JP2007307440A - Chemical reaction apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a chemical reaction apparatus in which even such a reaction that the diffusion of a raw material molecule is a rate controlling factor can be advanced at a high speed, a reaction of a liquid mixture can be advanced at a high rate and the production of by-products can be restrained and which can be used in a wide range of organic synthesis reactions. <P>SOLUTION: The chemical reaction apparatus 10 is provided with: a liquid raw material supply line 12 for supplying two or more liquid raw materials 14, 16 to a reaction tank 34; and a microwave emitting unit 52 for irradiating the liquid mixture 36, which is supplied to the reaction tank 34 through the liquid raw material supply line 12, with a microwave to advance the reaction of the liquid mixture 36. A micro mixer 30 is arranged on the liquid raw material supply line 12, which has a plurality of micro introduction pipelines which are used for introducing two or more liquid raw materials 14, 16 and each of which has a micrometer-sized pipeline diameter, a mixing part for joining the plurality of micro introduction pipelines to one another so that two or more liquid raw materials 14, 16 are merged and mixed with one another, and a micro discharge pipeline which is used for discharging the liquid mixture 36 mixed in the mixing part and has a micrometer-sized pipeline diameter. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a chemical reaction apparatus having a microwave irradiation unit for promoting a chemical reaction.

  Today, microwaves are used in cooking microwave ovens and are widely used in homes. It is also used industrially for rubber vulcanization, tea leaf drying, food sterilization and the like. On the other hand, the application of microwaves to chemical synthesis processes, particularly organic synthesis reactions, was slow compared to these, but in recent years its usefulness has been recognized and application to processes has begun. By irradiating the chemical reaction field with microwaves, if the raw material is a substance with a large dielectric loss, the temperature can be increased more rapidly than the conventional method of ripening from the outer jacket of the reaction vessel, and the reaction speed can be increased. Is possible. In addition, by rapidly applying energy to the reaction field, it is possible to expect an improvement in the selectivity of the target product, which was not seen in the conventional external heat transfer system. And the patent regarding the basic composition about the chemical reaction promotion method using a microwave and the chemical reaction promotion apparatus used for it is applied (patent document 1).

On the other hand, a microreactor is a general term for a microreactor having a channel having a width of 10 to 500 μm, and performs mixing, heat exchange, chemical reaction, and the like therein. Microreactors enable rapid mixing at the molecular level and uniform temperature control, and are expected to speed up chemical reactions and improve selectivity.
Japanese Patent Publication No. 7-63619

  However, a chemical reaction apparatus having a microwave irradiation apparatus can heat a raw material solution at a high speed, but the mixing of two or more raw material liquids is performed by a stirrer equipped with a stirring blade as in the conventional reaction apparatus. Therefore, density unevenness occurs at the molecular level in the reaction vessel. For this reason, in the reaction system in which the reaction rate depends on the diffusion rate of the raw material molecules, the reaction rate of the mixed solution may be low because it is difficult to speed up the reaction. In addition, in a portion where the raw material is unevenly distributed locally at the molecular level, there is a case where the reaction proceeds excessively and a by-product is generated instead of the target product.

  On the other hand, the microreactor has a fine flow path, and can precisely mix the raw material liquids at the point where two or more fine flow paths intersect. In addition, since the channel is narrow, precise temperature control is possible by heating and cooling the channel from the outside. When the speed of the chemical reaction and the improvement of the reaction rate occur in the microreactor, the diffusion of the raw material molecules is rate-determining at the reaction rate. In the reaction system in which the chemical reaction itself is rate-limiting, it is not possible to increase the speed of the reaction. Further, when a solid catalyst is used as a catalyst in a chemical reaction, it cannot be used because of clogging. In addition, when the chemical reaction is organic synthesis, when the raw material liquid has a boiling point lower than the reaction temperature, the gasified raw material liquid accumulates in the flow path or the electromagnetic valve, obstructs the flow, or the raw material liquid is localized due to gasification. May cause uneven concentration of raw material liquid. Therefore, the microreactor may not be applied as a reaction field.

