microchannel in a state where the reaction fluid is circulated to increase the flow velocity.

  In addition, the operation of the microchemical apparatus is stopped every time manual cleaning is performed, and the microchemical apparatus is disassembled, cleaned, assembled, and the like, so that the operation time of the operation for performing the unit operation or the reaction operation is reduced. Furthermore, there is a problem that manual cleaning causes an increase in labor.

  The present invention has been made in view of such circumstances, and a cleaning method for a microchemical apparatus that can efficiently remove contamination in a microchannel even during an operation in which a unit operation or a reaction operation is performed. The purpose is to provide.

  In order to solve the above-described problems, the present invention provides a micro operation in which a reaction operation or a unit operation is performed by merging a plurality of types of raw material fluids into one micro flow channel having an equivalent diameter of 1 mm or less through each fluid supply channel. In a cleaning method for a chemical device, there is provided a cleaning method for a micro chemical device, characterized in that a cleaning fluid is circulated through the microchannel, and a laminar vortex is generated in the microchannel to clean the microchannel. provide.

  In the present invention, the laminar flow vortex is preferably a vortex generated in a laminar flow region or a flow in a transition region from laminar flow to turbulent flow.

  According to the present invention, when the cleaning fluid flows in a laminar flow in the microchannel, the cleaning fluid C is disturbed by a vortex or the like while maintaining a certain degree of order in the vicinity of the inner wall of the microchannel. A laminar flow vortex (for example, Karman vortex) is generated. This laminar flow vortex causes an effect on the inner wall surface of the micro flow path, and produces an effect of knocking out the fouling attached to the inner wall surface of the micro flow path. Therefore, the contamination in the microchannel is efficiently removed by the laminar vortex.

  The present invention also relates to a cleaning method for a microchemical apparatus in which a plurality of types of raw material fluids are joined to one microchannel having an equivalent diameter of 1 mm or less through each fluid supply path to perform a reaction operation or a unit operation. The cleaning fluid is circulated through the micro-channel, and an air supply means is provided upstream of the micro-channel, and the cleaning fluid circulated in the micro-channel is made to contain gas so as to clean the micro-channel. A method for cleaning a microchemical device is provided.

  According to the present invention, the cleaning fluid and the gas circulated in the microchannel form a bubble flow with an appropriate flow rate ratio, and the bubbles pass while contacting the inner wall surface of the microchannel. As a result, the cleaning fluid in the vicinity of the wall surface is vibrated to improve the cleaning performance. Examples of the gas include an inert gas such as air and nitrogen, but other types of gases may be used as long as they react with the cleaning fluid and do not deteriorate the cleaning performance. Moreover, the gas which does not inhibit reaction of raw material fluid is preferable.

  In the present invention, it is preferable that the cleaning fluid generates a laminar vortex. As described above, since the cleaning fluid circulates by generating a laminar vortex while forming an interface due to the surface tension between the gas and the liquid, more vibration can be applied to the inner wall surface of the microchannel. Therefore, the microchannel can be efficiently cleaned.

  In the present invention, it is preferable that vibration applying means is provided in the microchemical device to apply vibration to the microchannel. As a result, a cavitation effect is generated in the microchannel, and the contamination can be removed by applying vibration to the inner wall surface of the microchannel. The vibration frequency is preferably 1 kHz to 10 MHz, more preferably 1 kHz to 1 MHz, and further preferably 20 kHz to 200 kHz. That is, it is preferable to use high frequency and ultrasonic bands. The output of vibration is preferably 1 W to 10 kW, more preferably 10 W to 5 kW, and even more preferably 100 W to 2 kW.

  In the present invention, it is preferable to apply ultrasonic waves to the cleaning fluid in the microchannel. By this method, a phenomenon such as a very small bubble or cavity being rapidly formed or severely broken in the microchannel, that is, a cavitation effect is generated. Therefore, it is possible to apply vibration to the inner wall surface of the micro flow path to scratch out the dirt. The vibration frequency and output are the same as described above.

  In the present invention, it is preferable that pressure control means is provided downstream of the microchannel, and the pressure is removed after applying a pressure of a predetermined value or more to the cleaning fluid in the microchannel.

  In this way, the flow path is blocked by the pressure control means provided on the downstream side of the micro flow path in a state where the cleaning fluid is flowing through the micro flow path, so that the inside of the micro flow path is pressurized. . Thereafter, at the moment when the pressure in the micro flow path is released by the pressure control means, the compressed gas in the cleaning fluid is discharged to the downstream side while expanding. At this time, the flow rate of the cleaning fluid increases, and the contamination in the microchannel can be efficiently removed.

  Moreover, in this invention, it is preferable to provide the step which distribute | circulates the said cleaning fluid to the said micro flow path, and the step which stops the distribution | circulation to the said micro flow path of the said cleaning fluid.

  Thus, by stopping the flow of the cleaning fluid, the contamination in the microchannel is diffused into the cleaning fluid while the microchannel is filled with the cleaning fluid, so that the cleaning performance is improved.

  Moreover, in this invention, it is preferable to provide the step which distribute | circulates the said cleaning fluid from the one end side of the said microchannel, and the step which distribute | circulates the said cleaning fluid from the other end side of the said microchannel. As described above, the contamination staying in the flow channel branching portion or corner portion in the micro flow channel can be removed by reversing the direction in which the cleaning fluid is circulated.

  In the present invention, it is preferable that a temperature adjusting means is provided in the microchemical device to heat the cleaning fluid in the microchannel. Thus, heating the cleaning fluid in the microchannel increases the rate at which the contamination in the microchannel diffuses into the cleaning fluid. Therefore, the inside of the microchannel can be cleaned efficiently.

  Further, in the present invention, a cleaning method for circulating a plurality of types of the cleaning fluid in the microchannel, wherein the last cleaning fluid to be circulated in the microchannel is subjected to a reaction operation or a unit operation in the microchannel. Preferably, the fluid does not hinder. Thereby, during the reaction operation or unit operation, the reaction or mixing is not hindered by the remaining washing fluid, so that a desired product can be obtained.

  In the present invention, it is preferable that the microfluidic channel is filled with the cleaning fluid and a predetermined time elapses, and then the cleaning fluid is discharged from the microchannel. As described above, by filling the microchannel with the cleaning fluid after the operation, it is possible to suppress drying with the contamination remaining in the microchannel. Furthermore, since the contamination in the microchannel can be diffused into the cleaning fluid, the cleaning performance is improved.

