JP2009255083A - Microchemical device-operating method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To remove a gas in a micro flow channel and conduct a homogeneous reaction in the micro flow channel, to gain a prescribed product. <P>SOLUTION: In a method for operating a microchemical device 30, two kinds of material fluids A and B join together in one micro flow channel 32 having an equivalent diameter of 1 mm or smaller through their own fluid feeding paths 34A and 34B, respectively, to conduct a reacting operation or a unit operation. In this case, before operating the device, one or more displacement fluids whose surface tension is smaller than that of either the material fluid A or the material fluid B pass through the micro flow channel 32, to remove the gas in the micro flow channel 32. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to a method for operating a microchemical apparatus, and more particularly, to a method for operating a microchemical apparatus 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, there has been proposed a precise reaction / mixing system for chemicals or the like using a fine flow path formed by a fine processing technique such as etching (see Patent Documents 1 and 2).

  Patent Document 1 discloses a flaky flow microreactor. This microreactor has a structure in which a Y-shaped liquid flow path is formed which includes a micro flow path for reacting two kinds of liquids and two liquid supply paths for joining the two kinds of liquids to the micro flow paths. Is. In this microreactor, two types of solutions are introduced from the inlet of the liquid supply path, and the solutions are reacted or mixed by being joined in the microchannel. In order to increase the reaction efficiency in the microchannel, the wall surface in the vicinity of the microchannel is thinned so that laser irradiation can be performed.

  Patent Document 2 discloses a cylindrical flow type microreactor. This microreactor has a structure in which a lid member, a plate, and a receiving member are laminated. In this microreactor, three kinds of solutions are allowed to flow from the inlet of the lid member, and are circulated in a micro flow path formed into a concentric circle formed in a plate, and a mixing flow path formed in a receiving member The three liquids are reacted or mixed at the same time. Thereby, it has a structure which can mix or react two or more types of fluids.

JP 2004-126686 A JP 2004-344877 A

  However, such a microchemical apparatus is operated in a continuous flow system, but at the start of operation, in many cases, bubbles or gas remains in the microchannel. FIG. 13 is a conceptual diagram showing a conventional Y-shaped channel 1. As shown in FIG. 13, when the raw material fluid is directly circulated in the Y-shaped flow channel 1 with the bubbles 2 remaining, the wettability of the raw material fluid with respect to the material of the inner wall surface of the micro flow channel. However, since the influence of the surface tension is large in the micro space, the bubbles are likely to remain at the channel branching portion and the corner portion in the micro channel. Since the bubbles 2 block the flow path 3, the raw material fluid or the product is not uniformly supplied or discharged in the flow path 3.

  Moreover, since the width of the flow path 3 is changed by the bubbles, there is a problem that the mixing ratio of the raw material fluid in the flow path 3 varies and it is difficult to obtain a desired product.

  In addition, when the timing of inflow or stoppage of two or more kinds of raw material solutions deviates from a predetermined range at the start or end of operation, the mixing ratio of these solutions changes, and aggregation and precipitation occur in the microchannel. appear. For this reason, there is a problem that it is difficult to obtain a desired product as described above.

  The present invention has been made in view of such circumstances, and at the start of operation, the product concentration in the microchannel can be prevented from increasing rapidly, and the precipitation / aggregation in the microchannel can be suppressed. It is an object of the present invention to provide a method for operating a microchemical apparatus capable of performing the above. It is another object of the present invention to provide a method for operating a microchemical apparatus that can remove a gas in a microchannel and perform a uniform reaction in the microchannel to obtain a desired product.

  In order to solve the above-mentioned problems, the present invention is a micro that performs a reaction operation or a unit operation by merging a plurality of types of raw material fluids into one micro flow path having an equivalent diameter of 1 mm or less through each fluid supply path. In the operation method of the chemical apparatus, a first step of circulating one or more first raw material fluids at the start of operation, and a second raw material other than the first raw material fluid after a predetermined time has elapsed from the first step And a second step of circulating a fluid. A method of operating a microchemical device is provided.

  According to the present invention, since the product concentration in the microchannel does not increase rapidly at the start of operation, precipitation / aggregation in the microchannel can be suppressed.

  Moreover, in this invention, when there are two or more said 1st raw material fluids in said 1st step, it is preferable that said 1st raw material fluid is a fluid which does not aggregate or precipitate mutually.

  Thus, in the case where reaction or mixing of two or more plural raw material fluids is started, the raw material fluids circulated at the same time do not cause precipitation or aggregation due to mutual reaction. Therefore, clogging of the microchannel is suppressed.

  Also, in the present invention, at the end of the operation, a third step of stopping the flow of the one or more second raw material fluids, and one or more other than the second raw material fluids after a predetermined time has elapsed from the third step And a fourth step of stopping the flow of the first raw material fluid. Moreover, in this invention, when there are two or more said 2nd raw material fluids in a said 4th step, it is preferable that said 2nd raw material fluid is a fluid which does not aggregate or precipitate mutually. Thus, when the reaction or mixing of a plurality of two or more raw material fluids is completed, the raw material fluids that are stopped at the same time do not cause precipitation or aggregation due to mutual reaction. Therefore, clogging of the microchannel is suppressed.

