JP2011115754A - Chemical apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a chemical apparatus feeding a constant quantity of raw materials to a microreactor in a simple structure and suppressing remaining air bubbles in priming. <P>SOLUTION: The chemical apparatus feeds different kinds and a plurality of raw materials to a reactor and obtains products by agitating or reacting in a fine flow channel inside the reactor. The chemical apparatus includes: a plurality of reactors; a plurality of loop channels circulating the different kinds and the plurality of raw materials; and a plurality of branched channels feeding the raw materials to the plurality of the reactors from the mid way of the respective loop channel. The loop channels are set to the sufficiently larger scales than the scales of the fine channels inside the reactor. <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

  The present invention relates to a chemical apparatus for scaling up the production throughput of a reactor (hereinafter referred to as a microreactor) using a microchannel.

  In recent years, microreactors that actively apply the advantages of micromachining technology and microscale to chemical processes have been actively researched and developed. Microreactors are expected to have various merits, one of which is the ease of scaling up the throughput. Normally, in the research and development and production of chemical products, the production volume is gradually scaled up to a mass production plant through research, product development and test plant at Laborepel.

  Generally, there are technical problems in scaling up from the laboratory level to the mass production level because the conditions under which the chemical reaction occurs are different between a small amount of chemical reaction at the beaker level and a large amount of chemical reaction in the production reactor. Often occurs.

  In order to avoid this problem as much as possible in the microreactor, a strategy has been proposed to scale up the processing volume at once by mounting multiple microreactors for low-volume processing developed and applied at the laboratory level according to the required volume at the mass production level. ing. This processing scale-up method, in which a single microreactor with a small amount of processing per unit is processed by the number of units mounted on the plant, is sometimes called numbering up. In the scale-up of the processing volume from the laboratory level processing volume using the microreactor to the mass production level in the plant, the numbering up is specifically generated by the type of piping to distribute the raw material equally to each microreactor. It is important to get things.

  In scale-up from the laboratory level to the plant level by numbering-up, for example, as disclosed in Patent Document 1 and Patent Document 2, a method of connecting microreactors in parallel to increase the number of mounting is often employed. The biggest merit of this parallel connection pipe is that the raw material is branched from one liquid feeding means (pump, header tank), so that the cost of the liquid feeding equipment can be suppressed. When branching, the liquid supply pressure at the branching portion is extremely reduced and the uniformity is not maintained, and the microchannel after branching is the adhering and remaining of bubbles due to the effect of capillary action, the flow path wall of the reactant in the microreactor In the case of blockage due to deposition on the surface, an imbalance in the flow resistance is exerted on all the other branch flow paths, and the desired liquid supply amount to each microreactor is disturbed.

  In addition, during the priming, i.e., when the plant raw material piping and the microreactor start from the empty state, the substitution failure that occurs in the initial state where the raw material is replaced with the raw material, that is, the residual gas phase, is It is highly uncertain whether it will flow into the microreactor, which may be a factor in reducing the performance of chemical operation in a micro space in the microreactor.

  As one of means for solving problems such as deposition of reactants in the microreactor on the flow path wall, Patent Document 1 monitors the liquid feed state of the raw material flowing through each flow path, and based on the information, the valve and liquid feed A method of controlling the means to maintain the raw material flowing through each flow path at a desired flow rate is disclosed.

JP 2008-80306 A JP 2004-344877 A

  However, in the technique described in Patent Document 1, a means for monitoring the flow rate and pressure for each branch flow path and a means for actively controlling flow path resistance such as a valve are implemented, and these always function correctly. It is a premise to continue. Therefore, in the technique described in Patent Document 1, the configuration of the chemical apparatus is complicated and expensive in order to maintain reliability. Also, Patent Document 2 shows an example of parallel-connected piping, but this is a piping configuration in which the adhesion and residual of bubbles due to the influence of the capillary phenomenon described above becomes a problem.

  In view of the above-mentioned problems of the prior art, the present invention does not mount flow rate monitoring and control means in each branch channel, but supplies a certain amount of raw material to each microreactor with a simpler configuration and method, and The present invention provides a chemical apparatus that can suppress the remaining of bubbles during priming, that is, a chemical apparatus that can completely replace the inside of a flow path with a raw material after the start of liquid feeding.