  In the present invention, the unit operation includes mixing, separation, classification, filtration, heating, cooling, heat exchange, extraction, crystallization, dissolution, evaporation, distillation, absorption, adsorption, and the reaction operation includes an inorganic substance or Ion reaction, redox reaction, electrolytic reaction, nitrification reaction, combustion reaction, combustion reaction, roasting reaction, halogenation reaction, sulfonation reaction, alkylation reaction, esterification reaction, fermentation reaction, heat for organic substances It preferably includes a reaction, a catalytic reaction, a radical reaction, and a polymerization reaction.

  In the present invention, it is preferable to introduce the washing method during the unit operation or the reaction operation. In this way, during the reaction operation or unit operation, when clogging due to precipitation or aggregation occurs in the microchannel, it is possible to immediately switch to the washing step. Therefore, waste of the raw material fluid can be suppressed.

  In the present invention, it is preferable that the cleaning fluid is circulated through the microchannel a plurality of times. In this way, it is possible to remove the contamination in the microchannel that cannot be removed by one circulation.

  As described above, according to the present invention, it is possible to efficiently remove the contamination in the micro flow channel during operation or during stoppage.

  Hereinafter, preferred embodiments of a cleaning method for a microchemical apparatus according to the present invention will be described in detail with reference to the accompanying drawings. FIG. 1 is a perspective view of a flaky flow type microchemical device main body 30, and FIG. 2 is a top view of the flaky flow type microchemical device main body 30 and a cross-sectional view taken along line F-F ′.

  First, the details of the flaky flow type microchemical device main body 30 of FIGS. As shown in FIGS. 1 and 2, the flaky flow type microchemical device main body 30 has a micro flow channel 32 for reacting two kinds of raw material fluids, and two kinds of raw material fluids are joined to the micro flow channel 32. A Y-shaped flow path including two fluid supply paths 34A and 34B is formed. In addition, inlets 36 and 37 for introducing two kinds of raw material fluids are formed at the upstream ends of the two fluid supply paths 34A and 34B, respectively. In addition, an outlet 38 is formed at the downstream end of the microchannel 32 to allow the product obtained by the reaction to flow out.

  The micro channel 32 is a micro channel having a circular cross section. The equivalent diameter of the cross section of the microchannel 32 is preferably 1 mm or less, and more preferably 500 μm or less. In addition to the circular shape, a rectangular shape, a trapezoidal shape, a semicircular shape, or the like can be adopted as the cross-sectional shape.

  As a material of the member constituting the microchemical device main body 30, a material having high strength, corrosion prevention, and high fluidity of the raw material fluid is preferable. For example, metal (iron, aluminum, stainless steel, titanium, other various metals), resin (fluorine resin, acrylic resin, etc.), glass (quartz etc.), ceramics (silicon etc.), etc. can be preferably used.

  A microfabrication technique is applied to manufacture the microchemical device main body 30. The microchemical device main body 30 in FIG. 3 covers a flat lid member 33 on a main body member 31 on which a micro flow path 32, fluid supply paths 34A and 34B, inlets 36 and 37, and an outlet 38 are formed. To be manufactured. Examples of applicable microfabrication techniques include the following.

(1) LIGA technology combining X-ray lithography and electroplating (2) High aspect ratio photolithography using EPON SU8 (3) Mechanical micro cutting (4) High aspect ratio processing of silicon by deep RIE ( 5) Hot Emboss processing method (6) Stereolithography method (7) Laser processing method (8) Ion beam processing method The joining method of the main body member 31 and the lid member 33 is Y-shaped by material alteration or deformation by high temperature heating. A precise method that maintains the dimensional accuracy without breaking the flow path is desirable, and solid phase bonding (for example, pressure bonding or diffusion bonding) or liquid phase bonding (for example, welding, eutectic bonding, Soldering, bonding, etc.) are preferably selected. For example, when silicon is used as the material, silicon direct bonding for bonding silicon, fusion bonding for bonding glasses, anodic bonding for bonding silicon and glass, diffusion bonding for bonding metals, and the like can be given. For bonding ceramics, bonding techniques other than mechanical sealing techniques such as metals are required. A bonding agent called glass solder is printed on alumina to a film thickness of about 80 μm without applying pressure. There is a method of heat treatment at 440-500 ° C. Further, as new technologies, there are surface activated bonding, direct bonding using hydrogen bonding, bonding using HF (hydrogen fluoride) aqueous solution, and the like.

  The raw material fluid in the microchemical device 30 is a fluid necessary for obtaining a product. The liquid, gas, a solid-liquid mixture in which solid fine particles are dispersed in the liquid, or the gas does not dissolve in the liquid. This refers to a dispersed gas-liquid mixture. In addition, when there are two or more types of fluids, not only when the type of fluid, chemical composition, surface tension, specific gravity, viscosity, etc. are different, but also for example, conditions such as temperature, gas-liquid ratio, and solid-liquid ratio may be different. , Contained in the raw fluid.

  Further, in the present invention, the fluid supply means is disposed in each of the pipes upstream or downstream of the microchemical apparatus 30. Specific examples of the fluid supply means include a liquid feed pump and an air pump. However, any other supply means may be used as long as it has a drive function of supplying fluid in a laminar flow.

  In the present invention, the cleaning fluid is a fluid that removes contaminants in the microchannel.

  The cleaning fluid is a liquid, gas, a solid-liquid mixture in which solid fine particles are dispersed in a solid, a solid-gas mixture in which solid fine particles are dispersed in a gas, or a gas in which a gas is not dissolved but dispersed in a liquid. Refers to liquid mixture. In addition, when there are two or more types of fluid, not only when the type of fluid, chemical composition, surface tension, specific gravity, viscosity, etc. are different, but also when, for example, the temperature, gas-liquid ratio, solid-liquid ratio, etc. are different, Included in cleaning fluid.

  Specific examples of the cleaning fluid depend on the type of fouling, and examples thereof include water, an aqueous surfactant solution, alcohols such as methanol and ethanol, benzene and acetone.

  In the present invention, the fluid supply means for generating the pulsating flow alternately performs the flow and stop of the cleaning fluid. For example, a pulsating flow pump may be used, but it may have a function of generating the pulsating flow. Other means may be used.

  In the present invention, the air supply means supplies gas, and examples thereof include an air pump, but other means may be used as long as it has a function of supplying gas.

  Further, in the present invention, the vibration applying means applies vibration to the cleaning fluid in the microchannel, and examples thereof include an ultrasonic vibrator, but other means as long as it has a function of vibrating. But you can.