  The present invention has been made in view of such circumstances, and eliminates the drawbacks of the prior art described above, speeding up the reaction even when the rate of diffusion of the starting material molecules is rate-limiting, and increasing the reaction rate of the mixed liquid. An object of the present invention is to provide a chemical reaction apparatus that can suppress the production of products and can be used for a wide range of organic synthesis reactions.

  According to the first aspect of the present invention, a raw material liquid supply line that supplies two or more kinds of raw material liquids to a reaction tank, and a mixed liquid supplied from the raw material liquid supply line to the reaction tank is irradiated with microwaves and mixed. And a microwave irradiation device for promoting a reaction of the liquid, wherein the raw material liquid supply line is a plurality of pipe lines for introducing the two or more kinds of raw material liquids, each having a pipe diameter. A micro-order fine introduction path, a mixing part for mixing raw material liquids by joining the fine introduction paths so that the two or more kinds of raw material liquids merge, and a mixed liquid mixed in the mixing part It is characterized by comprising a micromixer having a single conduit led out from the mixing section and having a fine lead-out passage with a micro-order pipe diameter.

  According to claim 1, in the chemical reaction device including a microwave irradiation device for irradiating microwaves, a fine flow channel having a tube diameter of micro-order, each passing two or more kinds of raw material liquids through the raw material liquid supply line; By providing a micromixer that has a contact point that joins two or more kinds of raw material liquids by joining the microchannels, even in reaction systems where the diffusion of raw material molecules is rate-determined, precise mixing at the molecular level using the micromixer After performing the process, the microwave irradiation device irradiates the mixture with microwaves and reacts, so a high-efficiency reaction that increases the reaction rate of the mixture can be realized, the yield can be improved, and the reaction can proceed too much. By-product is reduced because it decreases.

  Further, even in a reaction system in which the reaction is rate-determining, the reaction rate is increased and the high-speed reaction can be performed by irradiating the microwave with a microwave irradiation apparatus. That is, even in a reaction system in which molecular diffusion is rate-limiting and the reaction is rate-limiting, the reaction rate can be increased and a high yield can be realized.

  Even when a solid catalyst is used for the reaction, the mixture is mixed after being precisely mixed by the micromixer into the reaction tank of the chemical reaction apparatus, and at the same time, the reaction is performed by introducing the solid catalyst into the reaction tank. be able to.

  Here, the tube diameter of the micro order is preferably a tube diameter of 50 μm or less.

  According to a second aspect of the present invention, in the first aspect of the invention, the microwave irradiation apparatus includes a circulation pipe that circulates the mixed liquid in the reaction tank, and the mixed liquid that flows through the circulation pipe. It is characterized by irradiating microwaves.

  According to claim 2, even in a synthesis reaction using an organic solvent, which is difficult to apply only with a microreactor, after performing precise mixing at a molecular level with a micromixer, a microwave irradiation device provided with a circulation tube, By performing the reaction by irradiating microwaves and applying a predetermined temperature, the reaction rate is high and a high-speed reaction can be performed.

  According to a third aspect of the present invention, in the first or second aspect of the invention, the raw material liquid supply line is branched with respect to each of the two or more types of raw material liquids, and the micromixer is provided for each branch. It is provided.

  According to claim 3, the supply line is branched for each of two or more kinds of raw material liquids, and a micromixer is provided for each branch, so that a large amount of raw material liquids can be quickly and precisely mixed at the molecular level. It can be performed.

  According to the present invention, even a reaction in which the diffusion of raw material molecules is rate-limiting, the reaction can be accelerated, the reaction rate of the mixed solution can be increased, the production of by-products can be suppressed, and it can be used for a wide range of organic synthesis reactions.

  Hereinafter, embodiments of a chemical reaction apparatus according to the present invention will be described in detail with reference to the accompanying drawings.

