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WO2013047248A1 - Microréacteur et procédé de fabrication d'un produit de réaction - Google Patents

Microréacteur et procédé de fabrication d'un produit de réaction Download PDF

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Publication number
WO2013047248A1
WO2013047248A1 PCT/JP2012/073698 JP2012073698W WO2013047248A1 WO 2013047248 A1 WO2013047248 A1 WO 2013047248A1 JP 2012073698 W JP2012073698 W JP 2012073698W WO 2013047248 A1 WO2013047248 A1 WO 2013047248A1
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WIPO (PCT)
Prior art keywords
reaction
channel
slag
liquid
gas
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2012/073698
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English (en)
Japanese (ja)
Inventor
重司 榊原
慎太郎 二上
博之 南
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Dexerials Corp
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Dexerials Corp
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Filing date
Publication date
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Publication of WO2013047248A1 publication Critical patent/WO2013047248A1/fr
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Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
    • C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
    • C07C51/255—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting
    • C07C51/265—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting having alkyl side chains which are oxidised to carboxyl groups
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40—Static mixers
    • B01F25/42—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/433—Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
    • B01F25/4331—Mixers with bended, curved, coiled, wounded mixing tubes or comprising elements for bending the flow
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/30—Micromixers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00788—Three-dimensional assemblies, i.e. the reactor comprising a form other than a stack of plates
    • B01J2219/00792—One or more tube-shaped elements
    • B01J2219/00795—Spiral-shaped
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00831—Glass
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00851—Additional features
    • B01J2219/00858—Aspects relating to the size of the reactor
    • B01J2219/0086—Dimensions of the flow channels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00851—Additional features
    • B01J2219/00867—Microreactors placed in series, on the same or on different supports
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00891—Feeding or evacuation
    • B01J2219/00894—More than two inlets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00891—Feeding or evacuation
    • B01J2219/00903—Segmented flow
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00925—Irradiation
    • B01J2219/00934—Electromagnetic waves
    • B01J2219/00936—UV-radiations

Definitions

  • the present invention relates to a microreactor for producing a reaction product at a gas-liquid interface or a liquid-liquid interface and a method for producing a reaction product using the microreactor.
  • an apparatus for causing a chemical reaction at an interface between a gas phase and a liquid phase and between a liquid phase and a liquid phase to obtain a reaction product has been used.
  • a liquid sample 100 is supplied by a pump 101 and a reaction gas 102 is supplied.
  • a slag is formed in which a liquid sample and a reaction gas are alternately and continuously formed, a chemical reaction proceeds at a gas-liquid interface between the liquid sample and the reaction gas, and ultraviolet rays are applied to the slag flowing through the reaction tube 104.
  • Irradiating means such as a high pressure mercury lamp 105 for irradiating.
  • the supply unit 103 controls the pump 101 and the valve 106 so that the liquid sample and the reaction gas are alternately supplied to form a slag.
  • the reaction tube 104 is formed using a glass tube or the like, and is disposed so as to wrap around the outer periphery of the lamp, so that the slag flowing in the tube is irradiated with ultraviolet rays, and the chemical reaction caused thereby proceeds. Configure the road.
  • a flow path for performing a chemical reaction at the gas-liquid interface or the liquid-liquid interface is formed on one chip by using an ultrafine processing technique.
  • Microreactors have been developed.
  • a microreactor 109 shown in FIG. 7 is connected to, for example, a syringe 110 and supplied with a liquid sample, a gas channel 113 connected to a syringe 112 and supplied with a reaction gas, and these liquid channels.
  • the supply flow path 114 in which the liquid sample and the reaction gas are alternately supplied the supply flow path 114 is continuous, and the slag in which the liquid sample and the reaction gas are alternately continuous
  • the reaction channel 115 in which the chemical reaction proceeds at the gas-liquid interface between the liquid sample and the reaction gas is formed on the substrate.