  In the present invention, the pressure control means is provided in a part of the flow path and pressurizes the micro flow path or the cleaning fluid in the micro flow path. For example, a pressure reducing valve, a back pressure valve, a solenoid valve, a valve, Examples include dampers. However, other means may be used as long as it has a function of pressurizing the cleaning fluid in the flow path.

  In the present invention, the temperature adjusting means may be a constant temperature circulation tank using hot water or oil, various heaters, a hot air generator, etc., but other means as long as it has a function of controlling or adjusting temperature. But you can.

  Hereinafter, a preferred embodiment of a method for cleaning a microchemical apparatus according to the present invention will be described in detail.

  3-6 is a figure which shows the washing | cleaning method in the flaky flow type microchemical apparatus main body 30 of this invention. In addition, in each figure, the part which shows the same code | symbol as FIGS. 1-2 shall have the same thing or function.

  A first embodiment of the present invention will be described. In this embodiment, in the flaky flow type microchemical device main body 30 of FIG. 3, a cleaning fluid is circulated through the microchannel 32 and laminar vortices are generated in the microchannel 32 to perform cleaning. First, as shown in FIG. 3, the piping 18 and the piping 20 are circulated from the cleaning fluid storage unit 12 through a fluid supply unit (not shown) that generates the cleaning fluid C in a pulsating manner (for example, a pulsating pump). Then, the fluid is supplied to the micro flow path 32 from the fluid supply paths 34A and 34B. At this time, the cleaning fluid C is supplied so as to flow through the microchannel 32 in a laminar flow. In such a laminar flow, in the vicinity of the inner wall of the microchannel 32, the cleaning fluid C is turbulent, such as a vortex, while maintaining a certain degree of order, and a periodic laminar vortex (for example, Karman vortex) (It is thought that a fluid is dragged on the surface of the obstacle in the flow, and thereby a difference in pressure between the vicinity of the obstacle and the other portion is generated, and a vortex is generated). Moreover, when supplying by pulsating flow, since the pulsating flow of the cleaning fluid disturbs the laminar flow as an external force, a laminar vortex is generated as described above. This laminar flow vortex causes the inner wall surface of the microchannel 32 to sway, and has the effect of knocking out the dirt adhering to the inner wall surface of the microchannel, so that the contamination in the microchannel 32 can be removed.

  A second embodiment of the present invention will be described. This embodiment is a method of bubbling and cleaning the inside of the microchannel 32 by including the gas 4 in the cleaning fluid C in the flaky flow type microchemical device main body 30 of FIG. As shown in FIG. 4, the configuration for realizing this method is that a gas is provided between a fluid supply means (not shown) for generating a pulsating flow (for example, a pulsating pump) and the inlets 36 and 37 of the microchannel 32. 4 is the same as that of the first embodiment except that air supply means (for example, an air pump) 11 for injecting 4 and pipes 28A and 28B for connecting the air supply means 11, the pipe 18, and the pipe 20 are provided. is there.

  As shown in FIG. 4, first, the cleaning fluid C is circulated through the pipes 18 and 20 via a fluid supply unit (not shown) (for example, a pulsating pump) that generates a pulsating flow from the cleaning fluid storage unit 12. Then, the gas 4 is mixed into the cleaning fluid C flowing into the pipes 18 and 20 from the air supply means 11 through the pipes 28A and 28B. The cleaning fluid D mixed with the gas 4 is circulated to the micro flow path 32 through the fluid supply paths 34A and 34B. Thereby, the cleaning fluid D forms a segmented flow in the microchannel 32. Since this segmented flow flows on the inner wall surface of the microchannel while forming an interface due to the surface tension of the gas 4 and the liquid, the segmented flow is periodically vibrated on the inner wall surface of the microchannel. Thus, the contamination in the microchannel 32 is removed.

  A third embodiment of the present invention will be described. In this embodiment, in the flaky flow type microchemical device main body 30 of FIG. 5, the inside of the microchannel 32 is cleaned by applying and removing a predetermined pressure to the cleaning fluid D in the microchannel 32. It is a method to do.

  The configuration for realizing this method is the same as that of the second embodiment except that a pressure control means 13 is provided downstream of the microchannel 32 as shown in FIG. As shown in FIG. 5A, first, the cleaning fluid D in which the gas 4 is mixed by the air supply means 11 is circulated to the micro flow path 32 through the fluid supply paths 34A and 34B. Next, as shown in FIG. 5B, the pressure control means 13 (for example, a back pressure valve or the like) is operated while the cleaning fluid D is circulated through the micro flow path 32, and the flow path on the downstream side of the micro flow path 32. Close. Thereby, the cleaning fluid D mixed with the gas 4 in the microchannel 32 is pressurized. Next, after applying a pressure equal to or higher than a predetermined pressure value equal to or lower than the pressure resistance value of the microchannel 32, the pressure control means 13 is operated as shown in FIG. The path is opened, and the pressure in the microchannel 32 is released at once. As a result, the gas 4 mixed in the cleaning fluid D is caused to flow downstream of the microchannel 32 while expanding. At this time, since the flow rate of the cleaning fluid D flowing in the micro flow path 32 is increased, the contamination in the micro flow path 32 can be efficiently removed.

  A fourth embodiment of the present invention will be described. In this embodiment, in the flaky flow type microchemical device main body 30 of FIG. 6, the cleaning fluid C is circulated through the microchannel 32 in the forward direction and the reverse direction, and the inside of the microchannel 32 is cleaned. . As shown in FIG. 6 (A), first, the cleaning fluid C is circulated through the micro flow channel 32 through the fluid supply channels 34A and 34B (operation A). Next, as shown in FIG. 6B, the cleaning fluid C is circulated from the outlet 38 to the microchannel 32 in the direction opposite to that shown in FIG. 6A (operation B). Thereafter, operation A and operation B are alternately performed again. As a result, it is possible to efficiently remove the dirt accumulated in a portion that is difficult to remove by simply flowing the cleaning fluid C in one direction from the microchannel 32. Further, the cleaning fluid used in this cleaning method may be one in which the gas 4 is mixed.

  Next, the form of the microchemical apparatus different from FIGS.

  FIGS. 7A and 7B are perspective views of a cylindrical flow type microchemical device main body 40, which is an embodiment different from the flaky flow type microchemical device main body 30, and FIG. 8 is a cylindrical shape. FIG. 9 is a cross-sectional view of the vicinity of the micro flow path of the plate constituting the flow type microchemical device main body 40, and FIG. 9 is a partial perspective view showing the rib shape of the plate constituting the cylindrical flow type microchemical device main body 40; FIG. 10 is a partial perspective view showing the outflow side of the plate constituting the cylindrical flow type microchemical device main body 40.