  FIG. 1 is an explanatory diagram of a chemical reaction apparatus 10 according to the first embodiment. As illustrated, the raw material liquid A14 and the raw material liquid B16 are stored in the raw material liquid A tank 18 and the raw material liquid B tank 20, respectively. First, in the raw material liquid supply line 12, the raw material liquid A 14 and the raw material liquid B 16 are passed through the raw material liquid A supply pipe 26 and the raw material liquid B supply pipe 28 by the raw material liquid A supply pump 22 and the raw material liquid B supply pump 24. Then, it is transferred to the micromixer 30. In the micromixer 30, the raw material liquid is introduced into a micro flow channel having a micro-order pipe diameter, and a state close to complete mixing at the molecular level is created at the contact point of the micro flow channel for mixing the raw material liquids. The mixed solution mixed by the micromixer 30 is sent to the reaction tank 34 via the raw material liquid supply pipe 32.

  The reaction tank 34 is a tank provided with a jacket on the outside, and a cooling brine 38 for precisely controlling the temperature of the mixed liquid 36 in which the raw material liquid A14 and the raw material liquid B16 are mixed can be held in the outer jacket. . The brine 38 is stored in a brine tank 40 and is cooled to a predetermined temperature by a cooler 42. The brine 38 in the brine tank 40 is sent to the jacket portion of the reaction tank 34 by the brine supply pump 44, and circulates back to the brine tank 40 via the brine pipe 46. The liquid mixture 36 sent to the reaction tank 34 is mixed by a stirrer 50 equipped with a stirring blade 48 to reduce the temperature distribution in the tank. At this time, when a solid catalyst other than the raw material liquid A14 and the raw material liquid B16 is required for the reaction, the solid catalyst is charged into the mixed liquid 36 and stirred.

  The chemical reaction apparatus 10 is provided with a microwave irradiation device 52. A waveguide 54 of a microwave irradiation device 52 is connected to the reaction tank 34 at the top, and a microwave generator 56 is installed at the other end of the waveguide 54. The microwave converted from the electric energy by the microwave generator 56 is irradiated to the circulating liquid mixture 36.

  Unlike the normal external heating method, the liquid mixture 36 irradiated with microwaves reacts at high speed because the liquid mixture itself is uniformly heated by the spin motion of polarized molecules or clusters in which the molecules are associated. The reaction tank 34 is provided with a temperature sensor 58 and a thermometer 60 for measuring the representative temperature of the mixed liquid 36. The microwave generator 56 is controlled by a controller 62 linked to the thermometer 60 so that the temperature of the mixed liquid 36 detected by the thermometer 60 becomes a predetermined temperature. Control of the microwave generator 56 includes a method of repeatedly operating and stopping the microwave output while keeping the output constant, and a method of controlling the temperature of the liquid mixture 36 by raising and lowering the output variable.

  Thus, by using the chemical reaction apparatus 10 of the present invention, it is possible to increase the reaction rate and suppress by-products. That is, in the reaction system in which the diffusion of the raw material molecules is rate-determined, the micromixer 30 performs precise mixing at the molecular level, and then the microwave irradiation device 52 irradiates the mixture with the microwave to cause the reaction. A high-efficiency reaction that increases the reaction rate can be realized, the yield is improved, and by-products are suppressed because the reaction is less likely to proceed excessively. Further, even in a reaction system in which the reaction is rate-limiting, by irradiating the microwave with the microwave irradiation device 52, the reaction rate is increased and a high-speed reaction can be performed. That is, even in a reaction system in which molecular diffusion is rate-limiting and the reaction is rate-limiting, the reaction rate can be increased and a high yield can be realized. Even when a solid catalyst is used for the reaction, the mixed liquid after the precision mixing by the micromixer 30 is supplied into the reaction tank 34 of the chemical reaction apparatus 10 and at the same time, the solid catalyst is put into the reaction tank 34. The reaction can be carried out with