  • a microreactor is required to stably transport slag in a reaction channel that is secured for a long time because a chemical reaction proceeds at a gas-liquid interface between a liquid sample and a reaction gas. That is, as shown in FIG. 9, when the slag is disturbed in the reaction channel and the liquid sample is integrated with the preceding and following liquid samples, the area of the gas-liquid interface is reduced and the reaction is not promoted. For this reason, the microreactor is required to have a long reaction channel and to flow stably without disturbing the slag.
  • the pressure variation in the reaction channel is eliminated as much as possible, and the resistance against the pressure variation is increased even when the pressure variation in the supply channel propagates to the reaction channel.
  • the reaction channel is formed as thin as possible.
  • slugs are formed to be elongated, so that even when pressure fluctuations occur, the pressure can be absorbed by expanding and contracting in the longitudinal direction, and there is no disturbance in the width direction. In other words, the liquid samples moving back and forth are not integrated.
  • reaction flow path is narrowed, the area of the gas-liquid interface between the liquid sample and the reaction gas decreases, and the reaction cannot be promoted efficiently. Moreover, since the flow rate is fast in a narrow flow path, there is a risk of being discharged without sufficient reaction. Furthermore, when two microreactors are connected via the connecting pipe 119, the reaction path is divided and the slag becomes unstable. Therefore, it is necessary to configure a reaction channel in one substrate, but the limited substrate area There was a limit to the length of the reaction channel in the interior.
  • the present invention uses a microreactor capable of efficiently performing a chemical reaction at a gas-liquid interface or a liquid-liquid interface and allowing a slag to flow stably within a limited substrate area, and this microreactor. It aims at providing the manufacturing method of a reaction product.
  • a microreactor according to the present invention is supplied via a supply channel in which fluid samples forming a gas-liquid interface or a liquid-liquid interface are alternately supplied, and the supply channel.
  • a slag forming channel that forms a slag in which the sample is alternately continuous;
  • a reaction channel that is formed wider than the slag forming channel and that irradiates light to advance a chemical reaction at the interface of the sample;
  • a widened portion that is interposed between the slag forming flow channel and the reaction flow channel, one end is continuous with the slag forming flow channel, the other end is continuous with the reaction flow channel, and is gradually widened, and the reaction
  • a discharge channel that discharges the reacted sample continuously from the channel.
  • the reaction product manufacturing method forms a supply step in which fluid samples forming a gas-liquid interface or a liquid-liquid interface are alternately supplied, and a slag in which the supplied samples are alternately continuous.
  • a slag forming step, a reaction step of causing a reaction to proceed at the interface of the sample by irradiating light, and a discharge step of discharging the reacted sample, the slag comprising the slag forming step and the above By flowing through the widened portion where the flow path is gradually widened between the reaction step and the reaction step, the interface of the fluid sample is enlarged in the reaction step as compared with the slag formation step.
  • the widened portion 20 interposed between the reaction channel and the slag forming channel gradually increases the channel width from the slag forming channel to the reaction channel. Therefore, according to the present invention, it is possible to prevent a rapid change in pressure from the slag formation channel to the reaction channel, and to deform the slug shape of a thin and long fluid sample into a thick and short shape without breaking the slag. Thereby, according to this invention, reaction efficiency and a yield can be improved by expanding the cross-sectional area of the interface of a fluid sample in the state where the slag was stabilized, and slowing down the flow velocity of slag.
  • FIG. 1 is a perspective view showing a microreactor according to the present invention.
  • FIG. 2 is a plan view showing a slag forming flow channel and a reaction flow channel that are continuous via the widened portion.
  • FIG. 3 is a plan view showing a reaction channel and a discharge channel.
  • FIG. 4 is a perspective view showing a microreactor having a two-layer structure.
  • FIG. 5 is a plan view showing a configuration in which the rectilinear portion of the reaction channel is continued by the widened portion.
  • FIG. 6 is a diagram showing a configuration of a conventional apparatus for performing a gas-liquid reaction or a liquid-liquid reaction.