  Further, in the present invention, before the start of the operation of the microchemical device, one or more replacement fluids having better wettability than the one of the raw material fluids, that is, having a low surface tension, are circulated through the microchannel. It is preferable to remove the gas in the flow path.

  Before the operation is started, the replacement fluid is wetted on the entire inner wall surface of the microchannel, so that the fluidity of the replacement fluid is improved and the gas attached to the inner wall surface of the microchannel is easily removed. Therefore, the reaction or mixing between the raw material fluids is not hindered by the gas remaining in the microchannel during steady operation.

  The wettability described above depends on the correlation between bubbles or gas and the material of the inner wall surface of the microchannel, but in the present invention, the surface tension of the replacement fluid is preferably 1 to 100 mN / m. Moreover, 1-75 mN / m is more preferable, and 1-30 mN / m is further more preferable. When the surface tension is within this range, the replacement fluid quickly wets the entire inner wall surface of the microchannel, and the fluidity is improved. Therefore, the gas adhering to the inner wall surface of the microchannel is quickly removed out of the microchannel.

  In addition, before the start of operation, a first step of circulating a first replacement fluid having a surface tension smaller than any one of the raw material fluids, and a surface tension higher than that of the first replacement fluid in the microchannel It is preferable to include a second step of circulating a large second replacement fluid and a third step of circulating the third replacement fluid containing the raw material fluid or the raw material fluid in the microchannel.

  In this way, first, the replacement fluid having a small surface tension wets and flows on the inner wall of the microchannel, whereby the gas is quickly removed out of the microchannel. Furthermore, after that, the replacement fluid is gradually replaced with a fluid close to the raw material fluid, so that the replacement fluid in the micro-channel is washed away and the flow and reaction of the raw material fluid in steady operation is prevented from being hindered. Can do.

  Further, it is preferable that the step of circulating the replacement fluid through the microchannel and the step of stopping the flow of the replacement fluid are alternately repeated one or more times before the operation is started. Further, the operation that is alternately repeated one or more times may be continuous or discontinuous, and may be an operation that results in a pulsating flow when continuous.

  In this way, by stopping the flow of the replacement fluid, the replacement fluid can be diffused and spread throughout the microchannel. Thereafter, by allowing the replacement fluid to flow again, the gas can be removed out of the microchannel by the flow force of the replacement fluid.

  It is preferable that the method further includes a step of causing the replacement fluid to flow from one end side of the microchannel and a step of causing the replacement fluid to flow from the other end side of the microchannel. According to this method, the flow of the replacement fluid in the vicinity of the gas staying in a place such as a branch channel portion or a corner portion in the micro channel is changed in a complicated manner. Therefore, the gas easily flows and is removed out of the microchannel.

  Moreover, when removing the gas in the microchannel, it is preferable to tilt the microchemical device at an angle at which the gas can be removed. In this way, in the inclined micro channel, gas lighter than the specific gravity of the fluid rises in the micro channel in the direction opposite to the direction of gravity. Therefore, the gas in the microchannel is easily removed.

  Further, in the present invention, in a microchemical apparatus in which a switching unit is provided downstream of the microchannel and the microchannel is communicated with the waste recovery unit or the product recovery unit by the switching unit. A product that operates for a predetermined time in a disposal mode in which a product obtained by a reaction operation or unit operation in a channel is communicated to a waste recovery unit, and then operates the switching means to communicate the product to the product recovery unit. It is preferable to operate in the recovery mode.

  As described above, since the reaction or mixing in the micro flow path is not uniform and unstable for a predetermined time immediately after the start of operation, the waste that deviates from the desired physical properties is discarded. In addition, immediately after the start of operation, after a predetermined time has elapsed, the reaction or mixing state in the microchannel is uniform and stable, so that usable materials having desired physical properties are collected. Accordingly, only usable materials having desired physical properties are collected in the product collection unit.

  In the present invention, it is preferable to operate in the discard mode after the operation in the product recovery mode. In this way, the product deviated from the desired physical properties obtained at the end of the operation is discarded by the switching means. Therefore, it can suppress that the product which remove | deviated from the desired physical property mixes in a product collection | recovery part.

  In the present invention, after the start of operation, it is determined whether the product obtained by the reaction operation or the unit operation in the microchannel is a waste or usable product, and the switching means is operated, and the waste recovery unit or It is preferable that the microchannel is communicated with the product recovery unit.

  As described above, after the operation is started, the physical properties of the product reacted or mixed in the microchannel are determined as to whether or not the detection means can be used. When it is determined that the product is usable, the switching unit operates to communicate with the product recovery unit. Accordingly, it is possible to collect usable materials having desired physical properties with high accuracy.

  Further, in the present invention, after the start of operation, when determining whether the product obtained by the reaction operation or the unit operation in the microchannel is waste or usable, it can be used continuously for a predetermined time. It is preferable that when the determination is made, the switching means is operated to communicate the microchannel with the waste recovery unit or the product recovery unit.

