JP2010005582A - Blocking prevention device of micro-channel and blocking prevention method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a blocking prevention device of a micro-channel which reduces the expense of working cost and time cost in maintenance of a micro-reactor to enhance the productivity and to provide a blocking prevention method. <P>SOLUTION: The blocking prevention device of the micro-channel is provided with a passage formed body (11) to form the micro-channel (R) that advances the reaction of a fluid (L3) to be reacted and an ultrasonic vibration imparting means (13) to impart the ultrasonic vibration to the passage formed body (11). The ultrasonic vibration that the ultrasonic vibration imparting means (13) emits is transmitted to the fluid (L3) to be reacted flowing in the micro-channel (R) via the passage formed body (11). The characteristics of vibration is set to the frequency and amplitude so as to inhibit the bonding between molecules because the molecule of the fluid (L3) within the micro-channel (R) generates microvibration. Thus, the accumulation of high-viscosity fluid or granules that can be produced during the reaction progress, or the deposit of crystal is avoided. Resultingly, the blocking of the micro-channel (R) can be prevented. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to a microchannel blockage prevention device and a blockage prevention method. More specifically, the present invention relates to an apparatus and a method for preventing clogging of a microchannel in a microreactor that causes a reaction of a reaction fluid in the microchannel.

  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, and if the production technology of the product can be established at the laboratory level because the device is small, it can be easily used for mass production by numbering up. 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.

In a microchemical plant, a microreactor having a microchannel is used. The microchannel has a channel width on the order of several μm to several mm. As publicly known literatures concerning such microreactors, for example, the following patent documents 1 to 4 can be cited. Patent Document 1 discloses a tube body arranged in a zigzag straight line to form a microchannel. Japanese Patent Application Laid-Open No. H10-228667 discloses a micro-channel formed by spirally winding a tube body. Patent Document 3 has a micro-channel having an inlet portion branched in a substantially Y shape, and the first fluid is press-fitted and supplied from one inlet, and the second fluid is press-fitted and supplied from the other inlet. An interface contact is disclosed. Patent Document 4 discloses a micro flow path that alternately repeats clockwise rotation and counterclockwise rotation.
JP 2007-007570 A JP 2007-029887 A JP 2006-239640 A JP 2006-305505 A

The microchannels in the above microreactors are all narrow channels with a cross-sectional area of several mm ² or less when cut by a plane perpendicular to the flow direction, and therefore, increase the viscosity of the fluid or precipitation of granules and crystals. When used for reaction, the flow path may be blocked. Blockage of the flow path can be prevented or dealt with by periodically disassembling and cleaning the microreactor or flowing a cleaning solution into the microflow path, but this requires a lot of work and time costs for maintenance, and production It causes a decline in sex.

  The present invention has been made in view of such a problem, and it is possible to reduce the work cost and time cost for maintenance of the microreactor, and thus the productivity can be improved. And it aims at providing the obstruction | occlusion prevention method.

The above object is achieved by the present invention described below. The reference numerals in parentheses attached to each component in the “Claims” and “Means for Solving the Problems” column indicate the correspondence with the specific means described in the embodiments described later. It is.

  According to the first aspect of the present invention, ultrasonic vibration is applied to the flow path forming body (11) forming the micro flow path (R) for advancing the reaction of the reaction fluid (L3) and the flow path forming body (11). Ultrasonic vibration applying means (13) for applying is provided.

  According to the invention of claim 1, the ultrasonic vibration applying means (13) can emit ultrasonic vibration while the reaction fluid (L3) is proceeding with the reaction in the micro flow path (R). . The ultrasonic vibration generated by the ultrasonic vibration applying means (13) is transmitted to the reaction fluid (L3) flowing in the micro flow path (R) through the flow path forming body (11). This vibration characteristic is set to a frequency and an amplitude at which molecules of the reaction fluid (L3) in the micro flow channel (R) generate a minute vibration and prevent a bond between the molecules. This avoids the accumulation of deposits of highly viscous fluids or granules or crystals that can occur during the course of the reaction, and as a result, blockage of the microchannel (R) is prevented. In the present invention, the fluid in the middle of the reaction is also included in the reaction fluid (L3). Moreover, the application of ultrasonic vibration may be either continuous or intermittent.

  In the invention of claim 2, the ultrasonic vibration applying means (13) applies ultrasonic vibration to the flow path forming body (11) from the outside of the flow path forming body (11).