  • FIG. 7 is a diagram showing a configuration of a conventional microreactor.
  • FIG. 8 is a diagram showing the configuration of another conventional microreactor.
  • FIG. 9 is a plan view showing a state in which slag is disturbed in a conventional microreactor.
  • a microreactor 1 to which the present invention is applied has a slag formed between a liquid sample 3 and a reaction gas 4 or a slag formed between liquid samples 3 having different properties inside a rectangular substrate 2.
  • a small-diameter flow path is provided, and a chemical reaction proceeds at the gas-liquid interface or liquid-liquid interface of the slag by being irradiated with light rays such as ultraviolet rays from one side.
  • light rays such as ultraviolet rays from one side.
  • the microreactor 1 has different properties and forms slag without mixing. It can also be used when reacting liquid samples 3 to be reacted.
  • the substrate 2 is formed, for example, by bonding two pieces of glass on which each flow path described later is formed. Or the board
  • substrate 2 is formed by bonding the glass by which each flow path was formed on the surface, and the glass used as a top plate.
  • the flow path is formed using a fine processing technique such as etching or grinding.
  • a supply channel 10 that alternately supplies a liquid sample 3 and a reaction gas 4 that form a gas-liquid interface with each other, and a liquid sample 3 and a reaction gas 4 that are supplied via the supply channel 10 alternately.
  • a slag forming channel 11 that forms a continuous slag
  • a reaction channel 12 that is continuous with the slag forming channel 11 and that is irradiated with light, thereby allowing the reaction to proceed at the gas-liquid interface
  • a discharge channel 13 for discharging the reaction product.
  • the supply channel 10 includes a first supply channel 10a to which the liquid sample 3 is supplied, a second supply channel 10b to which the reaction gas 4 is supplied, and the first and second supply channels 10a and 10b merge. And is formed in a substantially Y shape.
  • the first and second supply paths 10a and 10b face outward through openings 15 and 16 formed on the upper surface of the substrate 2, respectively. Further, the combined channel 10 c is continuous with the slag forming channel 11.
  • the first supply channel 10 a is connected to a syringe 17 for injecting the reaction gas 4 through the opening 15, and the reaction gas 4 is injected into the combined channel 10 c at a predetermined pressure according to the operation of the syringe 17.
  • the second supply channel 10b is connected to a syringe 18 for injecting the liquid sample 3 through the opening 16, and the liquid sample 3 is intermittently injected into the combined channel 10c at a predetermined pressure according to the operation of the syringe 18. .
  • the liquid sample 3 and the reaction gas 4 are alternately and continuously supplied by intermittently injecting the liquid sample 3 into the reaction gas 4 flowing in the combined flow path 10 c.
  • the first supply path 10a, the second supply path 10b, and the combined flow path 10c are all formed with the same depth and the same width, for example, with a depth of 0.3 mm and a width of 0.3 mm. .
  • the supply channel 10 is configured so that the pressure received by the reaction gas 4 in the first supply channel 10a and the pressure received by the liquid sample 3 in the second supply channel 10b, and the liquid sample 3 and the reaction gas 4 in the combined channel 10c. The difference from the pressure received is reduced, and the liquid sample 3 and the reaction gas 4 are continuously supplied alternately and stably.
  • the slag forming flow path 11 is formed from the combined flow path 10c toward one side edge in the width direction of the substrate 2, and further, the one side edge is formed in the longitudinal direction.
  • the slag forming channel 11 stably forms and conveys a slag in which the liquid sample 3 and the reaction gas 4 are alternately continued, and is formed narrower than a reaction channel 12 described later.
  • the slag forming flow path 11 is formed with a narrow width, so that the slag is formed long and narrow. Therefore, the slag forming channel 11 can absorb the pressure variation by the expansion and contraction of the slag in the longitudinal direction even when the pressure fluctuation occurs in the supply channel 10, and there is no disturbance in the width direction.
  • the liquid samples 3 moving back and forth via 4 are not integrated.