  As shown in FIGS. 7A and 7B, the cylindrical flow type microchemical device main body 40 is a device that reacts or mixes by laminating three liquids in a concentric shape and mixing them simultaneously. The microchemical device main body 40 includes a plate 42, and a lid member 44 and a receiving member 46 that are disposed on the upstream side and the downstream side of the plate 42 and sandwich the plate 42. The lid member 44 and the plate 42 are integrated by connecting the convex portion 71 and the concave portion 73 of the lid member 44. In addition, screw holes 70, 72, and 74 are respectively formed so as to penetrate the receiving member 46, the plate 42, and the lid member 44. These screw holes 72, 74, 76 are integrated through the screw 76, and the cylindrical flow type microchemical device main body 40 is formed.

  The upstream side of the lid member 44 is provided with connectors 40A, 40B, and 40C to which three inflow pipes 48A, 48B, and 48C are detachably attached, and three kinds of raw material fluids A, B, and C flow in. Is done. The plate 42 is formed with a micro flow path 54 for laminating the fluid flowing out from the pipes 48A, 48B, and 48C in a concentric circle shape. The receiving member 46 is formed with a mixing flow channel 58 that simultaneously mixes or reacts the three liquids flowing out from the micro flow channel 54 to form a mixed fluid (product), and similarly, on the downstream side of the receiving member 46. In addition, an outflow tube 50 detachably attached to the connector is provided, and the product D is discharged.

  The lid member 44 is formed with lid member through holes 44A, 44B, and 44C into which fluids from the pipes 48A, 48B, and 48C flow, respectively.

  As shown in FIGS. 8 and 9, a plate through hole 42A communicating with the lid member through hole 44A is formed at the center of the plate 42. The inner diameter of the plate through hole 42A is a laminar flow through the plate through hole 42A. (That is, the Reynolds number is 2320 or less). Further, the lid member through hole 44A and the plate through hole 42A have the same diameter so that no step is generated between the lid member through hole 44A and the plate through hole 42A.

  The plate 42 includes a slit cylindrical through hole 42B formed in a slit shape around the plate through hole 42A, a radial flow path 43B communicating with the slit cylindrical through hole 42B and the lid member through hole 44B, Are formed, and the cross-sectional area of the radial flow path 43B is set so as not to become a bottleneck.

  Further, the plate 42 includes a thick short cylindrical recess 42C formed around the slit cylindrical through hole 42B, an outer layer through hole 41C communicating with the lid member through hole 44C, an outer layer through hole 41C and a thickness. A radial flow path 43C communicating with the thin short cylindrical recess 42C is formed. The radial flow path 43C is formed at a substantially symmetrical position with the radial flow path 43B, and the flow path cross-sectional area of the radial flow path 43C is set so as not to be a bottleneck.

  The plate through-hole 42A and the slit cylindrical through-hole 42B are separated by a thin short cylindrical inner partition plate 62, and the slit cylindrical through-hole 42B and the thick short cylindrical recess 42C are thin and short cylindrical. It is sectioned by a middle partition plate 64.

  The plate 42 includes a flow path wall forming portion 66 that forms the bottom of the thick short cylindrical recess 42C and the flow path wall on the outer peripheral side of the slit cylindrical through hole 42B. The plate portion 64 extends from the innermost side of the flow path wall forming portion 66 along the outflow direction.

  The length L of one side of the plate 42 is longer than 1.5 times the outer diameter D of the thick short cylindrical recess 42C. The plate 42 may be bonded after processing two plate members, or may be manufactured by cutting a single plate member.

  As shown in FIG. 8, the above-described mixing flow path 58 is formed in the receiving member 46, and fluids flowing out from the thick short cylindrical recess 42C, the slit cylindrical through hole 42B, and the plate through hole 42A, respectively. The reaction is mixed in the mixing channel 58. Further, on the upstream side of the receiving member 46, the cylindrical flow type microchemical device 40 is inserted into the thick-walled short cylindrical concave portion 42C when the cylindrical flow type microchemical device 40 is assembled. A ring-shaped raised portion 47 forming 45C is formed.

  As shown in FIG. 9, the slit cylindrical through hole 42B is provided with a plurality of ribs 68 that are continuous with the inner partition plate 64 and the flow path wall forming portion 66 and extend in the outflow direction. The ribs 68 are arranged so as to be substantially evenly spaced from each other, avoiding the space where the radial flow paths 43B and 43C are formed. Further, in the vicinity of the outlet of the slit cylindrical through hole 42B, the rib 68 is not provided in order to allow the fluid to flow out in a laminar flow in a circular tube shape.

  With the configuration described above, the fluid flowing through each of the outer layer flow path 45C, the slit cylindrical through hole 42B, and the plate through hole 42A flows in the same direction and in a laminar flow.

  As an example of the dimensions, as shown in FIG. 8, the diameter d of the plate through hole 42A is 500 μm, the flow path width (gap) W of the slit cylindrical through hole 42B is 100 μm, the thickness T of the plate 42 is 600 μm, and the rib 68 The wall thickness t (see FIG. 9) is 100 μm. In order to cause the three liquids to flow out from the plate 42 as a concentric laminar flow, the above dimensions may be changed as long as the Reynolds number is equal to or less than the critical Reynolds number (2320 in the case of a circular tube).

  Since the diffusion rate of the substance to be reacted is usually not so high, the longer the reaction time is required, the larger the diameters of the plate through hole 42A, the slit cylindrical through hole 42B, and the thick short cylindrical recess 42C. For this reason, it is preferable that these diameters are 1 mm or less. Further, in consideration of processing restrictions and the relationship between the flow resistance of the fluid to be flowed and the yield, these diameters are more preferably 1 μm or more.

    The material of the cylindrical flow type microchemical device 40 is the same as that of the thin piece flow type microchemical device body 30.