  According to the invention of claim 2, the ultrasonic vibration applying means (13) is provided, for example, in the microchannel (R), or a recess is formed on the inner wall of the microchannel (R), and is provided in the recess. Instead, it can be provided outside the flow path forming body (11). Since ultrasonic vibration is propagated from the outside of the flow path forming body (11) to the reaction fluid (L3) in the micro flow path (R) by applying ultrasonic vibration to the flow path forming body (11), Compared with the case where the ultrasonic vibration applying means (13) is provided in the micro-channel (R) or the like, the reaction fluid (L3) does not stay and the channel is less polluted (contamination).

  The invention of claim 3 includes a cooling means (60) for cooling the ultrasonic vibration applying means (13).

  According to the invention of claim 3, it is possible to suppress the temperature rise due to the heat generation of the ultrasonic vibration applying means (13) itself due to the generation of ultrasonic vibration, and the ultrasonic vibration applying means (13) malfunctions due to the temperature rise. And fluctuations in the generated frequency can be eliminated.

  In the invention of claim 4, the liquid chamber (12H) for interposing the liquid (W1) is provided between the ultrasonic vibration applying means (13) and the flow path forming body (11), and the ultrasonic vibration applying means (13). Applies ultrasonic vibration to the flow path forming body (11) using the liquid (W1) as a propagation medium of ultrasonic vibration.

  According to the invention of claim 4, the ultrasonic vibration applying means (13) applies ultrasonic vibration to the flow path forming body (11) using the liquid (W1) as a propagation medium of ultrasonic vibration. As a result, the ultrasonic vibration applied to the flow path forming body (11) is not localized and is uniform throughout the flow path forming body (11). It is possible to achieve blockage prevention without wrinkles.

  The invention of claim 5 includes a liquid temperature adjusting means (55) for adjusting the temperature of the liquid (W1) in the liquid chamber (12H).

  According to the invention of claim 5, by adjusting the temperature of the liquid (W1) in the liquid chamber (12H) by the liquid temperature adjusting means (55), the reaction fluid (L3) in the microchannel (R) is adjusted. The temperature can be controlled, and a high-quality reaction with high accuracy can be achieved. Thus, the liquid (W1) is provided with functions for both ultrasonic wave propagation and temperature adjustment in the liquid chamber (12H) which is one sealed space, and the apparatus efficiency is high.

  According to the sixth aspect of the present invention, ultrasonic vibration is applied to the flow path forming body (11) that forms the micro flow path (R) for advancing the reaction of the reaction fluid (L3) by the ultrasonic vibration applying means (13). To prevent the microchannel (R) from being blocked.

  According to the sixth aspect of the invention, similarly to the effect of the first aspect, the molecules of the fluid to be reacted (L3) generate minute vibrations and impart ultrasonic vibration having vibration characteristics for preventing the bonds between the molecules. This prevents the micro flow path (R) from being blocked.

  According to the present invention, it is possible to provide a microchannel blockage prevention device and a blockage prevention method that can reduce the work cost and time cost required for maintenance of a microreactor and thereby improve productivity.

  The best mode for carrying out the present invention will be described below with reference to the accompanying drawings. FIG. 1 is a schematic configuration diagram showing a microchemical plant 100 including a microchannel blockage prevention device 10 according to the present invention, and FIG. 2 is a partial front cross-sectional view showing a configuration overview of the microchannel blockage prevention device 10 according to the present invention. FIG. 3, FIG. 3 is a side sectional view showing an outline of the configuration of the microchannel blockage prevention device 10 according to the present invention, FIG. 4 is a front sectional view showing the schematic configuration of the ultrasonic transducer 13, and FIG. FIG. 2 is a partial cross-sectional view of two surfaces showing a flow path forming body 11 ′ (FIG. A shows a plan partial cross-sectional view and FIG. B shows a front partial cross-sectional view).

  As shown in FIG. 1, the microchemical plant 100 includes a microchannel blockage prevention device 10, a mixing unit 20, a first liquid supply unit 30, a second liquid supply unit 40, a thermal refrigerant circulation unit 50, and a cooling gas circulation unit. 60, a control unit 70 and a power source 80.

  As shown in FIGS. 2 and 3, the microchannel blockage prevention device 10 includes a channel formation body 11, a casing 12, and an ultrasonic transducer 13.

The flow path forming body 11 is obtained by winding a long flexible tube body into a coil shape. This tube body has a hollow portion having a cross-sectional area of 1 μm ² or more and several mm ² or less when cut by a plane perpendicular to the flow direction. Forming. The material of the flow path forming body 11 is not eroded or corroded by these liquids depending on the types of the liquid to be reacted, the liquid in the middle of the reaction, and the reacted liquid flowing through the micro flow path R. For example, a metal such as stainless steel or Hastelloy (registered trademark of US Haynes International) or a resin having high chemical resistance or corrosion resistance such as Teflon (registered trademark of US DuPont) can be used.