The present invention provides a chemical apparatus in which a plurality of different types of raw materials are supplied to a reactor and mixed or reacted in a fine channel inside the reactor to obtain a product.
A plurality of reactors and a plurality of loop flow paths for circulating a plurality of different types of raw materials, and a plurality of branches for supplying the raw materials from the middle of each loop flow path to the fine flow paths of the plurality of reactors Provided with a flow path, wherein the loop flow path is set to a scale sufficiently larger than the scale of the branch flow path or the fine flow path inside the reactor.

  In the above chemical apparatus, a control unit for controlling the flow rate, pressure, and temperature of the raw material in the loop flow path to desired values is provided.

  In the above chemical apparatus, the loop flow path, the branch flow path, and the reactor are formed in the material plane portion by grooving or drilling.

  In the above chemical apparatus, the plurality of loop channels and the plurality of branch channels are arranged inside the reactor.

  Further, the chemical apparatus is formed by connecting a plurality of the above chemical apparatuses.

  According to the present invention, since only the inside of the loop flow path is controlled by a pump or a valve, the number of flow rate monitors and pumps and valves used in the entire plant is greatly reduced, and the plant has a convenient configuration and is reliable. High system can be configured. In addition, the raw material is supplied from a loop pipe having a larger scale than the flow path in each microreactor, and the flow of the raw material in the loop pipe, in particular, the pressure thereof is controlled to be constant. For this reason, even if a part of the microreactors is blocked, a constant pressure is always applied to the other microreactors, so that the raw material is always distributed at a desired flow rate. Furthermore, in the present invention, since there is no branch part that distributes one flow to a plurality of fine flow paths at a time, there is no decrease in liquid feeding pressure in the middle, and frequent occurrences in conventional parallel branch pipe parts due to the influence of capillary action. The problem of air bubbles adhering to and remaining on the flow path wall is avoided.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is an explanatory diagram of a basic configuration of Embodiment 1 of the present invention. Explanatory drawing of Example 2 which applies Example 1 to a multistage reaction. FIG. 6 is an explanatory diagram of a Y-shaped mixing / reaction channel in Example 3. The exploded perspective view at the time of similarly installing a loop piping in a reactor. The assembly perspective view of a reactor similarly.

Example 1
FIG. 1 shows an explanatory diagram of the basic configuration of the piping and raw material liquid feed control of Embodiment 1 of the present invention. In this example, raw material A and raw material B are mixed or reacted to produce a product C, which is a two-raw material one-step reaction, or a mixing process.

  The raw material A and the raw material B are stored in the respective reservoir tanks 101 and 102, and are circulated through the loop pipes (flow paths) 109 and 110 by the pumps 103 and 104, respectively. The flow rates 111 and 112 flowing through the loop pipes 109 and 110 are monitored by the monitor 302 by the flow meters 107 and 108 so that the flow rates are suitable for the characteristics of the raw materials. Furthermore, the flow of the raw material (liquid feeding conditions) is adjusted by adjusting the outputs of the pumps 103 and 104 and the flow rate control valves 105 and 106 that can actively adjust the flow path opening degree based on the monitoring results. It is controlled to a desired condition (flow rate, pressure, temperature, etc.). These controls are controlled by the control unit 301.

  The raw materials A and B sucked into the respective loop pipes 109 and 110 by the pumps 103 and 104 return to the reservoir tanks 101 and 102 again after almost all of the raw materials have taken a round. In the middle of the process, a part of the raw material is finely divided into a plurality of microreactors 115 connected to the branch flow path 113 that is a part of the loop pipe 109 and the branch flow path 114 that is a part of the loop pipe 110. Distribution is performed via distribution channels 117 and 118.

  Distribution channels 117 and 118 are connected to a fine channel (not shown in FIG. 1) in microreactor 115 to supply raw materials. Therefore, the fine distribution channels 117 and 118 have the same flow rate and pressure as the connected fine channels. The distributed raw materials A and B are mixed or reacted in the fine flow path, collected as a product C, and collected in the tank 119 via the flow path 116.

