JP5139628B2 - Micro chemical devices - Google Patents

Description

  The present invention relates to a microchemical device that mixes and reacts fluids using minute flow paths.

  A microchemical plant is a production facility that uses mixing, chemical reaction, separation, etc. in a microscale space, and has many advantages over conventional batch-type plants using large tanks and the like. For example, mixing of multiple fluids and chemical reactions can be performed in a short amount of time with a small amount of sample. It can be installed in equipment, can be applied to reactions involving dangers such as explosions, can be quickly adapted to the production of compounds that require high-mix low-volume production, and production volume can be easily adjusted to meet demand. It can be done. For this reason, in the fields of chemical industry and pharmaceutical industry, it has been attracting attention as a suitable apparatus for producing materials and products by mixing or reacting fluids, and research and development has been actively conducted in recent years.

  The micro chemical plant has, as main components, a material supply device, a micromixer, a heat exchange device, a microreactor, a separation device, piping connecting these devices, a control device, and the like. Among these, the micromixer and the microreactor each have a minute flow channel having a flow channel width on the order of several μm to 1 mm, and are mixed or mixed by bringing a plurality of types of fluids led to the flow channel into contact with each other. It causes a chemical reaction. The micromixer and the microreactor are basically configured in common, and are generally called a micromixer when the application is mixing, and called a microreactor when they are chemical reactions.

  Such a micromixer and a microreactor are very important devices in a microchemical plant, and some patent literatures are also presented. By connecting such a micromixer and a microreactor in this order, a microchemical device that performs mixing and chemical reaction in this order can be configured. Conventionally, for this connection, as shown in FIG. 8, for example, as shown in FIG. 8, the outlet P2 ′ in the micromixer 1 ′ and the inlet P3 ′ in the microreactor 7 ′ are connected to each other using a pipe NP such as a nipple or a tube. Was.

JP-A-2005-77219 JP 2005-46652 A

  However, when the micromixer 1 ′ and the microreactor 7 ′ are connected to each other through the pipe NP, the fluid may stay in the pipe NP. Further, before the fluid mixed in the micromixer 1 ′ is introduced into the microreactor 7 ′, a chemical reaction may occur due to the influence of a disturbance such as temperature fluctuation caused by heat dissipation or heat reception. The inside of the pipe NP is a space in which the temperature conditions and the like cannot be controlled, and the occurrence of such a chemical reaction before being introduced into the microreactor 7 ′ that performs precise reaction control leads to quality degradation of the product. The present invention has been made in view of such problems, and provides a microchemical device that can eliminate the influence of disturbance such as fluid retention and temperature fluctuation, and can improve the quality of a product. For the purpose.

According to the first aspect of the present invention, in the microchemical device MD that mixes and reacts a plurality of types of fluids to be reacted via the microchannel, the first inlet port P1 for introducing the fluid to be reacted and the first inlet port P1 The first micro flow paths 43R and 43L for communicating with the fluid to be reacted and the first outlet port P2 for communicating the mixed fluids to be communicated with the first micro flow paths 43R and 43L. A micromixer 1 provided, a second inlet port P3 for introducing the mixed fluid mixed by the micromixer 1, and a plurality of second microflows for reacting the mixed fluid in communication with the second inlet port P3 A microreactor 7 having a channel 91 and a second outlet port P4 that communicates with each of the second microchannels 91 and leads out a reacted fluid that has been reacted. Sa 1 and the microreactor 7, a first outlet port P2 and the second inlet port P3 is communicatively connected directly to the second inlet port P3 is have a plurality of tube support hole 92H that is Nuki穿in zigzag and, second microchannel 91 is tubular, by being supported by being fitted into each tube support hole 92H of the second inlet port P3, in communication with the second inlet port P3 are arranged in a staggered manner It is characterized by being.

  In the invention of claim 2, the surface on which the first outlet port P2 is formed and the surface on which the second inlet port P3 is formed are flat surfaces that can be in close contact with each other.

In the invention of claim 3, the cross-sectional areas of the first micro flow paths 43R and 43L and the second micro flow path 91 are each 0.5 mm ² or less.