  As described above, after the operation is started, it is determined whether the physical property of the product obtained by the reaction or mixing in the micro flow channel is a usable material continuously for a predetermined time. When it is determined that the product is continuously usable for a predetermined time, the switching means operates to communicate with the product recovery unit. Therefore, usable materials having desired physical properties with higher accuracy can be collected.

  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.

  As described above, according to the present invention, at the start of operation, the product concentration in the microchannel can be prevented from increasing rapidly, and precipitation / aggregation in the microchannel can be suppressed.

It is a figure which shows the microchemical apparatus system to which this invention is applied. 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 driving | running method in this Embodiment. It is a figure which shows the other driving | running method in this Embodiment. It is a figure which shows the other driving | operation method in this Embodiment. It is a figure which shows the timing of the driving | running state in this Embodiment. It is a figure which shows the other driving | operation 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 bubble collected in the microchannel of a flaky flow type microchemical device before the start of operation.

  Hereinafter, preferred embodiments of a method for operating a microchemical apparatus according to the present invention will be described in detail with reference to the accompanying drawings.

  FIG. 1 shows a microchemical apparatus system 100 to which a method for operating a microchemical apparatus according to the present invention is applied, and FIGS. 2 and 3 show a microchemical apparatus main body 30 which is a main part of the microchemical apparatus system 100. Among these, FIG. 2 is a perspective view, FIG. 3A is a plan view, and FIG. 3B is a cross-sectional view taken along line F-F ′ of FIG. The microchemical device system 100 is a system for recovering a product by mixing or reacting two kinds of raw material fluids in a microchannel of a flaky flow type microchemical device. The microchemical apparatus system 100 includes a microchemical apparatus main body 30 having a micro flow path, raw material fluid storage units 10A and 10B, a replacement fluid storage unit 12, a product recovery unit 14, a waste recovery unit 16, It comprises pipes 18, 20, 22, 24, 26, and 28 that connect them.

  First, details of the microchemical device main body 30 will be described. As shown in FIG. 2, the flaky flow type microchemical device main body 30 includes a micro flow channel 32 that reacts two kinds of raw material fluids, and two pieces that join two kinds of raw material fluids into the micro flow path 32. A Y-shaped liquid flow path including the 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. In the microchemical device system 100, pipes 18, 20, and 22 are connected to the inlets 36 and 37 and the outlet 38, respectively.

  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, It is preferable to select soldering, adhesion, etc. 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 to 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 used in the present invention is a fluid necessary for obtaining a product, such as a liquid, a gas, a solid-liquid mixture in which solid fine particles are dispersed in the liquid, and 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.

  The replacement fluid is a fluid having a surface tension smaller than any one of the raw material fluids, and the gas in the flow path is removed by circulating the fluid through the micro flow path 32. Examples thereof include surfactants, commercially available neutral detergents, alcohols such as methanol and ethanol, benzene and acetone. In addition to changing the type of fluid, it is also possible to reduce the surface tension by increasing the temperature. The surface tension of the replacement fluid is preferably 1 to 100 mN / m, more preferably 1 to 75 mN / m, and still more preferably 1 to 30 mN / m.

  In the microchemical device system 100 of FIG. 1, the raw material fluid storage units 10 </ b> A and 10 </ b> B each store the raw material fluid necessary for the reaction in the microchemical device main body 30. The replacement fluid storage unit 12 stores a replacement fluid used for removing the gas in the microchannel 32 before the start of operation for reaction. The product recovery unit 14 recovers the product discharged from the microchemical device main body 30. The waste collection unit 16 collects the waste discharged from the microchemical device main body 30.

  Further, pipes 18 and 20 are provided so as to connect between the raw material fluid storage units 10A and 10B and the inlets 36 and 37 of the microchemical device main body 30, respectively. A pipe 22 is provided so as to connect the outlet 22 of the microchemical device main body 30 and the product recovery unit 14.

  The pipes 18 and 20 are connected to the microchemical device main body via fluid supply means (pumps or the like) (not shown) to supply the raw material fluids A and B from the raw material fluid storage units 10A and 10B to the microchemical device main body 30, respectively. 30 inlets 36, 37 are connected. The pipe 22 is connected to the product recovery unit 14 so as to supply the product obtained from the microchemical device main body 30 to the product recovery unit 14.

  Further, the fluid supply means may be arranged in either one of the upstream piping or the downstream piping relative to the microchemical device main body 30. A specific example of the fluid supply means is a pump, but other supply means may be used as long as it has a drive function of sending fluid.

  Further, as shown by a dotted line in FIG. 1, a pipe 24 is provided to connect between the replacement fluid storage unit 12 and the pipe 18. Similarly, a pipe 26 is provided to connect between the replacement fluid storage unit 12 and the pipe 20. A pipe 28 is provided to connect the pipe 22 and the waste collection unit 16.