  FIG. 2 is an explanatory diagram of the micromixer 30. The micromixer 30 is provided with one or more chips 30a in the micromixer. The two fine introduction pipes 31a and 31a of the chip 30a in the micromixer are provided with the raw material liquid A supply pipe 26 and the raw material liquid B supply. A pipe 28 is connected to each other. The raw material liquid A and the raw material liquid B injected from the raw material liquid A supply pipe 26 and the raw material liquid B supply pipe 28 come into contact with each other at the junction 31b via the fine introduction pipes 31a and 31a. The fine lead-out pipe 31c flows while being precisely mixed at the level. The mixed liquid mixed in the fine outlet pipe 31 c is sent to the raw material liquid supply pipe 32.

  FIG. 3 is an explanatory diagram of a chemical reaction apparatus 70 according to the second embodiment. The raw material liquid supply line 12 and the cooling unit for the mixed liquid 36 are the same as those in FIG. What is different from FIG. 1 is a microwave irradiation device 52 ′, which is a method of irradiating the mixed liquid 36 with microwaves. In the chemical reaction apparatus 70, a part of the mixed solution 36 is sent to the circulation pipe 72 outside the reaction tank 34 by the circulation pump 74. Microwaves converted from electrical energy by the microwave generator 56 are applied to the circulating mixed liquid 36 at a location where the waveguide 54 and the circulation pipe 72 located in the middle of the circulation pipe 72 intersect. When the liquid temperature of the mixed liquid 36 irradiated with microwaves is measured by the temperature sensor 58 and the thermometer 60 arranged at the subsequent stage of the waveguide 54 and becomes higher than a predetermined temperature, the temperature sensor 58 is interlocked with the thermometer 60. The controller 62 controls the microwave generator 56 so that the mixed liquid 36 has a constant temperature. The mixed liquid 36 irradiated with the microwave is returned to the reaction vessel 34.

  By using the chemical reaction device 70 in this way, even in a synthesis reaction using an organic solvent, which is difficult to apply only with a microreactor, the micromixer 30 performs precise mixing at the molecular level, and then a circulation pipe 72 is provided. In addition, by performing the reaction by applying a predetermined temperature with the microwave irradiation device 52, the reaction rate is high and a high-speed reaction can be performed.

  FIG. 4 is an explanatory diagram of a raw material liquid supply line 12 ′ which is another embodiment of the raw material liquid supply line 12 according to the chemical reaction apparatus 10, 70 of the present invention. As shown in the drawing, the raw material liquid A14 and the raw material liquid B16 are divided into a raw material liquid A supply pipe 26 branched by a raw material liquid A supply pump 22 and a raw material liquid B supply pump 24 and a raw material liquid B supply pipe 28 branched. To the micromixers 30, 30. The micromixer 30 is configured by a micro flow path having a micro diameter, but the flow rate of the raw material liquid that can flow is limited to a small amount because the flow path is fine. Therefore, as shown in FIG. 3, the raw material liquid supply line 12 ′ includes two or more micromixers 30, and the raw material liquid discharged from the raw material liquid supply pump is distributed, and a number of micromixers 30, 30 ... mixed. Here, if the distribution of the raw material liquid from the raw material liquid supply pump to the micromixers 30, 30... Is not performed uniformly, a flow meter and a control valve are provided in the branched pipe so that the flow rate becomes uniform. You may control. The mixed liquid mixed by the micromixers 30, 30... Is sent to the reaction tank 34 through the raw material liquid supply pipe 32. By using such a raw material liquid supply line 12 ′, a large liquid mixture flow rate can be sent to the reaction vessel 34.

  FIG. 5 is an explanatory diagram of another form of the chemical reaction device 10 according to the first embodiment. If the raw material liquid A14 and / or the raw material liquid B16 has a boiling point equal to or lower than the reaction temperature, as shown in FIG. 5, a reflux pipe 76 is installed in the reaction tank 34, and the mixed liquid evaporated during the reaction. A part of 36 is cooled by the refrigerant pipe 78 of the reflux pipe 76, and can be returned to the reaction tank 34 as a liquid.