  Next, an operation method in which the second embodiment of the present invention is applied to the cylindrical flow type microchemical device body 40 will be described. First, before flowing the cleaning fluid C through the cylindrical flow type microchemical device main body 40, as shown in FIG. 4, the cleaning fluid C is made to contain a gas by the air supply means 11 (cleaning fluid D). Thereafter, as shown in FIGS. 7A and 7B, the cleaning fluid D is supplied to the plate through-hole 42A in the microchannel 54 from the inflow piping 48A, 48B, 48C on the upstream side of the lid member 44. The cylindrical through hole 42B and the thick short cylindrical recess 42C are circulated. Then, the three liquids that have been laminarized in the microchannel 54 flow through the mixing channel 58 and are discharged from the outlet 50 (cleaning fluid D '). At this time, while the cleaning fluid D is flowing through the micro flow channel 54 and the mixing flow channel 58, the cleaning fluid D is supplied in a pulsating flow. Thereby, in the vicinity of the inner walls of the micro flow path 54 and the mixing flow path 58, the cleaning fluid D is disturbed such as a vortex and a periodic laminar vortex (for example, Karman vortex) is generated. The laminar flow vortex causes the inner wall surfaces of the micro-channel 54 and the mixing channel 58 to sway, and the dirt adhering to the inner wall surface of the mixing channel 58 is knocked out, thereby efficiently cleaning the inside of the mixing channel 58. be able to. Further, since the cleaning fluid D flows on the inner wall surface of the mixing channel 58 while forming an interface due to the surface tension of the gas 4 and the liquid, the cleaning fluid D periodically vibrates on the inner wall surface of the mixing channel 58. Thus, the inside of the mixing channel 58 can be cleaned efficiently.

  In addition to the second embodiment of the present invention, a method of cleaning the mixing channel 58 by generating a laminar vortex in the mixing channel 58, or a predetermined pressure is applied to the cleaning fluid in the mixing channel 58. Is applied and the pressure is removed, and the mixing channel 58 is washed. The cleaning fluid is passed through the mixing channel 58 in the forward direction and the reverse direction, and the mixing channel 58 is washed. A method of cleaning by applying vibration to or applying ultrasonic waves, a method of filling the mixing channel 58 with the cleaning fluid and heating the mixing channel 58, and a method of cleaning the mixing channel 58 multiple times The method for cleaning a microchemical apparatus according to the present invention, such as a method for cleaning by circulation, can be applied.

[Example A]
In the following, as an example to which the microchemical apparatus cleaning method according to the present invention is applied, a silver halide dispersion solution having excellent monodispersibility is synthesized in the flaky flow type microchemical apparatus body 30, and then the flaky flow A case of cleaning the inside of the main body 30 of the type microchemical device will be described.

  A method for synthesizing a silver halide dispersion solution for a light-sensitive material is performed by bringing an aqueous silver nitrate solution (solution P) into contact with an aqueous halide salt solution (solution Q).

  The photosensitive silver halide in this example is not particularly limited as a halogen composition, and is silver chloride, silver chlorobromide, silver bromide, silver iodobromide, silver iodochlorobromide. Of these, silver bromide and silver iodobromide are preferred. The distribution of the halogen composition in the grains may be uniform, the halogen composition may be changed stepwise, or may be continuously changed. Further, silver halide grains having a core / shell structure can be preferably used. The structure of the silver halide grains is preferably a 2- to 5-fold structure, more preferably a 2- to 4-fold core / shell grain.

Moreover, the photosensitive silver halide grain can contain a metal or a metal complex of Group 8 to Group 10 of the Periodic Table (showing Groups 1 to 18). Rhodium, ruthenium, and iridium are preferred as the metal of Group 8 to Group 10 of the periodic table or the central metal of the metal complex. One kind of these metal complexes may be used, or two or more kinds of complexes of the same metal and different metals may be used in combination. The content of the metal complex is preferably in the range of 1 × 10 ⁻⁹ mol to 1 × 10 ⁻³ mol with ^respect to 1 mol of silver.

  Various gelatins can be used as the gelatin contained in the silver halide dispersion used in this example. In order to satisfactorily maintain the dispersion state of the photosensitive silver halide emulsion in the organic silver salt-containing coating solution, it is preferable to use low molecular weight gelatin having a molecular weight of 500 to 60,000.

  Next, a specific example of synthesizing a silver halide dispersion solution in the flaky flow type microchemical apparatus 30 will be described.

  First, 3.1 mL of a 1% by mass potassium bromide solution was added to 1421 mL of distilled water, and 3.5 mL of 0.5 mol / L sulfuric acid and 31.7 g of phthalated gelatin were added. While maintaining the temperature of this solution at 30 ° C., while stirring in a stainless steel reaction vessel, distilled water was added to 22.22 g of silver nitrate and diluted to 95.4 mL to obtain Solution A. Furthermore, Solution B, in which 15.3 g of potassium bromide and 0.8 g of potassium iodide were diluted with distilled water to a volume of 97.4 mL, was added to Solution A over a period of 45 seconds to prepare Solution C. .

  Thereafter, 10 mL of a 3.5 mass% aqueous hydrogen peroxide solution was added to Solution C, and 10.8 mL of a 10 mass% aqueous solution of benzimidazole was further added. Further, distilled water was added to 51.86 g of silver nitrate to dilute to 317.5 mL to obtain a solution P (silver nitrate aqueous solution). Further, 44.2 g of potassium bromide and 2.2 g of potassium iodide were diluted to a volume of 400 mL with distilled water to prepare a solution Q (an aqueous halide salt solution). Then, the entire amount of the solution P is circulated from the inlet 36 to the microchannel 32 over a period of about 20 minutes at a constant flow rate, and the solution Q is supplied from the inlet 37 to the microchannel 32 while maintaining pAg at 8.1. The mixture was circulated and mixed in the microchannel 32. In this way, a silver halide dispersion solution was synthesized.

  As described above, a silver halide dispersion solution can be synthesized by bringing a silver nitrate aqueous solution (solution P) and a salt halide aqueous solution (solution Q) into contact in the flaky flow type microchemical device body 30. .

  Next, a method for evaluating the cleaning property when the cleaning method for the microchemical apparatus according to the present invention is applied after the operation of synthesizing the silver halide dispersion is stopped will be described.

  After synthesizing the silver halide dispersion, the cleaning fluid is circulated from the fluid supply paths 36 and 37 to the microchannel 32 and the transparency of the cleaning fluid discharged from the outlet 38 of the microchannel 32 is measured. Thus, the cleaning property was evaluated. As a specific method, first, the cleaning fluid discharged from the outlet 38 was sampled. Next, the absorbance of the cleaning fluid sampled by the spectrophotometer was measured, and the time when the detection limit was reached was defined as the cleaning completion time. In addition, after the cleaning of the microchemical device main body 30 was finished, the microchemical device main body 30 was disassembled, and the cleaning performance was visually evaluated.