  At the confluence of the pipe 18 and the pipe 24, the flow path for connecting the raw fluid A from the raw fluid storage section 10A to the inlet 36 of the microchemical device main body 30 via the fluid supply means (not shown) is replaced with the replacement fluid. Switching means (not shown) that can be switched is arranged in the flow path that is connected from the fluid storage unit 12 to the inlet 36 of the microchemical device main body 30 via a fluid supply means (not shown). Similarly, switching means (not shown) is also provided at the junction of the pipe 20 and the pipe 26. Further, at the junction of the pipe 22 and the pipe 28, the product is discharged from the outlet 38 of the microchemical device main body 30 to the product recovery unit 14, and the product is discharged from the outlet 38 of the microchemical device main body 30. A switching means (not shown) that can be switched to a flow path for discharging to the waste collection unit 16 is arranged. Further, this switching means can close not only one of the flow paths but also both the flow paths.

  Specific examples of such switching means include valves, dampers, electromagnetic valves, and the like, but other switching means may be used as long as they have a function of switching the flow path.

  In addition, the microchemical device main body 30 is provided with a rotation driving means (not shown) so as to be inclined so that the gas in the microchannel 32 is easily removed. A specific example of the rotation drive means is a motor or the like, but other drive means may be used as long as it has a rotation drive function.

  Next, an operation method of the microchemical device system will be described. First, a basic operation method of the microchemical device system 100 will be described.

  As an operation method in the microchemical device system 100 of FIG. 1, first, the raw material fluids A and B are supplied from the raw material fluid storage units 10A and 10B by fluid supply means (not shown). Thereafter, a flow path is selected by a switching means (not shown) so as to be connected to the inlets 36 and 37 of the microchemical device main body 30, respectively. The raw material fluids A and B flowing in from the inflow ports 36 and 37 flow through the fluid supply paths 34A and 34B, respectively, and then merge in the micro flow path 32. Then, after reacting or mixing in the microchannel 32, it flows out from the outlet 38. For the fluid that has flowed out, a flow path that connects to the product recovery unit 14 (or the next step) or the waste recovery unit 16 can be selected via the switching means.

  The timing for switching the flow path will be described later. In addition, the microchemical device main body 30 can be inclined at an angle at which bubbles in the microchannel 32 can be easily discharged by a rotation driving means (not shown). This may be tilted at regular intervals, or may be tilted to an angle that is easy to discharge when bubbles are detected by a detection means or the like. In addition, after the gas is discharged from the microchannel 32, the microchemical device body 30 is inclined at an angle at which the product can easily flow. However, the angle at which the gas is discharged may be maintained.

  Next, the operation method of the microchemical apparatus of the present invention will be described in the case where the raw fluid is flowed after the microchannel is washed with the replacement fluid before the operation of the microchemical apparatus is started.

  FIGS. 4-8 is a figure which shows the operation method in the case of two types of raw material fluids (raw material fluid A, B) in the flaky flow type microchemical device system 100 of the present invention. Among these, FIG. 7 is a time chart showing the operation timing for circulating the replacement fluid and the operation method for circulating the two types of raw material fluids. In addition, in each figure, the part which shows the code | symbol same as FIGS. 1-3 shall have the same thing or function.

  In the flaky flow type microchemical device main body 30 of FIG. 4, a replacement fluid having a surface tension smaller than any one of the raw material fluids is circulated, and the gas in the microchannel 32 is removed. First, as shown in FIG. 4A, the replacement fluid C having the smallest surface tension is first circulated through the micro flow channel 32 through the fluid supply channels 34A and 34B. Thereafter, as shown in FIG. 4B, the replacement fluid D having a surface tension larger than that of the replacement fluid C is circulated to the micro flow channel 32 through the fluid supply channels 34A and 34B. Then, as shown in FIG. 4C, in the final stage, the solvent of the raw material fluid A or B, the replacement fluid E containing the raw material fluid A or B, or the raw material fluid A or B is supplied from the fluid supply paths 34A and 34B. The microchannel 32 is circulated. In this way, by allowing the replacement fluid having a large surface tension to flow in a stepwise manner, the gas that hinders the reaction during steady operation can be removed from the flow path. In addition, by this method, not only the gas in the microchannel 32 but also impurities remaining in the microchannel 32 (things other than the replacement fluid and the raw material fluid) can be removed. Thereafter, the raw material fluids A and B are circulated from the fluid supply paths 34A and 34B to the microchannel 32, and an operation for performing a unit operation or a reaction operation is started.

  FIG. 5 shows a method of removing the gas in the microchannel 32 by changing the direction in which the replacement fluid is circulated through the microchannel 32 before starting the operation in the flaky flow type microchemical device main body 30. First, an operation is performed in which the replacement fluid C having a surface tension smaller than any one of the raw material fluids is circulated from the inlets 36 and 37 of the fluid supply paths 34A and 34B as shown in FIG. Next, as shown in FIG. 5B, an operation is performed in which the replacement fluid C is circulated from the outlet 38 of the microchannel 32 to the microchannel 32 in the direction opposite to that in FIG. Thereby, the gas collected in the location which cannot be easily removed only by circulating the replacement fluid C in one direction can be efficiently removed. Thereafter, the raw material fluids A and B are circulated from the fluid supply paths 34A and 34B to the microchannel 32, and an operation for performing a unit operation or a reaction operation is started.