  The casing 12 includes an inner cylinder 1, an outer cylinder 2, a horizontal lid 3, and a horizontal lid 4, and a thermal refrigerant chamber 12H and a cooling gas chamber 12C are formed therein. The inner cylinder 1 is a cylindrical body that surrounds the flow path forming body 11. The outer cylinder 2 is a cylindrical body in which the inner cylinder 1 is nested while being arranged concentrically with the inner cylinder 1. The horizontal lid 3 is provided on one end side of the outer cylinder 2 and the inner cylinder 1 so as to close their openings. An inlet port 11I that communicates with one end of the microchannel R and serves as an inlet of the reaction liquid L3 is provided at the center of the horizontal lid 3. The horizontal lid 4 is provided on the other end side of the outer cylinder 2 and the inner cylinder 1 so as to close their openings. An outlet port 11D that communicates with the other end of the microchannel R and serves as an outlet of the reacted liquid L4 is provided at the center of the horizontal lid 4.

  The thermal refrigerant chamber 12H is a sealed space surrounded by the inner circumferential surface of the inner cylinder 1, the inner side surface of the horizontal lid 3, and the inner side surface of the horizontal lid 4, and this sealed space is a thermal refrigerant (heat medium or refrigerant) W1. Has come to circulate. For example, cold water, hot water, hot water, or the like is used as the thermal refrigerant W1. The cooling gas chamber 12 </ b> C is a sealed space surrounded by the inner peripheral surface of the outer cylinder 2, the outer peripheral surface of the inner cylinder 1, the inner side surface of the horizontal lid 3, and the inner side surface of the horizontal lid 4. The working gas W2 is circulated. For the cooling gas W2, for example, a low-temperature gas such as cooling air is used. The inner cylinder 1 is formed with an inlet port 1I that communicates with the thermal refrigerant chamber 12H and serves as an inlet for the thermal refrigerant W1, and an outlet port 1D that serves as an outlet. The outer cylinder 2 is formed with an inlet port 2I that communicates with the cooling gas chamber 12C and serves as an inlet for the cooling gas W2, and an outlet port 2D that serves as an outlet.

  The casing 12 is provided with a liquid temperature sensor 14. The liquid temperature sensor 14 is configured to measure the temperature of the thermal refrigerant W1 flowing through the thermal refrigerant chamber 12H and send the temperature signal S1 to the control unit 70.

  As shown in FIG. 4, the ultrasonic transducer 13 includes a piezoelectric material 131 that is an ultrasonic wave generation source, electrodes 132 and 133 that are provided above and below the piezoelectric material 131, and a sound absorbing material that is attached to the surface of the lower electrode 133. The acoustic matching layer 135 is attached to the surface of the material 134 and the upper electrode 132. The ultrasonic transducer 13 is a flexible type that can be curved by bending the upper surface (ultrasonic radiation surface) 136 into a concave shape. As shown in FIG. 3, the ultrasonic transducer 13 is attached to two locations on the outer peripheral surface of the inner cylinder 1 by an adhering means such as an adhesive, with the upper surface 136 curved in a concave shape. The ultrasonic transducer 13 is supplied with power from a power source 80. The characteristic of the vibration generated by the ultrasonic transducer 13 is variable by the control signal S3.

Returning to FIG. 1, the mixing unit 20 joins the first liquid L1 that is the reaction liquid before mixing and the second liquid L2 that is the reaction liquid before mixing, and then mixes both liquids. , and the outlet port 20D for deriving the inlet port 20I ₁ and the inlet port 20I _2, blended of the reaction liquid L3 for introducing a respective first liquid L1 and second liquid L2, and the inlet port 20I ₁ and an inlet port 20I ₂ and the flow passage forming body 21 for mixing disposed between the outlet port 20D. The flow path forming body 21 can be formed of a tube body wound in a coil shape in the same manner as the flow path forming body 11.

The first liquid supply unit 30 includes a first liquid storage tank 31, and the like pump 32 and valve 33, is connected to the inlet port 20I ₁ of the mixing device 20 through the pipe 34, the first liquid L1 at a predetermined pressure It is configured to be pumpable. The second liquid supply unit 40, similarly to the first liquid supply unit 30, the second liquid storage tank 41, and the like pump 42 and valve 43, is connected to the inlet port 20I ₂ of the mixing device 20 via a pipe 44 The second liquid L2 is configured to be pumped at a predetermined pressure.