  • the microreactor 1 sends a long and stable slag to the reaction channel 12 by providing a narrow and long slag forming channel 11 between the supply channel 10 and the reaction channel 12. be able to.
  • the slag formation flow path 11 has the same depth and the same width as the supply flow path 10, for example, is formed in depth 0.3mm and width 0.3mm.
  • the reaction channel 12 is a channel that causes a chemical reaction to proceed at the interface by irradiating the gas-liquid interface of the slag with light such as ultraviolet rays.
  • a plurality of rectilinear portions 12a that advance straight in the longitudinal direction of the substrate 2 are formed in parallel in the width direction, The end portions are continuous by the curved portion 12b, and thereby, the end portions are formed to meander over the entire surface of the substrate 2.
  • both the rectilinear portion 12a and the curved portion 12b are formed with the same depth and the same width, thereby suppressing fluctuations in pressure and enabling stable conveyance without disturbing the slag. That is, the reaction channel 12 can be provided with a rectilinear portion where the pressure fluctuation does not occur by providing the rectilinear portion 12a along the longitudinal direction of the substrate 2, and the curved portion 12b has the same width as the rectilinear portion 12a.
  • the slag can be curved and the direction can be changed while suppressing fluctuations in pressure.
  • the reaction channel 12 is formed wider than the slag forming channel 11.
  • the microreactor 1 increases the gas-liquid contact time and the ultraviolet irradiation time by widening the cross-sectional area of the gas-liquid interface of the slag and slowing the flow rate of the slag, thereby efficiently promoting the gas-liquid reaction. Can do. Therefore, the microreactor 1 can obtain a gas-liquid reaction product with a high yield.
  • the reaction channel 12 and the slag forming channel 11 are connected via the widened portion 20.
  • the widening section 20 is a flow path that gradually widens the width of the flow path from the slag forming flow path 11 to the reaction flow path 12, thereby deforming the liquid sample 3 and the reaction gas 4 thickly and shortly without breaking the slag. is there.
  • the widened portion 20 is formed to have the same width as that of the slag forming channel 11 on one end side and the same width as that of the reaction channel 12 on the other end side, and gradually widens.
  • the widening portion 20 prevents a sudden change in pressure from the slag forming channel 11 to the reaction channel 12, widens the cross-sectional area of the gas-liquid interface while stabilizing the slag, and slows the flow rate of the slag. can do.
  • the widened portion 20 is formed such that one end side has the same depth of 0.3 mm and width 0.3 mm as the slag forming channel 11, and the other end side has the same depth 0.3 mm and width 0 as the reaction channel 12. .5mm.
  • the microreactor 1 has the same depth (0.3 mm) over the supply flow path 10, the slag formation flow path 11, the widened portion 20, and the reaction flow path 12, so that each flow path is controlled only by width control. Can be more easily formed by etching or the like.
  • the widened portion 20 is formed in a curved shape in which the end portions of the slag forming flow channel 11 and the reaction flow channel 12 formed adjacent to each other in parallel in the width direction of the substrate 20 are continuous. That is, the liquid sample 3 and the reaction gas 4 constituting the slag are gradually deformed thicker and shorter while the widened portion 20 is curved.
  • the widened portion 20 is curved from the slag forming channel 11 to the reaction channel 12 to reduce the flow rate of the slag.
  • the widening section 20 gradually widens the slag in a decelerated state, so that the slag is prevented from being disturbed due to pressure fluctuations, the cross-sectional area of the gas-liquid interface is widened in a stable slag, and the slag The flow rate can be reduced.
  • the widened portion 20 is bent at 180 ° in order to make the end portions of the slag forming flow channel 11 and the reaction flow channel 12 formed in parallel to each other continue.
  • slag can be decelerated to the maximum.
  • the slag is depressurized by passing through the widened portion 20 that gradually widens, but at that time, since it is decelerated by the curved shape, rapid fluctuations in pressure are prevented and the front and rear liquid samples 3 are connected to each other. However, it is stably deformed from a thin and long shape to a thick and short shape.