  Next, in the flaky flow type microchemical device main body 30 of FIG. 6, a device is added at the start and end of operation when there are two types of raw material fluids (raw material fluids A and B). At the start of operation, as shown in FIG. 6B, from the state before the start of operation shown in FIG. 6A, first, the raw material fluid B is circulated from the fluid supply path 34B to the micro flow path 32 stably for a certain period of time. After that, as shown in FIG. 6C, the flow of the other raw material fluid A is started from the fluid supply path 34A (operation 1). Thereby, the clogging by a product which generate | occur | produces when the density | concentration of the product in the microchannel 32 increases rapidly can be suppressed. In addition, aggregation and precipitation that occur due to a variation in the mixing ratio accompanying a shift in the distribution timing can be suppressed.

  At the end of the operation, the opposite means to that at the start of operation is performed. That is, as shown in FIG. 6B from the steady operation state of FIG. 6C, first, the raw material fluid A is stopped, and then the raw material fluid B is stopped as shown in FIG. ). As a result, the product does not remain in the microchannel 32 and is finally discharged by the raw material fluid B that stops the circulation. Therefore, the contamination in the microchannel 32 can be reduced.

  FIG. 7 is a time chart showing the timing when the raw material fluid is circulated. As shown in FIG. 7, before the start of operation, the replacement fluid C is allowed to flow from the inlets 36 and 37 to the microchannel 32 for a certain period of time (forward flow). Thereafter, the replacement fluid C is allowed to flow from the outlet 38 to the microchannel 32 for a predetermined time (back flow). Thereafter, the replacement fluid C is allowed to flow through the microchannel 32 in a forward direction for a certain period of time. In this way, by changing the direction in which the replacement fluid C flows to the micro flow path 32 in the reverse direction at regular intervals, it is possible to remove the gas present at a location that tends to stay in the flow path.

  Furthermore, at the start of operation, the flow from the raw material fluid B to the micro flow channel 32 is started, and then the flow of the raw material fluid A to the micro flow channel 32 is started after a predetermined time has elapsed. After the steady operation, at the end of the operation, the flow of the raw material fluid A to the micro flow path 32 is first stopped, and then the flow of the raw material fluid B is stopped. Thereby, the clogging by the product in the microchannel 32 can be suppressed.

  FIG. 8 shows switching to the product recovery (or supply to the next process) mode or the waste recovery mode at the start or end of the operation in the vicinity of the outlet 38 of the microchannel 32 of the flaky flow type microchemical device body 30. Is the method.

  At the start of operation, as shown in FIG. 8 (A), the outlet 38 is connected to the pipe 28 introduced into the waste collection unit 16 until a predetermined time has passed after the raw material fluid A is circulated, The operation is performed in a mode in which the fluid discharged from the passage 32 is discarded. Thereafter, as shown in FIG. 8B, the outlet 38 is connected to the pipe 22 introduced into the product recovery unit 14 by the switching means, and the fluid discharged from the microchannel 32 is recovered as a product ( Alternatively, the operation is performed in the mode of supplying to the next process (operation 3).

  Immediately after the end of the operation, as shown in FIG. 8B, the outlet 38 is connected to the pipe 22 introduced into the product recovery unit 14, and the fluid discharged from the microchannel 32 is recovered as a product ( Or supply to the next process). Thereafter, as shown in FIG. 8 (A), the outlet 38 is connected to the pipe 28 introduced into the waste collection unit 16 by the switching means, and the fluid discharged from the microchannel 32 is discarded (operation 4). . Thereby, it can suppress that the waste which has physical properties other than a desired product mixes in a product collection | recovery part (or next process).

  Further, the physical property of the fluid discharged from the microchannel 32 is determined by a detection means (not shown), and it is determined whether the physical property is stably within a predetermined range for a predetermined time. For example, it is possible to connect to the pipe 22 to be introduced into the product recovery unit 14, and to be connected to the pipe 28 to be introduced into the waste recovery unit 16 if it is out of the predetermined range.

  Next, the form of the microchemical apparatus different from that shown in FIGS.

  9A and 9B 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. 10 is a cylindrical shape. FIG. 11 is a partial perspective view showing the outflow side of the plate constituting the cylindrical flow type microchemical device main body 40. FIG. 12 is a partial perspective view showing the rib shape of the plate constituting the cylindrical flow type microchemical device body 40.

  As shown in FIGS. 9A and 9B, the microchemical device main body 40 is a device that reacts 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 assembled by connecting the convex portion 71 and the concave portion 73 of the lid member 44. Similarly, 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, and 76 are integrated through the screw 70, whereby the cylindrical flow type microchemical device 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 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 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. 10 and 11, 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. 10, 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. 12, the slit cylindrical through hole 42B is provided with a plurality of ribs 68 that are continuous with the inner partition wall plate portion 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. 10, 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. 12) 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 microchemical device is the same as that of the flaky flow type microchemical device main body 30.

  Next, the case where the operation method of the microchemical apparatus of the present invention is applied to the cylindrical flow type microchemical apparatus main body 40 will be described.