  The thermal refrigerant circulation unit 50 includes a thermal refrigerant storage tank 51, a pump 52, a valve 53, a temperature control unit 55, and the like, and is connected to an inlet port 1I and an outlet port 1D of the microchannel blockage prevention device 10 via a pipe 54. The heat refrigerant W1 is configured to circulate at a predetermined flow rate in the heat refrigerant chamber 12H.

  The cooling gas circulation unit 60 includes a cooling gas generation unit 61, a pump 62, a valve 63, and the like, and is connected to the inlet port 2I and the outlet port 2D of the microchannel blockage prevention device 10 via the pipe 64 for cooling. The gas W2 is configured to circulate at a predetermined pressure in the cooling gas chamber 12C.

  Based on the temperature signal S1 sent from the liquid temperature sensor 14, the control unit 70 heats or cools the thermal refrigerant W1 so that the temperature of the reaction liquid L3 flowing through the microchannel R becomes an optimum temperature for the reaction. Thus, the temperature of the reaction liquid L3 is controlled. This control is performed by a control signal S2. Further, the control unit 70 can set and change the amplitude and frequency of the power supply 80 so that the characteristics of the vibration generated by the ultrasonic transducer 13 change according to the reaction mode. The vibration characteristic is selected such that the molecules of the reaction liquid L3 flowing through the micro flow path R generate minute vibrations and prevent the bonds between the molecules. This control is performed by a control signal S3.

  Next, the operation and effect of the microchemical plant 100 will be described. In FIG. 1, the first liquid L <b> 1 and the second liquid L <b> 2 derived from the first liquid supply unit 30 and the second liquid supply unit 40 at a predetermined pressure, respectively, are introduced into the mixing unit 20. After the first liquid L1 and the second liquid L2 introduced into the mixing unit 20 merge at the merge point r0, the mixing proceeds by passing through the flow path formed in the flow path forming body 21, After the mixing is completed, the reaction liquid L3 is derived. The to-be-reacted liquid L3 led out from the mixing unit 20 is introduced into the inlet port 11I of the flow path forming body 11 to advance the reaction while passing through the micro flow path R, and finally as the reacted liquid L4 at the outlet port. 11D.

  While the reaction liquid L3 is proceeding with the reaction in the micro flow path R, the ultrasonic vibrator 13 emits ultrasonic vibration. The ultrasonic vibration generated by the ultrasonic vibrator 13 is transmitted to the inner cylinder 1 and then transmitted to the flow path forming body 11 via the thermal refrigerant W1. The ultrasonic vibration transmitted to the flow path forming body 11 is transmitted to the reaction liquid L3 flowing in the micro flow path R. The vibration characteristic of this ultrasonic vibration is set to a value that prevents the molecules of the reaction liquid L3 from generating minute vibrations and preventing the bonds between the molecules. That is, to the reaction liquid L3 in the micro flow path R, each molecule of the reaction liquid L3 generates a minute vibration, and an ultrasonic vibration having a frequency and an amplitude that prevents the binding between the molecules is applied. This avoids accumulation of deposits of highly viscous fluids or granules or crystals that may occur during the course of the reaction, and as a result, blockage of the microchannel R is prevented. Further, even when the reaction liquid L3 is stopped in the microchannel R, the microchannel R is prevented from being blocked for the same reason as above.

  In this embodiment, the ultrasonic transducer 13 imparts ultrasonic vibration to the flow path forming body 11 using the thermal refrigerant W1 as a propagation medium for ultrasonic vibration. As a result, the ultrasonic vibration applied to the flow path forming body 11 is not localized, and is uniform throughout the flow path forming body 11, so that there is no wrinkle over the entire micro flow path R. Prevention can be achieved.

  On the other hand, the thermal refrigerant W1 is circulated at a predetermined flow rate in the thermal refrigerant chamber 12H. The thermal refrigerant W1 is heated by the temperature control unit 55 based on the temperature signal S1 sent from the liquid temperature sensor 14 so that the temperature of the liquid to be reacted L3 flowing through the microchannel R becomes an optimum temperature for the reaction. Cooled and temperature controlled. Thereby, a high-quality reaction with high accuracy can be achieved. As described above, the thermal refrigerant W1 has both the functions of ultrasonic wave propagation and temperature adjustment in the thermal refrigerant chamber 12H which is one sealed space, and the apparatus efficiency is high.

  Further, the cooling gas W2 is circulated at a predetermined flow rate in the cooling gas chamber 12C. As a result, the temperature rise due to the heat generation of the ultrasonic vibrator 13 itself due to the generation of the ultrasonic vibration can be suppressed, and the malfunction of the ultrasonic vibrator 13 due to the temperature rise and the fluctuation of the generated frequency can be eliminated. it can.