  • the discharge flow path 13 that is continuous with the reaction flow path 12 and discharges the reaction product is approximately 90 ° from the front end of the reaction flow path 12 provided on the other end side in the width direction of the substrate 2. It is formed toward the one end side in the width direction of the substrate 2 through a bent portion 24 that bends to the side. Further, the discharge channel 13 has the other end opposite to the one end continuous with the reaction channel 12 facing outward from the opening 25 formed in the lower surface of the substrate 2. Further, the discharge channel 13 is formed to have the same depth as the reaction channel 12 and narrower than the reaction channel 12, for example, the reaction channel 12 has a depth of 0.3 mm and a width of 0.5 mm. On the other hand, the discharge channel 13 is formed with a depth of 0.3 mm and a width of 0.3 mm.
  • the discharge channel 13 is formed to be narrower than the reaction channel 12, thereby transporting the slag in a stable state and discharging the gas-liquid reaction product from the opening 25. That is, since the discharge flow channel 13 faces outward from the opening 25, the internal pressure is released from the opening 25, so that pressure fluctuation is likely to occur and the slag becomes unstable. When the pressure fluctuation in the discharge channel 13 propagates to the reaction channel 12, the pressure balance in the reaction channel 12 is lost and the liquid samples 3 may be integrated.
  • the microreactor 1 can stably transport slag having a large cross-sectional area at the gas-liquid interface to the end of the reaction channel 12, and the gas-liquid contact time and The irradiation time of ultraviolet rays can be increased.
  • the discharge channel 13 is continuous with the reaction channel 12 via the bent portion 24, the deformation of the slag due to the pressure balance variation from the opening 25 is further prevented from propagating to the reaction channel 12. can do.
  • One end of the bent portion 24 is continuous with the reaction flow path, the other end is continuous with the discharge flow path 13, and is bent so as to gradually become narrower. Therefore, the slag flowing from the reaction flow path 12 to the bent portion 24 flows out to the discharge flow path 13 in a stable state without sudden pressure fluctuation.
  • the microreactor 1 is provided with the discharge flow path 13 narrower than the reaction flow path 12 via the bent portion 24, thereby stabilizing the slag flow in the reaction flow path 12 and improving the efficiency of the gas-liquid reaction, High yields can be achieved.
  • the syringe 17 containing the reaction gas 4 is connected to the first supply path 10a via the opening 15 of the substrate 2, and the syringe 18 containing the liquid sample 3 is supplied to the second supply via the opening 16. Connect to path 10b. Then, by operating the syringe 17, the reaction gas 4 is injected from the first supply path 10 a into the combined flow path 10 c, and by operating the syringe 18, intermittently from the second supply path 10 b to the combined flow path 10 c. The liquid sample 3 is injected into.
  • the supply channel 10 is supplied with the liquid sample 3 and the reaction gas 4 alternately and continuously by intermittently injecting the liquid sample 3 into the reaction gas 4 flowing in the combined channel 10c.
  • a slag flow in which the liquid sample 3 and the reaction gas 4 are alternately continued is formed in the slag formation flow channel 11 continuous with the combined flow channel 10c.
  • the first and second supply channels 10a and 10b, the combined channel 10c, and the slag forming channel 11 of the supply channel 10 all have the same depth (for example, 0.3 mm) and the same width (for example, 0.2 mm). 3 mm), the pressure fluctuation in the flow path is suppressed, and the slag can be stably formed and transported.
  • the channel can be formed only by controlling the width when the channel is formed by etching the substrate 2 or the like.
  • the slag flow that flows through the slag forming channel 11 flows into the reaction channel 12 that is wider than the slag forming channel 11 through the widened portion 20, whereby the shapes of the liquid sample 3 and the reaction gas 4 constituting the slag are changed. It is deformed thick and short. Further, the reaction flow path 12 is irradiated with light rays such as ultraviolet rays from the upper surface side of the substrate 2, and a chemical reaction proceeds at the gas-liquid interface.