  First, in FIGS. 9 (A) and 9 (B), before starting the operation, the replacement fluid is supplied from the three inflow pipes 48A, 48B, and 48C on the upstream side of the lid member 44 in the plate 42, respectively. It is made to distribute | circulate to the micro flow path 54 and the mixing flow path 58 which are laminarized in the shape of a core circle. Thereby, the replacement fluid having a surface tension smaller than that of the raw material fluid is wetted on the entire inner wall of the mixing channel 58, and the fluidity of the replacement fluid is improved, so that the gas in the mixing channel 58 can be easily removed.

  Next, in FIGS. 9A and 9B, at the start of operation, the raw material fluid A is circulated to the plate through hole 42 </ b> A in the microchannel 54 from the inflow pipe 48 </ b> A on the upstream side of the lid member 44. . Thereafter, after a predetermined time has elapsed, the raw material fluid B is circulated to the cylindrical through hole B in the microchannel 54 through the inflow pipe 48B. Further, after a predetermined time has elapsed, the raw material fluid C is circulated from the inflow pipe 48 </ b> C to the thick-walled short cylindrical recess 42 </ b> C in the microchannel 54. Then, the three liquids laminarized in the micro flow channel 54 are uniformly mixed or reacted in the mixing flow channel 58 to obtain a product D. By such an operation method, clogging of the mixing channel 58 by the product can be suppressed without the product concentration rapidly increasing in the mixing channel 58 formed in the receiving member 46.

  In addition, a method of appropriately changing the direction in which the replacement fluid flows through the micro flow channel 54 or the mixing flow channel 58 before the start of operation, and the replacement fluid having different surface tensions flow through the micro flow channel 54 or the mixing flow channel 58 multiple times step by step. By applying a pulsating method, a method of circulating a replacement fluid to the micro flow channel 54 or the mixing flow channel 58, a method of inclining the cylindrical flow type microchemical device main body 40, and the like. Gas can be removed from the flow path 58. In addition, a method of switching to product recovery (or supply to the next process) mode or waste recovery mode at the start or end of operation, a method of determining the physical properties of the product with the detection means, and controlling the switching means, etc. are applied. By doing, it can suppress that the waste which remove | deviated from the desired physical property range mixes in the product collect | recovered by a product collection | recovery part (or next process).

  As an example to which the operation method of the microchemical apparatus according to the present invention is applied, a case where a pigment fine particle dispersion excellent in monodispersibility is synthesized in the flaky flow type microchemical apparatus main body 30 will be described below. First, a method for producing the solutions P and Q to be raw material solutions will be described.

  In the synthesis of the pigment fine particle dispersion, the organic P is dissolved in the solution P, the aqueous medium Q, and at least one of them contains a dispersant, and the two liquids P and Q are brought into contact with each other to precipitate the organic pigment. To do. As a method of bringing the solution P in which the organic pigment is dissolved into contact with the aqueous medium Q, the present invention uses a microchemical apparatus system 100 shown in FIG.

  The organic pigment contained in the solution P is not particularly limited, and examples thereof include quinacridone pigments, phthalocyanine pigments, azo pigments, quinophthalone pigments, and isoindolinone pigments.

  Examples of quinacridone pigments include unsubstituted or substituted quinacridones such as unsubstituted quinacridone, 2,9-dimethylquinacridone, and 4,11-dichloroquinacridone, and solid solutions thereof.

The organic pigment is not limited in terms of hue, and a magenta pigment, a yellow pigment, or a cyan pigment can be used. Specifically, organic pigments are perylene, perinone, quinacridone, quinacridonequinone, anthraquinone, anthanthrone, benzimidazolone, disazo condensation, disazo, azo, indanthrone, phthalocyanine, triarylcarbonium, dioxazine, aminoanthraquinone, diketopyrrolo Magenta pigments such as pyrrole, thioindigo, isoindoline, isoindolinone, pyranthrone or isoviolanthrone pigments or mixtures thereof, yellow pigments, or cyan pigments.

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).

  In the method of preparing the solution P by dissolving the organic pigment, it is preferable to use a solvent having strong dissolving power and water miscibility, and examples thereof include a method using sulfuric acid. When the organic pigment is a quinacridone pigment, the solvent is preferably a mixture of an aprotic polar organic solvent, water, and caustic alkali.

  Specific examples of the aprotic polar organic solvent include dimethyl sulfoxide, dimethylformamide, N-methyl-2-pyrrolidone, 2-pyrrolidone, and tetramethylurea. The amount of the solvent used is appropriately 5 to 20 times that of the quinacridone pigment. The ratio of the aprotic polar organic solvent to water (organic solvent / water) is preferably used at a weight ratio of 97/3 to 70/30. The caustic alkali is preferably contained in an amount of 1.5 mol or more, more preferably 2 to 3 mol ratio per mol of the quinacridone pigment.

  The aqueous medium Q is water or a mixture of water and an aqueous solvent. In the case of a mixture, it is preferable to contain 50% or more by volume of water, and more preferably 80% or more. As the aqueous solvent, a water-soluble organic solvent having a vapor pressure lower than that of water can be preferably used.