(Example 1) When performing pulsating washing After synthesizing a silver halide dispersion solution, using a single diaphragm pump (manufactured by Takumina Co., Ltd.) that generates pulsating flow, room temperature (about 20 ° C) Distilled water was circulated from the fluid supply paths 36 and 37 to the microchannel 32 at a flow rate of 100 mL / min. At this time, it was confirmed that the cleaning fluid was circulating in the microchannel while forming a laminar vortex. Thereafter, the cleaning fluid discharged from the outlet 38 of the microchannel 32 was sampled, and the absorbance was measured using a spectrophotometer. And it was 3 to 4 minutes when the cleaning completion time until the light absorbency of the sampled cleaning fluid reached the detection limit was measured. Thereafter, as a result of disassembling and observing the microchemical device main body 30, it was confirmed that the fouling in the microchannel 32 was almost completely removed and the cleaning property was high.

(Comparative Example 1) When no pulsating washing is performed After synthesizing a silver halide dispersion solution, a triple plunger pump (manufactured by Fuji Techno Industry Co., Ltd.) with little pulsating flow is used, and room temperature (about 20 ° C) distilled water was circulated from the fluid supply paths 36 and 37 to the microchannel 32 at a flow rate of 100 mL / min. At this time, a laminar vortex due to the cleaning fluid was not generated in the microchannel 32. Thereafter, the cleaning fluid discharged from the outlet 38 of the microchannel 32 was sampled, and the absorbance was measured using a spectrophotometer. And it was 5 to 6 minutes when the cleaning completion time until the absorbance of the sampled cleaning fluid reached the detection limit was measured. Then, as a result of disassembling and observing the microchemical device main body 30, it was confirmed that the contamination in the micro flow 32 path remained.

[Example B]
Next, as another example to which the method for cleaning a microchemical device according to the present invention is applied, a pigment fine particle dispersion excellent in monodispersibility is synthesized in a cylindrical flow type microchemical device body 40 and then cylindrical. A case where the flow type microchemical device main body 40 is cleaned will be described.

  The pigment fine particle dispersion is synthesized by bringing the three solutions P and Q and the functional solution R into contact with each other.

  Next, a specific example of synthesizing the pigment fine particle dispersion in the cylindrical flow type microchemical device main body 40 will be described.

  Solution P was prepared by mixing dimethyl sulfoxide (DMSO), PVP as a polymer, 0.8 mol KOH as an alkaline agent, and Pigment Red as a pigment. The pigment concentration at this time was 1.0 wt%.

  Solution Q was prepared by mixing water and W-136 (manufactured by Sankyo Chemical Co., Ltd.) as a surfactant. The surfactant concentration at this time was 0.84 wt%.

  The functional liquid R was prepared by mixing sulfoxide (DMSO), 0.8 mol KOH as an alkali agent, and PVP as a polymer.

  The solution P, Q and the functional solution R are supplied from the pipes 48A, 48C, 48B for the inflow of the cylindrical flow type microchemical device main body 40 to the plate through hole 42A, the thick short cylinder in the microchannel 54. A concentric circle three-layer structure (see FIG. 10) in which a functional layer of the functional solution R is sandwiched between the raw material solutions P and Q is circulated through the cylindrical recess 42C and the cylindrical through-hole 42B. Circulated. In this three-layer structure, the central layer is the solution P, the outer layer is the solution Q, and the intermediate layer is the functional solution R.

  At this time, the flow rate of the solution P forming the central layer is 1 mL / hour, the flow rate of the solution Q forming the outer layer is 48 mL / hour, and the flow rate of the functional solution R forming the intermediate layer is 0.2 mL / hour. Thus, the solutions P and Q and the functional solution R were circulated in the micro flow channel 54 and the mixing flow channel 58. In this way, the pigment fine particle dispersion was synthesized in the mixing flow path 58 and continuously manufactured for 7 hours.

  Further, after the operation of synthesizing the pigment fine particle dispersion is stopped, the cleaning property evaluation method when the cleaning method of the microchemical device according to the present invention is applied is the same as that of the above-described silver halide dispersion solution. Went to.

(Example 1) Washing with a cleaning solution mixed with bubbles First, a cleaning solution was prepared such that dimethyl sulfoxide (DMSO) and water had a volume ratio of 90:10. After synthesizing the pigment fine particle dispersion, the cleaning solution was added at a flow rate of 0.5 mL / min while mixing air at a flow rate of 0.05 mL / min at room temperature (about 20 ° C.). Then, the plate was passed through the plate through hole 42A, the thick short cylindrical recess 42C, the cylindrical through hole 42B, and the mixing channel 58 in the micro channel 54.

  At this time, it was confirmed that bubbles in the cleaning solution formed a segmented flow in the microchannel 54 and the mixing channel 58 in the microchannel 54 and the mixing channel 58. Thereafter, the cleaning fluid discharged from the cylindrical flow type microchemical device main body 40 was sampled, and the absorbance was measured using a spectrophotometer. Then, when the cleaning completion time until the absorbance of the sampled cleaning fluid reached the detection limit was measured, it was 15 minutes. Then, as a result of disassembling and observing the cylindrical flow type microchemical device main body 40, it was confirmed that the contamination in the mixing channel 58 was almost removed.

(Example 2) Washing solution containing bubbles and washing with ultrasonic waves First, dimethylsulfoxide (DMSO) and water were adjusted to a volume ratio of 90:10. After the pigment fine particle dispersion was synthesized, the cleaning solution was mixed at a flow rate of 0.5 mL / min at room temperature (about 20 ° C.) while air was mixed into the cleaning solution at a flow rate of 0.05 mL / min. The micro-channels 54 were passed through the plate through-holes 42 </ b> A, the thick short cylindrical recesses 42 </ b> C, the cylindrical through-holes 42 </ b> B, and the mixing channel 58. During this time, the cylindrical flow type microchemical device 40 was placed in an ultrasonic cleaner (manufactured by Branson), and vibration was applied to the cylindrical flow type microchemical device 40 under conditions of an output of 320 W and a frequency of 44 kHz.

  At this time, it was confirmed that the bubbles in the cleaning solution were in random contact with the inner wall surfaces of the microchannel 54 and the mixing channel 58 in the microchannel 54 and the mixing channel 58. Thereafter, the cleaning fluid discharged from the cylindrical flow type microchemical device main body 40 was sampled, and the absorbance was measured using a spectrophotometer. And it was 5 to 6 minutes when the cleaning completion time until the absorbance of the sampled cleaning fluid reached the detection limit was measured. Thereafter, as a result of disassembling and observing the cylindrical flow type microchemical device main body 40, it was confirmed that the fouling in the mixing channel 58 was almost completely removed and the cleaning property was high.