  According to the microchemical device MD of the present invention, the first outlet port P2 in the micromixer 1 and the second inlet port P3 in the microreactor 7 are directly connected to each other without a pipe, so that fluid stays and temperature fluctuations occur. The influence of various disturbances can be eliminated, and the quality of the product can be improved.

  The best mode for carrying out the present invention will be described below with reference to the accompanying drawings. 1 is a partial front sectional view of a microchemical device according to the present invention, FIG. 2 is a partial front sectional view of a micromixer, FIG. 3 is a sectional view taken along line AA in FIG. 1, and FIG. FIG. 5 is a diagram schematically showing a micro flow path in the micromixer, FIG. 6 is a partial cross-sectional front view of the microreactor, and FIG. FIG. FIG. 4A shows the first element, and FIG. 4B shows the second element.

  As shown in FIG. 1, the microchemical device MD according to the present invention includes a micromixer 1 and a microreactor 7.

  As shown in FIG. 2, the micromixer 1 is composed of an outer shell 2, a lid 3 with a flow path forming body chamber, a flow path forming body 4, a plug 5, and the like, and a liquid to be reacted introduced from an inlet port P1. The monomer and the polymerization initiator are mixed in the flow path forming body 4 and led out from the outlet port P2. All the above components are made of stainless steel.

  The outer shell 2 is a bottomed cylindrical body having an opening at one end. The side wall 21 is provided with a coolant inlet port H1, a coolant outlet port H2, and a bolt fastening hole H3, and the bottom lid 22 is provided with a plug insertion hole H4. The coolant inlet port H1 and the coolant outlet port H2 are through holes formed in the thickness direction of the side wall 21 so as to be equidiagonal with respect to the axis J1 of the micromixer body. The bolt fastening holes H <b> 3 are bottomed holes that are formed in a total of six locations on the peripheral surface of the side wall 21 on the opening side so as to be equally spaced in the circumferential direction. The plug insertion hole H <b> 4 is a through hole formed in the thickness direction of the bottom lid 22. Each of these holes is formed with a female screw.

  The lid 3 with the flow path forming body chamber includes a lid 31 for sealing the opening of the outer shell 2, and a hollow columnar portion 32 extending in the direction of the axis J 1 from the center of one end of the lid 31. Consists of. The hollow portion in the columnar portion 32 functions as a flow path forming body chamber 32S for interior of the flow path forming body 4. The other end of the lid 31 is a flat surface. As shown in FIG. 3, a total of six bolt holes H <b> 5 are penetrated through the peripheral portion of the lid portion 31 so as to correspond to the positions of the bolt fastening holes H <b> 3 in the outer shell body 2. The lid portion 31 includes an outlet port P2 communicating with the flow path forming body chamber 32S in the cylindrical portion 32. The outer shell body 2 and the flow path forming body chamber-attached lid body 3 are integrated by fastening with a bolt B1 (see FIG. 1). A sealed space that functions as the coolant chamber 3S is formed between the outer peripheral surface of the columnar portion 32 and the inner peripheral surface of the outer shell 2. The coolant is supplied to the coolant chamber 3S from a coolant circulation pump (not shown) connected to the coolant inlet port H1 and the coolant outlet port H2 by piping.

The flow path forming body 4 is configured by connecting a plurality of first elements 4R and second elements 4L alternately in series. In this embodiment, there are five stages. As shown in FIG. 4A, the first element 4R has a pin hole 41 and a micro flow path 43R. Specifically, as shown in FIG. 5, two microchannels 43R1 and 43R2 each formed by partitioning the inside of the two through holes with partition walls BW each having a twist angle of 180 degrees in the clockwise direction. , 43R1 ′, 43R2 ′. The cross-sectional area of the through hole is 1 mm ² , and thus the cross-sectional area of each microchannel 43R is about 0.4 mm ^2.

  As shown in FIG. 4B, the second element 4L has a pin hole 41 and a micro flow path 43L. The second element 4L is basically the same except that it includes two microchannels each formed by partitioning the inside of the two through holes with a partition wall having a twist angle of 180 degrees in the counterclockwise direction. The configuration is the same as that of the first element 4R. The first element 4R and the second element 4L are integrated by connecting a total of five in series via pins 45 inserted into the pin holes 41, thereby forming the flow path forming body 4 to form the flow path. The interior of the body chamber 32S.