  Specific examples include polyhydric alcohols typified by ethylene glycol, propylene glycol, diethylene glycol and the like; lower alkyl ethers of polyhydric alcohols such as ethylene glycol monomethyl (or ethyl) ether and diethylene glycol monomethyl (or ethyl) ether Heterocycles such as 2-pyrrolidone, N-methyl-2-pyrrolidone and 1,3-dimethyl-2-imidazolidinone; Sulfur-containing compounds such as sulfolane and dimethyl sulfoxide; Multifunctionals such as diacetone alcohol and diethanolamine Compound; and other urea derivatives.

  The dispersant has the action of (1) quickly adsorbing on the surface of the pigment deposited to form fine pigment particles, and (2) preventing these particles from aggregating again. As such a dispersant, anionic, cationic, amphoteric and nonionic surfactants, polymers, pigment derivatives into which polar substituents are introduced, and the like can be used.

  Specific examples of the anionic surfactant include acyl methyl taurate, fatty acid salt, alkyl sulfate ester salt, alkyl benzene sulfonate, alkyl naphthalene sulfonate, and the like.

  Specific examples of nonionic surfactants include polyoxyethylene alkyl ethers, polyoxyethylene alkyl aryl ethers, polyoxyethylene fatty acid esters, and the like.

  Specific examples of the polymer include polyvinyl pyrrolidone, polyvinyl alcohol, polyvinyl methyl ether, polyethylene oxide, polyacrylamide, vinyl alcohol-vinyl acetate copolymer, polyacrylate, polyvinyl sulfate, polyamide, polyallylamine salt. , Condensed naphthalene sulfonate, methacrylic acid ester-acrylate copolymer, cellulose derivative and the like. In addition, natural polymers such as alginate, gelatin, albumin, casein and gum arabic can also be used.

  The blending amount of the dispersant is preferably in the range of 0.1 to 250 parts by mass, more preferably in the range of 1 to 100 parts by mass with respect to 100 parts by mass of the pigment.

  As described above, the solution P in which the organic pigment is dissolved, the aqueous medium Q, and at least one of them contains a dispersant, and the two liquids P and Q are contained in the flaky flow type microchemical device body 30. To obtain a pigment fine particle dispersion.

  Next, a method of synthesizing the pigment fine particle dispersion in the flaky flow type microchemical device main body 30 by applying the first or third embodiment of the present invention will be described.

  13.5 g of dimethyl sulfoxide, 1.5 g of water, and 0.75 g of caustic potash were mixed, and 1.5 g of dimethylquinacridone pigment was added while stirring at room temperature. When stirring was continued at room temperature, the liquid gradually turned blue-purple and changed from a slurry to a deep blue-purple solution. After stirring for about 1.5 hours, suction filtration was performed with a No. 4 (pore size: 2.7 μm) glass filter to remove impurities remaining in a trace amount, thereby obtaining a dimethylquinacridone solution. This is designated as Solution P. Next, 0.75 g of oleylmethyl taurine sodium salt and 90 cm 3 of water were mixed as a dispersant. This is designated as Solution Q.

Example 1
After removing the gas in the flaky flow type microchemical device main body 30, a pigment particle dispersion solution was synthesized. First, before starting the operation of bringing the solutions P and Q into contact, methanol as a replacement fluid was circulated in the microchannel 32 at a flow rate of 1 mL / min for 10 minutes. It was confirmed visually that the gas had been completely removed.

  After that, 1 minute after the solution Q which had been sufficiently stirred started to flow through the inlet 37 of the microchemical device main body 30, the solution P was supplied from the inlet 36 of the microchemical device main body 30. When the two liquids were brought into contact with each other in the microchannel 32, it was confirmed by visual observation that no precipitation or aggregation occurred, and a uniform dispersion liquid was continuously obtained.

(Example 2)
In Example 2, before starting operation, a method in which a fluid having a small surface tension was circulated through the microchannel by pulsating flow was used to remove the gas in the flaky flow type microchemical device main body 30. First, before starting the operation in which the solutions P and Q are brought into contact with each other, methanol is circulated at a flow rate of 1 mL / min for 1 minute from the inlets 36 and 37 of the microchemical device main body 30 and then the circulation is stopped. (Step 1). Next, after flowing methanol as a replacement fluid at a flow rate of 1 mL / min for 1 minute from the outlet 38 of the microchemical device main body 30, the flow was stopped (step 2). Further, when Step 1 was performed again, it was confirmed by visual observation that the gas remaining in the microchannel 32 was completely removed.

  Next, a pigment particle dispersion solution was synthesized in the flaky flow type microchemical device main body 30. First, the solution Q which was sufficiently stirred was circulated from the inlet 36 of the microchemical device main body 30 one minute after starting to circulate the solution Q to the inlet 37 of the microchemical device main body 30. When the two liquids were brought into contact with each other in the microchannel 32, no precipitation or aggregation occurred, and a uniform dispersion was continuously obtained.