(Comparative example) When washing with a washing solution in which bubbles are not mixed First, a washing solution was prepared such that dimethyl sulfoxide (DMSO) and water were in a volume ratio of 90:10. After synthesizing the pigment fine particle dispersion, this washing solution is flowed at a flow rate of 0.5 mL / min at room temperature (about 20 ° C.) using a syringe pump (Harvard). The plate was passed through the plate through hole 42A, the thick short cylindrical recess 42C, the cylindrical through hole 42B, and the mixing channel 58.

  At this time, no laminar vortex was generated in the mixing channel 58 due to the cleaning fluid. Thereafter, the cleaning solution discharged from the cylindrical flow type microchemical device main body 40 was sampled, and the absorbance was measured using a spectrophotometer. And it was 30 minutes when the cleaning completion time until the light absorbency of the sampled cleaning fluid reached the detection limit was measured. Thereafter, as a result of disassembling and observing the cylindrical flow type microchemical device main body 40, it was confirmed that the contamination in the mixing channel 58 remained in the vicinity of the outlet.

  As described above, by applying the method for cleaning a microchemical device according to the present invention, it is possible to efficiently remove the fouling in the microchannel and improve the product quality even during operation. .

  As a method for synthesizing the pigment fine particle dispersion, the example of Pigment Red has been described in Example B. However, the present invention is not limited to this, and a magenta pigment, a yellow pigment, or a cyan pigment can also be used. Specifically, perylene, perinone, quinacridone, quinacridonequinone, anthraquinone, anthanthrone, benzimidazolone, disazo condensation, disazo, azo, indanthrone, phthalocyanine, triarylcarbonium, dioxazine, aminoanthraquinone, diketopyrrolopyrrole, thioindigo, A magenta pigment such as isoindoline, isoindolinone, pyranthrone or isoviolanthrone pigment, or a mixture thereof, a yellow pigment, or a cyan pigment can be used.

  More specifically, for example, C.I. I. Pigment Red 190 (C.I. bangou 71140), C.I. I. Pigment red 224 (C.I. No. 71127), C.I. I. Perylene pigments such as CI Pigment Violet 29 (C.I. No. 71129); I. Pigment orange 43 (C.I. No. 71105), or C.I. I. Perinone pigments such as CI Pigment Red 194 (C.I. No. 71100); I. Pigment violet 19 (C.I. No. 73900), C.I. I. Pigment violet 42, C.I. I. Pigment red 122 (C.I. No. 73915), C.I. I. Pigment red 192, C.I. I. Pigment red 202 (C.I. No. 73907), C.I. I. Pigment Red 207 (C.I. No. 73900, 73906) or C.I. I. Pigment Red 209 (C.I. No. 73905), a quinacridone pigment, C.I. I. Pigment red 206 (C.I. No. 73900/73920), C.I. I. Pigment orange 48 (C.I. No. 73900/73920), or C.I. I. Quinacridone quinone pigments such as CI Pigment Orange 49 (C.I. No. 73900/73920); I. Anthraquinone pigments such as CI Pigment Yellow 147 (C.I. No. 60645); I. Anthanthrone pigments such as CI Pigment Red 168 (C.I. No. 59300); I. Pigment brown 25 (C.I. No. 12510), C.I. I. Pigment violet 32 (C.I. No. 12517), C.I. I. Pigment yellow 180 (C.I. No. 21290), C.I. I. Pigment yellow 181 (C.I. No. 11777), C.I. I. Pigment orange 62 (C.I. No. 11775), or C.I. I. Benzimidazolone pigments such as CI Pigment Red 185 (C.I. No. 12516); I. Pigment yellow 93 (C.I. No. 20710), C.I. I. Pigment yellow 94 (C.I. No. 20038), C.I. I. Pigment yellow 95 (C.I. No. 20034), C.I. I. Pigment yellow 128 (C.I. No. 20037), C.I. I. Pigment yellow 166 (C.I. No. 20035), C.I. I. Pigment orange 34 (C.I. No. 21115), C.I. I. Pigment orange 13 (C.I. No. 21110), C.I. I. Pigment orange 31 (C.I. No. 20050), C.I. I. Pigment red 144 (C.I. No. 20735), C.I. I. Pigment red 166 (C.I. No. 20730), C.I. I. Pigment red 220 (C.I. No. 20055), C.I. I. Pigment red 221 (C.I. No. 20065), C.I. I. Pigment red 242 (C.I. No. 20067), C.I. I. Pigment red 248, C.I. I. Pigment red 262, or C.I. I. Disazo condensation pigments such as CI Pigment Brown 23 (C.I. No. 20060); I. Pigment yellow 13 (C.I. No. 21100), C.I. I. Pigment yellow 83 (C.I. No. 21108), or C.I. I. Disazo pigments such as CI Pigment Yellow 188 (C.I. No. 21094); I. Pigment red 187 (C.I. No. 12486), C.I. I. Pigment red 170 (C.I. No. 12475), C.I. I. Pigment yellow 74 (C.I. No. 11714), C.I. I. Pigment red 48 (C.I. No. 15865), C.I. I. Pigment red 53 (C.I. No. 15585), C.I. I. Pigment orange 64 (C.I. No. 12760), or C.I. I. Azo pigments such as C.I. Pigment Red 247 (C.I. No. 15915), C.I. I. Indanthrone pigments such as CI Pigment Blue 60 (C.I. No. 69800); I. Pigment green 7 (C.I. No. 74260), C.I. I. Pigment Green 36 (C.I. No. 74265), Pigment Green 37 (C.I. No. 74255), Pigment Blue 16 (C.I. No. 74100), C.I. I. Phthalocyanine pigments such as CI Pigment Blue 75 (C.I. No. 74160: 2) or 15 (C.I. No. 74160); I. Pigment blue 56 (C.I. No. 42800), or C.I. I. Triarylcarbonium pigments such as CI Pigment Blue 61 (C.I. No. 42765: 1); I. Pigment violet 23 (C.I. No. 51319) or C.I. I. Dioxazine pigments such as CI Pigment Violet 37 (C.I. No. 51345); I. Aminoanthraquinone pigments such as CI Pigment Red 177 (C.I. No. 65300); I. Pigment red 254 (C.I. No. 56110), C.I. I. Pigment Red 255 (C.I. No. 561050), C.I. I. Pigment red 264, C.I. I. Pigment red 272 (C.I. No. 561150), C.I. I. Pigment orange 71, or C.I. I. Diketopyrrolopyrrole pigments such as C.I. Pigment Orange 73; I. Thioindigo pigments such as CI Pigment Red 88 (C.I. No. 7313); I. Pigment yellow 139 (C.I. No. 56298), C.I. I. Pigment Orange 66 (C.I. No. 48210) and the like, isoindoline pigments such as C.I. I. Pigment yellow 109 (C.I. No. 56284), or C.I. I. Pigment Orange 61 (C.I. No. 11295) and other isoindolinone pigments, C.I. I. Pigment Orange 40 (C.I. No. 59700) or C.I. I. Pyranthrone pigments such as CI Pigment Red 216 (C.I. No. 59710), or C.I. I. It is an isoviolanthrone pigment such as CI Pigment Violet 31 (60010).