  The loop pipes 109 and 110 are configured with a flow path scale sufficiently larger than the total scale of the fine flow paths in the microreactor 115. Here, the total scale of each fine flow path in the microreactor 115 is a scale of a level at which the capillary action of the raw material, that is, the wettability of the flow path wall surface mainly affects the behavior of the raw material during priming. The scale of a sufficiently large flow path of the loop pipes 109 and 110 indicates a scale (flow rate and pressure) at which the influence of the capillary action can be ignored. For example, each scale is set so that the flow rates or pressures of the loop pipes 109 and 110 are not less than 10 times the total flow rate or total pressure of all of the plurality of distribution channels 117 and 118 (or a plurality of fine channels). Is set.

  According to the present embodiment, the following effects can be obtained. Since the scale of the flow paths of the branch flow path portions 113 and 114 of the loop piping is sufficiently larger than the distribution flow connections 117 and 118 to the microreactors 115, the behavior (distribution) of the raw material in each microreactor during priming Is governed not by capillarity in the fine distribution channels 117, 118 or in the microreactor 115 but by the pressure in the loop pipes 109, 110. Accordingly, since the influence of the capillary phenomenon in the fine channels 117 and 118 is small, the remaining / attachment of bubbles during priming is avoided.

  Furthermore, as compared with the case where the raw material is stored in a tank or the like, the liquid phase is agitated by the cyclic flow of the raw material in the loop pipes 109 and 110, so that other compositions having different densities float in the liquid phase. In the case of raw materials such as slurry, a uniform dispersion effect is also obtained.

  The number of reactors 115 mounted is determined by the processing amount per microreactor and the desired processing amount of the entire plant, and the pipe diameter of the loop piping for circulating the raw material, the flow rate of the raw material, and the pressure according to the mounting number However, according to the present embodiment, these can be easily realized.

(Example 2)
In Example 2 of the present invention shown in FIG. 2, after obtaining the product C from the raw material A and the raw material B, the product C and the raw material D are further mixed or reacted to obtain a product E. Or it is an example of the process of reaction. A portion 201 surrounded by a dotted line in FIG. 2 is the same as the configuration described in FIG. A portion 202 surrounded by a dotted line is the same as the configuration of FIG. 1 or the portion 201 except that the product C obtained in the portion 201 is guided to the raw material tank 204 of the portion 202. Thus, in the present Example 2, it is applied to a plurality of multistage processes by constituting a mixture or reaction with one stage and two stages.

  Moreover, in Example 1 and Example 2 shown in FIG. 1 and FIG. 2, two-input one-output type mixing / reaction in which one product is obtained from two raw materials is shown as an example. It goes without saying that even a process for obtaining a product from a raw material can be handled by configuring the number of loop pipes according to the number of types of the raw material.

  1 and FIG. 2 both have loop pipes (flow paths) formed outside a plurality of microreactors and distribute raw materials to each microreactor, but the amount of processing is not so large. Alternatively, this pipe (channel) configuration can be manifolded inside the microreactor. An example is shown in the following examples.

(Example 3)
FIG. 3 shows an example of a typical microreactor that mixes or reacts two kinds of raw materials. The raw material F301 and the raw material G302 are made to flow through the two flow path portions 304 and 305 of the Y-shaped fine flow path, respectively, and the mixing / reaction flow path portion 303 mixes or reacts using molecular diffusion between both raw materials. . FIG. 4 and FIG. 5 show Example 3 in which the shape of this Y-shaped mixing / reaction channel (fine channel) is followed as it is and numbered up in the microreactor.

  In FIG. 4, the Y-shaped mixing / reaction channel (fine channel) shown in FIG. 3 is processed into a plurality of grooves (22 in FIG. 4) radially concentrically as indicated by 406. A plate-like component 408 arranged on the surface and an annular loop channel (FIGS. 1 and 2) formed concentrically by groove processing of a scale sufficiently larger than the Y-shaped mixing / reaction channel (fine channel) 404 and 405 are shown as plate-like components 409 arranged on the surface.

  In the Y-shaped mixing / reaction channel (fine channel) 406, a radially extending channel 502 (branch channel) formed by drilling is communicated with one radially extending inlet, A flow path 503 (branch flow path) that extends downward and is formed by drilling is also communicated with the other radially short inlet. In addition, ports 401 and 410 formed by drilling are communicated with both ends of the loop flow path 404, and the both ends of the loop flow path 405 are removed downward with the drilling process. Ports 402 and 403 are in communication.