(Comparative example)
Before starting the operation of bringing the solutions P and Q into contact, the two solutions P and Q are simultaneously applied to the microchemical apparatus while the gas remains in the microchannel 32 of the flaky flow type microchemical apparatus main body 30. It was circulated through the inlets 36 and 37 of the main body 30. As a result, the gas in the microchannel 32 blocked a part of the channel, and the solutions P and Q could not be circulated smoothly. Furthermore, since the two liquids were circulated at the same time, precipitation and aggregation occurred in the microchannel and clogging occurred, making it impossible to continue the operation.

  As described above, by performing the operation method of the microchemical apparatus according to the present invention, the uniform reaction in the microchannel can be continued.

  DESCRIPTION OF SYMBOLS 10A, 10B ... Raw material fluid storage part, 12 ... Replacement fluid storage part, 14 ... Product recovery part, 16 ... Waste collection part, 18, 20, 22, 24, 26, 28 ... Piping, 30 ... Flaky flow type Microchemical device main body, 31 ... main body member, 32 ... microchannel, 33 ... lid member, 34A, 34B ... fluid supply channel, 36, 37 ... inlet, 38 ... outlet, 40 ... cylindrical flow type microchemical device Main body, 42 ... Plate, 42A ... Plate through hole, 42B ... Cylindrical through hole, 42C ... Thick short cylindrical recess, 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 method of operating a microchemical apparatus in which a plurality of types of raw material fluids are joined to a single microchannel having an equivalent diameter of 1 mm or less through each fluid supply path to perform a reaction operation or a unit operation.
A first step of circulating one or more first raw material fluids at the start of operation of the microchemical apparatus; and a second raw material fluid other than the first raw material fluid after a predetermined time has elapsed from the first step. A method for operating a microchemical apparatus, comprising: a second step for distribution.   2. The method of operating a microchemical device according to claim 1, wherein when there are two or more first raw material fluids in the first step, the first raw material fluids are fluids that do not aggregate or precipitate each other.   A third step of stopping the flow of the one or more second raw material fluids at the end of the operation; and a predetermined time after the third step, one or more of the first raw material fluids other than the second raw material fluid The method for operating a microchemical device according to claim 1, further comprising a fourth step of stopping the flow of the raw material fluid.   4. The method of operating a microchemical device according to claim 3, wherein when there are two or more second raw material fluids in the fourth step, the second raw material fluids are fluids that do not aggregate or precipitate with each other.   Before starting the operation of the microchemical device, one or more replacement fluids having a surface tension smaller than any one of the raw material fluids are circulated through the microchannels to remove gas in the microchannels. The operation method of the microchemical device according to any one of claims 1 to 4.   The microchemical apparatus operating method according to claim 5, wherein the displacement fluid has a surface tension of 1 to 100 mN / m.   Before starting the operation, a first step of circulating a first replacement fluid having a surface tension smaller than any one of the raw material fluids, and a surface tension greater than the first replacement fluid in the microchannel The second step of circulating a second replacement fluid, and the third step of circulating a third replacement fluid containing the raw material fluid or the raw material fluid in the microchannel. Operation method of micro chemical equipment.   6. The method of operating a microchemical device according to claim 5, wherein the step of circulating the replacement fluid through the microchannel and the step of stopping the flow of the replacement fluid are alternately repeated one or more times before starting the operation. .   The method of operating a microchemical device according to claim 5, comprising a step of flowing the replacement fluid from one end side of the microchannel and a step of flowing the replacement fluid from the other end side of the microchannel. .   The method for operating a microchemical device according to any one of claims 5 to 9, wherein when the gas in the microchannel is removed, the microchemical device is inclined at an angle at which the gas can be removed. In the microchemical apparatus that provides the switching means downstream of the microchannel, and communicates the microchannel with the waste recovery unit or the product recovery unit by the switching unit,
After starting operation of the microchemical device, after operating for a predetermined time in a disposal mode in which a product obtained by a reaction operation or unit operation in the microchannel is communicated to a waste recovery unit, the switching means is operated, The operation method of the microchemical device according to any one of claims 1 to 10, wherein the operation is performed in a product recovery mode in which the product is communicated with a product recovery unit.   The operation method of the microchemical device according to claim 11, wherein the operation is performed in the disposal mode after the operation in the product recovery mode.   After starting operation, it is determined whether the product obtained by the reaction operation or the unit operation in the microchannel is waste or usable, and the switching means is operated to operate the waste recovery unit or the product recovery unit. The method of operating a microchemical device according to claim 11, wherein the microchannel is communicated with each other.   After the start of operation, when determining whether the product obtained by the reaction operation or unit operation in the microchannel is waste or usable, the switching is performed when it is determined that the product is usable continuously for a predetermined time. 14. The method of operating a microchemical device according to claim 13, wherein the microchannel is communicated with the waste recovery unit or the product recovery unit by operating means.   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 operating a microchemical apparatus according to claim 1, comprising a radical reaction and a polymerization reaction.   The manufacturing method of the pigment using the operating method of the microchemical apparatus of any one of Claims 1-15.

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