  The plug 5 includes an inlet port P1 penetrating in a constricted shape, and a male screw that can be screwed with a female screw of the plug hole H4 on the outer peripheral surface. The tip 51 of the plug 5 is fitted into the upstream side of the flow path forming body chamber 32S and serves as a pressing portion that can press the upstream end face of the flow path forming body 4. In a state where the flow path forming body 4 is installed, the flow path forming body 4 is fixedly held by fastening the plug 5 to the plug insertion hole H4 so as to press-contact the upstream end face of the flow path forming body 4. The inlet port P1 is connected to a reaction liquid supply system (not shown) by piping. The reaction liquid supply system is means for simultaneously feeding the monomer and the polymerization initiator to the micromixer 1 as the reaction liquid.

  When a polymer is produced by radical polymerization, for example, vinyl chloride, vinyl acetate, methyl acrylate, methyl methacrylate, acrylonitrile, styrene or the like is used as a monomer. Benzoyl oxide, 2,2-azobisisobutyronitrile and the like are used. When a polymer is produced by anionic polymerization, for example, styrene, acrylonitrile, methyl acrylate, methyl methacrylate or the like is used as a monomer, and as a polymerization initiator at that time, for example, butyl lithium, sodium, sodium phthalate, etc. Ren etc. are used.

  As shown in FIG. 6, the microreactor 7 includes a housing 8, a reaction chamber formation body 9, and a lid body 10. The microreactor 7 reacts in the reaction chamber formation body 9 with the mixed liquid to be reacted flowing from the inlet port P <b> 3. The device is derived from the outlet port P4. All the above components are made of stainless steel.

  The housing 8 is provided with a first large diameter portion 81 and a second large diameter portion 82 at both ends in the longitudinal direction, and is a substantially cylindrical body having a substantially H shape in front view. The side wall of the first large-diameter portion 81 is penetrated with a heat medium outlet port H6 toward the cavity of the housing 8, and a total of six bolt holes H8 are penetrated in a direction perpendicular to the penetration direction of the heat medium outlet port H6. Is done. An end portion of the inner peripheral surface of the first large diameter portion 81 has a groove portion 811. On the side wall of the second large diameter portion 82, a heat medium inlet port H7 toward the cavity is drilled, and a total of six bolt fastening holes H9 are drilled in a direction perpendicular to the penetration direction of the heat medium inlet port H7. . The bolt fastening holes H <b> 9 are bottomed holes that are formed in a total of six locations on the circumferential surface of the second large diameter portion 82 so as to be equally spaced in the circumferential direction. Each of these holes is formed with a female screw.

The reaction chamber forming body 9 includes a total of 19 fine-diameter tubes 91 and two supports 92 (92A and 92B) that support both ends of the fine-diameter tubes 91. Each support body 92 has a tube support hole 92H formed in a zigzag shape on the surface thereof. The small-diameter tube 91 has a cross-sectional area of 0.5 mm ² or less on its inner peripheral surface, and is supported at both ends by fitting both ends into tube support holes 92H of the respective supports 92 and fixing them by brazing or the like. The In the reaction chamber forming body 9 thus manufactured, first, the support 92B is inserted into the hollow portion 8S of the housing 8 from the opening on the first diameter large portion 81 side, and subsequently formed on the first diameter large portion 81 side. By engaging the support 92 </ b> A with the groove 811 formed, a total of 19 fine-diameter tubes 91 are arranged in the hollow portion 8 </ b> S of the housing 8. At this time, the end surface of the second large diameter portion 82 and the end surface of the support 92B are configured to be flush with each other, and the surface is a flat surface. Further, the end surface of the first large-diameter portion 81 and the end surface of the support 92A are configured to be flush with each other, and the surface is a flat surface. In addition, each opening part of the 19 fine diameter tubes 91 is equivalent to the 2nd inlet port of this invention.