  • the liquid sample 3 and the reaction gas 4 in the reaction channel 12 are prevented in a state in which a rapid change in pressure is prevented and the slag flow is stabilized by passing through the widened portion 20 where the channel width gradually increases.
  • the area of the gas-liquid interface can be enlarged.
  • the widened portion 20 is formed in a curved shape, so that the flow path width is gradually widened while the flow rate of the slag is reduced. Accordingly, it is possible to suppress the slag disturbance due to a rapid change in pressure, to expand the cross-sectional area of the gas-liquid interface in a stable state of the slag, and to reduce the flow rate of the slag.
  • the reaction flow path 12 increases the contact area at the gas-liquid interface and the irradiation time of the ultraviolet rays by expanding the contact area at the gas-liquid interface without reducing the slag and reducing the flow rate of the slag, A gas-liquid reaction can be advanced efficiently. Therefore, the microreactor 1 can obtain a gas-liquid reaction product with a high yield.
  • the reaction product generated in the reaction channel 12 flows into the discharge channel 13 and is discharged from the opening 25.
  • the pressure of the discharge channel 13 becomes zero when the opening 25 is opened.
  • the discharge channel 13 is formed to be narrower than the reaction channel 12, the disturbance of the slag due to the pressure variation is suppressed, and the pressure variation is applied to the reaction channel 12. Can be prevented from propagating.
  • the discharge channel 13 is continuous with the reaction channel 12 via the bent portion 24, the propagation of the pressure fluctuation can also be prevented by this.
  • Examples of the gas-liquid reaction using the microreactor 1 include a photo-oxidation reaction of a methyl group on an aromatic ring.
  • this photo-oxidation reaction 4-tert-butyltoluene and oxygen are reacted by irradiating with ultraviolet rays in the presence of a catalytic amount of LiBr to produce 4-tert-butylbenzoic acid in which methyl groups on the aromatic ring are oxidized. It is a gas-liquid reaction.
  • the slag flow composed of 4-tert-butyltoluene and oxygen flows into the reaction channel 12 through the widened portion 20 and is stably deformed from a thin and long shape to a thick and short shape.
  • the slag flow composed of 4-tert-butyltoluene and oxygen has a wide cross-sectional area at the gas-liquid interface, and the flow rate is slowed down, so that the contact time between 4-tert-butyltoluene and oxygen and the ultraviolet rays are reduced.
  • the irradiation time can be increased and the reaction can proceed efficiently. Therefore, the microreactor 1 can obtain 4-tert-butylbenzoic acid in which the methyl group on the aromatic ring is oxidized with a high yield.
  • the maricro reactor 1 can be used for a liquid-liquid reaction between liquid samples that form a slag flow without being mixed with each other because of different properties such as an aqueous system and an oil system.
  • Examples of the liquid-liquid reaction using the microreactor 1 include a photo-oxidation reaction between oxygen water and a liquid sample such as organic esters. Specifically, oxygen water and a liquid sample such as organic esters are respectively supplied from the first and second supply passages 10a and 10b at a predetermined pressure, and the oxygen water and the liquid sample are supplied through the slag formation passage 11. And slag is formed and conveyed alternately.
  • the slag flow comprising oxygen water and a liquid sample is stably deformed from a thin and long shape to a thick and short shape by flowing into the reaction channel 12 via the widened portion 20.
  • the slag flow composed of oxygen water and the liquid sample is irradiated with light in the reaction channel 12 because the cross-sectional area of the liquid-liquid interface is widened and the flow velocity is slow, so that the liquid slag liquid
  • the oxidation reaction proceeds at the interface.
  • liquid-liquid reaction is a photopolymerization reaction using various acrylic monomers and a photopolymerization initiator contained in an aqueous liquid sample.
  • an acrylic monomer such as an acrylate ester and a photopolymerization agent contained in an aqueous liquid sample are supplied from the first and second supply paths 10a and 10b, respectively, at a predetermined pressure to form slag.