  Each of the plurality of flow paths 502 that exits below the Y-shaped mixing / reaction flow path (fine flow path) 406 is annularly disposed so as to face directly above the arc of the loop flow path 404, A plurality of flow paths 503 that pass through the Y-shaped mixing / reaction flow path 406 are arranged in an annular shape so as to face directly above the arc of the loop flow path 405. Therefore, in a state where the plate-shaped component 408 overlaps the plate-shaped component 409, the plurality of flow paths 502 communicate with the loop flow path 404 in a shape along an arc, and the plurality of flow paths 503 are connected to the loop flow path. 405 communicates along the arc.

  The flow path 407 is a recovery flow path that is located in the center of the concentric circles of the loop flow paths 404 and 405 of the plate-like member 409 and is opened through vertically. This corresponds to the radiation center of the Y-shaped mixing / reaction channel (fine channel) 406. Therefore, in the state where the plate-like component 408 overlaps the plate-like component 409, the centers of the many Y-shaped mixing / reaction channels 406 and the recovery channel 407 communicate with each other.

  The microreactor according to the present embodiment is configured by stacking the plate-like component 409 on the plate-like component 408, and further stacking the plate-like material 501 serving as a lid on the plate-like component 408 and combining the whole. FIG. 5 shows the assembled microreactor.

  In FIG. 5, raw material A and raw material B supplied from the outside of the microreactor are introduced from ports 401 and 402, flow (recirculate) through loop flow paths 404 and 405, and are discharged from ports 410 and 403, respectively. During this time, a part of the raw material A and the raw material B flowing through the loop pipe passes through the flow paths 502 and 503 as branch flow paths communicating with the plurality of Y-shaped mixing / reaction flow paths 406, and each Y-flow The product is guided to the channel, mixed / reacted, and the product gathers at the center of the plurality of Y-shaped mixing / reaction channels 406 and is recovered outside the microreactor via the recovery channel 407.

  According to the present embodiment, in addition to the effects described in the first and second embodiments, in an application where the processing amount is not so large, the processing amount can be scaled up compactly inside the microreactor. In addition, since each Y-shaped mixing / reaction channel 406 from the loop channels 404 and 405 to the recovery channel 407 has the same length, the mixing / reaction conditions in each reaction channel 406 are the same, and the homogeneous The correct mixture / reaction can be collected. The feed state, pressure, and temperature of the raw materials in the loop flow paths 404 and 405 are made by monitoring means (not shown) provided outside the microreactor.

  In addition, according to the present embodiment, even when the processing amount is the same as in the first and second embodiments, the loop flow paths 404 and 405 are shortened, and the installation space can be reduced. it can.

  As mentioned above, although several Example of this invention was described, this invention is not limited to the above-mentioned example, A various deformation | transformation is possible in the range of the invention described in the claim.

  115, ... reactor, 117, 118, 502, 503 ... branch flow path, 109, 110, 113, 114, 404, 405 ... loop flow path (loop piping), 301 ... control unit, 303-305, 406 ... fine Flow path.

Claims (5)

In a chemical apparatus that supplies a plurality of different types of raw materials to a reactor and mixes or reacts in a fine channel inside the reactor to obtain a product,
A plurality of reactors and a plurality of loop flow paths for circulating a plurality of different types of raw materials, and a plurality of branches for supplying the raw materials from the middle of each loop flow path to the fine flow paths of the plurality of reactors A chemical apparatus comprising a flow path, wherein the loop flow path is set to a scale sufficiently larger than a scale of a fine flow path inside the reactor.   The chemical apparatus according to claim 1, further comprising a control unit that controls a flow rate, a pressure, and a temperature of the raw material in the loop flow path to desired values.   2. The chemical apparatus according to claim 1, wherein the loop flow path, the branch flow path, and the reactor are formed in the material plane portion by grooving or drilling.   The chemical apparatus according to any one of claims 1 to 3, wherein the plurality of loop flow paths and a plurality of branch flow paths are arranged inside the reactor.   A chemical apparatus comprising the chemical apparatus according to claim 1 or 2 connected in a plurality of stages.

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