  In the above-described embodiment, the flow path forming body 11 may have the following form in addition to the long flexible tube body wound in a coil shape.

  For example, the flow path forming body may be one in which long flexible tube bodies are simply arranged linearly.

  Moreover, it is good also as a form which has a micro flow path as shown in Unexamined-Japanese-Patent No. 2006-305505 (patent document 4) which repeats clockwise rotation and counterclockwise rotation alternately.

Further, for example, as in the flow path forming body 11 ′ shown in FIG. 5, the inlet portion of the micro flow path R ′ is branched in a substantially Y shape, and the first liquid L1 is supplied from _one inlet port 11′I1. Is injected and supplied, and the second liquid L2 is injected and supplied from the other inlet port 11′I ₂ and collides at the branch point R ′ ₀ to cause a reaction. The flow path forming body 11 ′ includes a micro through groove plate 91 and lid plates 92 and 93. The micro through groove plate 91 includes a micro through groove 94 that penetrates in the thickness direction and continues in the surface direction. The plan view of the micro through-groove 94 has a substantially Y shape. With the flat surfaces of the lid plates 92 and 93 facing the micro through-groove plate 91, respectively, both sides in the thickness direction of the micro through-groove plate 91 are clamped by the lid plates 92 and 93 so that the plan view is substantially Y. A micro-channel R ′ having a letter shape is formed. When using this embodiment, the may be directly attached 'ultrasonic transducer 13 to the outer wall portion corresponding to _0' branch point R. A strong ultrasonic vibration is locally applied to the branch point R ′ ₀ to effectively prevent clogging due to accumulation of high-viscosity fluid or precipitation of granules or crystals that may occur at the time of collision between the first liquid L1 and the second liquid L2. Because it can be done.

  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 this 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. That is, the structure, shape, size, material, number, etc. of the whole or a part of the microchannel blockage prevention device 10 can be variously changed in accordance with the spirit of the present invention. The present invention can also be applied to simple mixing without chemical reaction.

BRIEF DESCRIPTION OF THE DRAWINGS It is a structure schematic diagram which shows the microchemical plant provided with the microchannel blockage | blocking prevention apparatus which concerns on this invention. It is a front partial sectional view showing the composition outline of the micro channel blockade prevention device concerning the present invention. It is side surface partial sectional drawing which shows the structure outline | summary of the microchannel obstruction | occlusion prevention apparatus which concerns on this invention. It is front sectional drawing which shows schematic structure of an ultrasonic transducer | vibrator. It is 2 surface partial sectional drawing which shows the flow-path formation body of another form.

Explanation of symbols

10 Micro-channel blockage prevention device (Micro-channel blockage prevention device)
11 Channel formation body 11 'Channel formation body 12H Thermal refrigerant chamber (liquid chamber)
13 Ultrasonic vibrator (Ultrasonic vibration applying means)
55 Temperature controller (liquid temperature control means)
60 Cooling gas circulation part (cooling means)
L3 Reaction liquid (reaction fluid)
R Micro flow path W1 Thermal refrigerant (liquid)

Claims (6)

  A flow path forming body (11) that forms a micro flow path (R) for advancing the reaction of the reaction fluid (L3), and an ultrasonic vibration applying means that applies ultrasonic vibration to the flow path forming body (11). (13) A device for preventing clogging of a micro flow path.   The microchannel blockage prevention device according to claim 1, wherein the ultrasonic vibration applying means (13) applies ultrasonic vibration to the flow path forming body (11) from the outside of the flow path forming body (11).   The microchannel blockage prevention device according to claim 1 or 2, further comprising a cooling means (60) for cooling the ultrasonic vibration applying means (13).   A liquid chamber (12H) for interposing the liquid (W1) is provided between the ultrasonic vibration applying means (13) and the flow path forming body (11), and the ultrasonic vibration applying means (13) The microchannel blockage prevention device according to any one of claims 1 to 3, wherein ultrasonic vibration is applied to the flow path forming body (11) by using ultrasonic vibration as a propagation medium.   The microchannel blockage prevention device according to claim 4, further comprising a liquid temperature adjusting means (55) for adjusting the temperature of the liquid (W1) in the liquid chamber (12H).   By applying ultrasonic vibration to the flow path forming body (11) that forms the micro flow path (R) for advancing the reaction of the reaction fluid (L3) by the ultrasonic vibration applying means (13), A method for preventing clogging of a microchannel, wherein the clogging of the channel (R) is prevented.

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