  • slag in which acrylic monomers and photopolymerization initiators are alternately continued is formed and conveyed.
  • the slag flow composed of the acrylic monomer and the photopolymerization initiator flows to the reaction flow path 12 through the widened portion 20, so that the cross-sectional area of the liquid-liquid interface similarly increases, and the flow rate becomes slow.
  • light such as ultraviolet rays
  • radicals by the photopolymerization initiator are generated at the liquid-liquid interface of the slag, and the radical polymerization reaction of the acrylic monomer proceeds.
  • the reaction to proceed at the liquid-liquid interface of the slag and polymerizing the surface of the acrylic monomer, it is possible to suppress agglomeration of the separated particles, and then perform the main polymerization. Can do.
  • reaction gas 4 decreases as the reaction proceeds. Therefore, in the slag flow consisting of the reaction product solution and a small amount of the reaction gas 4 downstream of the reaction channel 12, the reaction product solution is reduced. There is a risk of instability, such as linking with the solution before and after.
  • the microreactor 1 may supply an inert gas that does not react with the liquid sample 3, the reaction gas 4, and the reaction product together with the reaction gas 4.
  • an inert gas that does not react with the liquid sample 3, the reaction gas 4, and the reaction product together with the reaction gas 4.
  • the microreactor to which the present invention is applied is not limited to the above-described configuration.
  • the reaction channel 12 may be multilayered in the thickness direction of the substrate 2.
  • the substrate 2 is formed with an upper reaction channel 30, a lower reaction channel 31, and a connection channel 32 that connects the upper and lower reaction channels 30, 31.
  • the upper and lower reaction channels 30, 31 Similar to the reaction channel 12, the upper and lower reaction channels 30, 31 have a plurality of rectilinear portions 30a, 31a that go straight in the longitudinal direction of the substrate 2 in parallel in the width direction and are adjacent to each other. The ends of the rectilinear portions 30 a and 31 a are continuous with each other by the curved portions 30 b and 31 b, thereby forming a meandering over the entire surface of the substrate 2.
  • the upper layer reaction channel 12 is connected to the widened portion 20 at one end, meanders in the upper layer surface of the substrate 2, and is connected at the end on the other end side in the width direction of the substrate 2.
  • the lower reaction channel 31 is continued through the channel 32.
  • One end of the lower reaction channel 31 is continuous with the connection channel, meanders in the lower surface of the substrate 2, and is continued with the discharge channel 13 at the end of one end in the width direction of the substrate 2.
  • the upper and lower reaction channels 30 and 31 are formed so that the rectilinear portions 30a and 31a do not overlap each other, and the upper reaction channel 30 does not block light such as ultraviolet rays irradiated from the upper surface side of the substrate 2.
  • the lower reaction channel 31 can also be irradiated.
  • the channel through which gas-liquid reaction or liquid-liquid reaction proceeds can be lengthened, and the reaction efficiency and yield can be improved in a limited substrate space. Can do.
  • the microreactor to which the present invention is applied is not only between the slag forming channel 11 and the reaction channel 12, but also between the rectilinear portions 12a of the reaction channel 12 via the widened portion 20. May be gradually widened. That is, in the microreactor 1, the channel width is widened through the widened portion 20 from the slag forming flow channel 11 to the reaction flow channel 12, and the widened portion 20 is provided between the plurality of rectilinear portions 12a of the reaction flow channel 12.
  • the reaction channel 12 may be gradually widened by being continued through.
  • the widened portion 20 that connects the plurality of rectilinear portions 12a of the reaction flow path 12 is also curved so that the slag is gradually widened in a decelerated state, so that slag disturbance due to pressure fluctuations is suppressed.
  • the cross-sectional area of the gas-liquid interface can be expanded while the slag is stable, and the flow rate of the slag can be reduced.
  • the microreactor 1 irradiates light such as ultraviolet rays in the reaction channel to advance the gas-liquid reaction or liquid-liquid reaction, but also irradiates the slag forming channel 11, the widened portion 20, or the discharge channel 13.