  The lid 10 is sized to cover the opening on the second large diameter portion 82 side of the housing 8. A total of six bolt holes H10 are penetrated through the peripheral edge of the lid 10 so as to correspond to the positions of the bolt fastening holes H9 in the housing 8. The lid body 10 also includes an outlet port P4 that communicates with the fine-diameter tube 91 in the reaction chamber forming body 9. The lid 10 is attached to the housing 8 by tightening the bolt B1 such that the bolt hole H10 of the lid 10 and the bolt fastening hole H9 of the second large diameter portion 82 are aligned. In that case, you may provide sealing members, such as packing, between the support body 2B and the cover body 10. FIG. A sealed space that functions as the heat medium chamber 8 </ b> S is formed between the two support bodies 92 and the inner peripheral surface of the housing 8. A heat medium is supplied to the heat medium chamber 8S from a heat medium circulation pump (not shown) connected to the heat medium inlet port H7 and the heat medium outlet port H6 by piping.

  The micromixer 1 and the microreactor 7 configured as described above are the bolt hole H5 of the cover portion 31 in the micromixer 1, the bolt fastening hole H3 of the outer shell 2, and the bolt hole of the first large diameter portion 81 in the microreactor 7. The bolts B2 are tightened so that the positions of the bolts H8 are aligned with each other. Here, the other end of the lid portion 31 is a flat surface, and the end surface of the first large-diameter portion 81 is configured to be flush with the end surface of the support 92A, and the surface is a flat surface. The outlet port P2 in the micromixer 1 and the inlet port P3 in the microreactor 7 are in direct communication connection.

  Therefore, the inlet port P1 in the micromixer 1 and the outlet port P4 in the microreactor 7 communicate with each other through the microchannels 43R and 43L, the outlet port P2, and the fine diameter tube 91 in the channel formation body 4. . The reaction liquid pumped to the inlet port P1 by the reaction liquid supply system is first mixed in the micromixer 1 by flowing so as to alternately perform clockwise rotation and counterclockwise rotation. Subsequently, a chemical reaction is performed in the microreactor 7 and is led out from the outlet port P4.

  Since the outlet port P2 in the micromixer 1 and the inlet port P3 in the microreactor 7 are directly connected to each other without a pipe, the influence of disturbance such as fluid retention and temperature fluctuation can be eliminated, and the quality of the product is improved. Can be achieved.

  As mentioned above, although embodiment of this invention was described, embodiment disclosed above is an illustration to the last, Comprising: The scope of the present invention is not limited to these embodiment. The scope of the present invention is defined by the terms of the claims, and is intended to include any modifications within the scope and meaning equivalent to the terms of the claims.

1 is a partial front sectional view of a microchemical device according to the present invention. It is a partial front sectional view of a micromixer. It is an AA arrow line view of FIG. It is an external appearance perspective view of the 1st element and 2nd element which comprise a flow-path formation body. It is a figure which shows typically the micro flow path in a micro mixer. It is a front fragmentary sectional view of a microreactor. It is a BB line arrow line view of FIG. It is a front fragmentary sectional view of the conventional microchemical device.

Explanation of symbols

1 Micromixer 7 Microreactor 43 Microchannel (first microchannel)
91 Micro tube (second micro flow path)
MD micro chemical device P1 inlet port (first inlet port)
P2 exit port (1st exit port)
P3 inlet port (second inlet port)
P4 exit port (second exit port)

Claims (3)

In a microchemical device that mixes and reacts a plurality of types of fluids to be reacted via a microchannel, a first inlet port for introducing the fluid to be reacted and a fluid to be reacted communicated with the first inlet port A micromixer having a first microchannel and a first outlet port communicating with the first microchannel to extract a mixed fluid to be reacted, and the mixed fluid mixed by the micromixer is introduced A second inlet port for communicating with the second inlet port, a plurality of second microchannels for reacting the mixed fluid, and a reacted fluid that has been reacted by communicating with each second microchannel and a microreactor and a second outlet port for a micro mixer and micro reactor, a first outlet port and the second inlet port is communicatively connected directly to the Inlet port has a plurality of tube support hole which is Nuki穿in zigzag, the second microchannel is tubular, by being supported by being fitted into each tube support holes of the second inlet port, a staggered A microchemical device that is arranged in a line and communicates with a second inlet port.   The microchemical device according to claim 1, wherein the surface on which the first outlet port is formed and the surface on which the second inlet port is formed are flat surfaces that can be in close contact with each other. The microchemical device according to claim 1 or ^{2, wherein} each of the first microchannel and the second microchannel has a cross-sectional area of 0.5 mm ² or less.

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