It is a perspective view which shows the flaky flow type | mold microchemical apparatus to which this invention is applied. It is the top view and sectional drawing which show the flaky flow type | mold microchemical apparatus to which this invention is applied. It is a figure which shows the washing | cleaning method in this Embodiment. It is a figure which shows the other washing | cleaning method in this Embodiment. It is a figure which shows the further another washing | cleaning method in this Embodiment. It is a figure which shows the further another washing | cleaning method in this Embodiment. It is a perspective view which shows the microchemical apparatus system of the other form of this Embodiment. It is sectional drawing of the microchannel in the microchemical apparatus system of the other form of this Embodiment. It is a fragmentary perspective view in the micro channel outflow side in the microchemical device system of other forms of this embodiment. It is a fragmentary perspective view which shows the rib shape of a plate in the microchemical apparatus system of the other form of this Embodiment. It is a figure of the prior art example which the fouling accumulated in the microchannel of a flaky flow type microchemical device.

Explanation of symbols

    2 ... Fouling, 4 ... Gas, 10A, 10B ... Raw material storage unit, 11 ... Air supply means, 12 ... Cleaning fluid storage unit, 13 ... Pressure control means, 14 ... Product recovery unit, 18, 20, 28A, 28B ... Piping, 30 ... Flame flow type microchemical device main body, 31 ... Main body member, 32 ... Micro flow path, 33 ... Cover member, 34A, 34B ... Fluid supply path, 36, 37 ... Inlet, 38 ... Outlet, DESCRIPTION OF SYMBOLS 40 ... Cylindrical flow type micro chemical apparatus, 42 ... Plate, 42A ... Plate through-hole, 42B ... Cylindrical through-hole, 42C ... Thick-walled short cylindrical recessed part, 44 ... Lid member, 44A, 44B, 44C ... Lid member through Hole, 45C ... outer layer flow path, 46 ... receiving member, 48A, 48B, 48C ... piping, 54 ... micro flow path (cylindrical flow type), 58 ... mixing flow path

Claims (16)

In a cleaning method of a microchemical apparatus in which a plurality of types of raw material fluids are joined to one micro flow channel having an equivalent diameter of 1 mm or less through each fluid supply path to perform a reaction operation or a unit operation,
A cleaning method for a microchemical device, wherein a cleaning fluid is circulated through the microchannel and laminar vortices are generated in the microchannel to clean the microchannel.   The method for cleaning a microchemical device according to claim 1, wherein the laminar flow vortex is a vortex generated in a laminar flow region or a flow in a transition region from laminar flow to turbulent flow. In a cleaning method of a microchemical apparatus in which a plurality of types of raw material fluids are joined to one micro flow channel having an equivalent diameter of 1 mm or less through each fluid supply path to perform a reaction operation or a unit operation,
A microchemical apparatus characterized in that a cleaning fluid is circulated through the microchannel, an air supply means is provided upstream of the microchannel, and a gas is mixed into the cleaning fluid to clean the microchannel. Cleaning method.   The method of cleaning a microchemical device according to claim 3, wherein the cleaning fluid generates a laminar vortex.   The method for cleaning a microchemical device according to any one of claims 1 to 4, wherein a vibration applying means is provided in the microchemical device to apply vibration to the microchannel.   The method for cleaning a microchemical device according to claim 1, wherein an ultrasonic wave is applied to the cleaning fluid in the microchannel. A pressure control means is provided downstream of the microchannel,
The method for cleaning a microchemical device according to any one of claims 1 to 6, wherein the pressure is released after applying a pressure of a predetermined value or more to the cleaning fluid in the microchannel.   The microchemical device according to any one of claims 1 to 7, comprising a step of causing the cleaning fluid to flow through the microchannel and a step of stopping the flow of the cleaning fluid to the microchannel. Cleaning method.   9. The method according to claim 1, further comprising: circulating the cleaning fluid from one end side of the microchannel; and circulating the cleaning fluid from the other end side of the microchannel. Cleaning method for micro chemical equipment. The microchemical device is provided with temperature control means,
The method for cleaning a microchemical device according to any one of claims 1 to 9, wherein the cleaning fluid in the microchannel is heated.   A cleaning method for circulating a plurality of types of the cleaning fluid in the microchannel, wherein the last cleaning fluid to be circulated in the microchannel is a fluid that does not inhibit a reaction operation or a unit operation in the microchannel. The method for cleaning a microchemical device according to any one of claims 1 to 10.   The method for cleaning a microchemical device according to claim 11, wherein the cleaning fluid is filled in the microchannel and allowed to elapse for a predetermined time, and then the cleaning fluid is discharged from the microchannel.   The unit operation includes mixing, separation, classification, filtration, heating, cooling, heat exchange, extraction, crystallization, dissolution, evaporation, distillation, absorption, adsorption, and the reaction operation targets inorganic substances and organic substances. Ion reaction, redox reaction, electrolytic reaction, nitrification reaction, combustion reaction, combustion reaction, roasting reaction, halogenation reaction, sulfonation reaction, alkylation reaction, esterification reaction, fermentation reaction, thermal reaction, catalytic reaction, The method for cleaning a microchemical device according to claim 1, comprising a radical reaction and a polymerization reaction.   The method for cleaning a microchemical apparatus according to any one of claims 1 to 13, wherein the cleaning method is introduced during the unit operation or the reaction operation.   The method for cleaning a microchemical device according to any one of claims 1 to 14, wherein the cleaning fluid is caused to flow through the microchannel a plurality of times. The manufacturing method of the pigment which introduce | transduced the washing | cleaning method of the microchemical apparatus of any one of Claims 1-15.

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