  • the reaction may be promoted.
  • reaction flow path 1 microreactor, 2 substrate, 3 liquid sample, 4 reaction gas, 10 supply channel, 10a first supply channel, 10b second supply channel, 10c combined channel, 11 slag formation channel, 12 reaction channel, 12a straight line Part, 12b curved part, 13 discharge flow path, 15, 16 opening, 17, 18 syringe, 20 widening part, 24 bending part, 25 opening, 30, 31 reaction flow path

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Micromachines (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)

Abstract

L'invention concerne un microréacteur dans lequel la surface de l'interface gaz-liquide est agrandie sans que le laitier ne soit perturbé. Cette invention a : un canal d'alimentation (10) à travers lequel des échantillons fluides (3, 4), qui forment une interface gaz-liquide ou une interface liquide-liquide l'une avec l'autre, sont fournis de façon alternée; un canal de formation de laitier (11) pour former un laitier dans lequel les échantillons (3, 4) adressés à travers le canal d'alimentation (10) sont continus de façon alternée; un canal de réaction (12) formé de façon à être plus large que le canal de formation de laitier (11), le canal de réaction étant irradié par de la lumière, ce par quoi une réaction chimique est provoquée sur l'interface entre les échantillons; une section de largeur agrandie (20) interposée entre le canal de formation de laitier (11) et le canal de réaction (12), une extrémité de la section de largeur agrandie étant continue avec le canal de formation de laitier (11), l'autre extrémité de la section de largeur agrandie étant continue avec le canal de réaction (12), la section de largeur agrandie (20) ayant une largeur qui s'agrandit progressivement; et un canal de décharge (13) pour décharger les échantillons ayant réagi, le canal de décharge étant continu à partir du canal de réaction (12).
PCT/JP2012/073698 2011-09-29 2012-09-14 Microréacteur et procédé de fabrication d'un produit de réaction Ceased WO2013047248A1 (fr)

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JP2011215092A JP5908244B2 (ja) 2011-09-29 2011-09-29 マイクロリアクタ及び反応生成物の製造方法

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TWI701075B (zh) * 2015-05-29 2020-08-11 日商昭榮化學工業股份有限公司 奈米粒子的製造方法
CN112206727A (zh) * 2019-07-10 2021-01-12 中国石油化工股份有限公司 一种微通道气液反应装置和强化气液反应的方法及制备己二酸的方法
WO2021189639A1 (fr) * 2020-03-25 2021-09-30 南京延长反应技术研究院有限公司 Système de réaction amélioré et procédé d'hydratation du propylène catalysé par un liquide ionique

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JP6086250B2 (ja) * 2014-04-25 2017-03-01 大陽日酸株式会社 気液反応方法及びアミノシランの製造方法
JP6406959B2 (ja) * 2014-09-30 2018-10-17 デクセリアルズ株式会社 小型反応器、及び反応装置
CN107413405A (zh) * 2017-06-09 2017-12-01 吴振嘉 防止流体逆流的微流体反应器

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TWI701075B (zh) * 2015-05-29 2020-08-11 日商昭榮化學工業股份有限公司 奈米粒子的製造方法
CN109647303A (zh) * 2018-12-11 2019-04-19 浙江工业大学 全氟磺酸树脂/铜锰复合物微纤化微通道反应器的制备方法和应用
CN112206727A (zh) * 2019-07-10 2021-01-12 中国石油化工股份有限公司 一种微通道气液反应装置和强化气液反应的方法及制备己二酸的方法
CN112206727B (zh) * 2019-07-10 2024-01-05 中国石油化工股份有限公司 一种微通道气液反应装置和强化气液反应的方法及制备己二酸的方法
WO2021189639A1 (fr) * 2020-03-25 2021-09-30 南京延长反应技术研究院有限公司 Système de réaction amélioré et procédé d'hydratation du propylène catalysé par un liquide ionique

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