  FIG. 6 is an explanatory diagram of another form of the chemical reaction device 70 according to the second embodiment. A reflux pipe 76 is installed in the reaction tank 34, and a part of the mixed liquid 36 evaporated during the reaction is cooled by the refrigerant pipe 78 of the reflux pipe 76, so that it can be returned to the reaction tank 34 as a liquid.

  Moreover, FIG. 7 is explanatory drawing of another form of the chemical reaction apparatus 10 which concerns on 1st Embodiment. The introduced mixed liquid reacts in the reaction tank 34, and the reacted liquid (product) can be continuously transferred to the product tank 82 by the product extraction pump 80.

It is explanatory drawing of the chemical reaction apparatus which concerns on 1st Embodiment. It is explanatory drawing of the micromixer which concerns on this invention. It is explanatory drawing of the chemical reaction apparatus which concerns on 2nd Embodiment. It is explanatory drawing of the other raw material liquid supply line which concerns on embodiment. It is explanatory drawing of another form of the chemical reaction apparatus which concerns on 1st Embodiment. It is explanatory drawing of another form of the chemical reaction apparatus which concerns on 2nd Embodiment. It is explanatory drawing of another form of the chemical reaction apparatus which concerns on 1st Embodiment.

Explanation of symbols

DESCRIPTION OF SYMBOLS 10, 10 ', 10''... Chemical reaction apparatus, 12, 12' ... Raw material liquid supply line, 14 ... Raw material liquid A, 16 ... Raw material liquid B, 18 ... Raw material liquid A tank, 20 ... Raw material liquid B tank, 22 ... Raw material liquid A supply pump, 24 ... Raw material liquid B supply pump, 26 ... Raw material liquid A supply pipe, 28 ... Raw material liquid B supply pipe, 30 ... Micromixer, 30a ... Chip in micromixer, 31a ... Fine introduction pipe , 31b ... Junction section, 31c ... Fine outlet pipe, 32 ... Pipe for supplying raw material liquid, 34 ... Reaction tank, 36 ... Mixed liquid, 38 ... Brine, 40 ... Brine tank, 42 ... Cooler, 44 ... Brine supply pump, 46 Pipe for brine, 48 agitating blade, 50 agitator, 52, 52 ′, microwave irradiation device, 54 waveguide, 56 microwave generator, 58 temperature sensor, 60 thermometer, 62 control 70, 70 '... chemical reaction Device, 72 ... circulating pipe, 74 ... circulation pump, 76 ... return pipe, 78 ... refrigerant pipe, 80 ... product discharge pump, 82 ... product tank

Claims (3)

Microwave irradiation for irradiating microwaves to the liquid mixture supplied to the reaction tank from the raw material liquid supply line by supplying two or more kinds of raw material liquids to the reaction tank and accelerating the reaction of the mixed liquid A chemical reaction device comprising:
In the raw material liquid supply line,
A plurality of pipelines for introducing the two or more kinds of raw material liquids, respectively, and a micro-introduction channel having a pipeline diameter of micro-order;
A mixing unit for mixing the raw material liquids by joining the fine introduction paths so that the two or more kinds of raw material liquids merge;
A chemical reaction apparatus comprising: a micromixer having a single liquid channel for extracting the mixed liquid mixed in the mixing unit from the mixing unit, and a fine channel having a micro pipe diameter. .   The said microwave irradiation apparatus is provided with the circulation pipe which circulates the said liquid mixture in the said reaction tank, and irradiates a microwave with respect to the liquid mixture which flows through this circulation pipe. Chemical reactor.   The chemical solution according to claim 1 or 2, wherein the raw material liquid supply line is branched with respect to each of the two or more kinds of raw material liquids, and the micromixer is provided for each branch. Reactor.

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