JP2002292271A - Flow type fine reaction passage, reaction apparatus and reaction method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To improve the productivity of a desired material by efficiently mixing reaction fluids and securing the reaction time in a confluent part while suppressing the increase of pressure loss in a flow type fine reaction passage, a reaction apparatus and a reaction method. SOLUTION: In the fine flow type reaction passage 3 provided with a plurality of introducing flow passages 10A and 10B each having a fine cross-sectional surface area and a confluent passage 20 formed by joining the introducing flow passages 10A and 10B in the confluent part 15 and for joining and reacting the reaction fluids FA and FB flowing through each introducing flow passage 10A and 10b with each other in the confluent passage 20, the confluent passage 20 is structured to be provided with a throttle part 21 having a smaller cross-sectional surface area than the sum total of that of each introducing flow passages 10A and 10B formed in the confluent part 15 and an expanded part 22 provided in the downstream side of the throttle part 21 and having a larger cross-sectional surface area than that of the throttle part 21.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a flow-type micro reaction channel, a reaction apparatus, and a reaction method for causing a chemical reaction while flowing a reaction fluid in a micro flow channel.

[0002]

2. Description of the Related Art In recent years, since a chemical reaction can be efficiently performed, a flow-type microreaction in which a plurality of reactants are caused to flow through a reaction path having a small flow path cross-sectional area (1 cm ² or less) to cause a chemical reaction. Roads (hereinafter, also simply referred to as reaction paths) are attracting attention. This is because the specific surface area (surface area per unit volume) of the reactants in the reaction path can be increased by making the flow path cross-sectional area of the reaction path minute, so that high heat removal efficiency can be obtained and the temperature control of the reaction system can be performed. For this reason, application to production of a reaction product (target substance) accompanied by a particularly large exothermic reaction has been considered.

[0003] Figure 10 is a diagram showing an example of such a conventional flow type micro-channel configuration. The reaction channel 100
Are the introduction paths 101A, 101B and 101A, 1
01B are configured to include a reaction channel 102 formed by the confluence, the introduction path 101A, the reaction fluid F _A introduced respectively 101B, the F _B so as to merge react in the reaction channel 102. ing.

The cross-sectional area of the reaction path 102 is
It is substantially equal to the sum of the cross-sectional area of the flow path of 1A and the cross-sectional area of the flow path of the introduction path 101B, and is constant from the inlet (upstream end) 102a to the outlet (downstream end) 102b. Further, although not shown, the reaction path is placed in a thermostat, and the ambient temperature thereof is controlled to a temperature optimum for the reaction.

[0005]

However, in the flow-through micro-reaction path as described above, the throughput of the reaction fluid (predetermined time) is required in order to secure the residence time of the reaction fluid in the reactor, that is, the reaction time over a predetermined time. When the amount of the reaction fluid passing through the reactor per hour) is set to a small amount, the reaction flow path 1
Productivity of the target substance per reaction path for the cross-sectional area is minute 02 becomes low. Therefore, in order to secure such a residence time for a predetermined time or longer and to improve production efficiency, it is conceivable to increase both the throughput of the reaction fluid and the reaction path length, but the pressure loss of the reaction fluid is greatly increased. It is not realistic because it will be.

Further, when the throughput of the reaction fluid to the reaction channel 102 is small, because the flow of the reaction fluid in the reaction channel 102 of the laminar flow, the mixing of the reactant fluid F _A and reactant fluid F _B, the interface This is performed only by molecular diffusion through the substrate. Thus, the reaction fluid F _A, in order to carry out the mixing and hence chemical reaction of F _B efficiently, by reducing the cross-sectional area of the reaction channel 102, to be increased ratio of interfacial area (contact area) on throughput No.

However, in order to make such an effect remarkable, it is necessary to reduce the diameter of the reaction channel 102 to about 10 μm. In this case, too, the pressure loss of the reaction fluid in the reaction channel 102 is large. turn into. The present invention has been made in view of such a problem, and suppresses an increase in pressure loss, effectively mixes a reaction fluid and secures a reaction time at a junction, thereby increasing productivity of a target substance. It is an object of the present invention to provide a flow-type micro reaction channel, a reaction apparatus, and a reaction method that can be improved.

[0008]

According to the present invention, there is provided a flow-type minute reaction channel according to the present invention, wherein a plurality of introduction channels each having a minute cross-sectional area are provided, and the introduction channel is formed at a junction. A reaction channel flowing through each of the introduction channels, and reacting by combining the reaction fluids through the respective junction channels. In the microflow-type reaction channel, the junction is formed at the junction. A throttle section having a cross-sectional area smaller than the sum of the cross-sectional areas of the introduction flow paths, and an enlarged section provided downstream of the throttle section and having a cross-sectional area larger than the cross-sectional area of the throttle section. It is characterized by being constituted.

According to a second aspect of the present invention, there is provided the flow-type micro reaction channel according to the first aspect, wherein the flow channel has a cross-sectional area of 1 cm ² or less at the junction of the introduction flow channel. It is characterized by having. According to a third aspect of the present invention, there is provided the flow-type micro reaction channel according to the first or second aspect, wherein the equivalent diameter of the cross section of the combined flow channel is 1c.
m or less.

The equivalent diameter ds is defined by the flow path cross-sectional area As and the flow path cross-sectional circumferential length Ls according to the following equation (1). become. ds = 4 × As / Ls (1) The flow-type micro reaction channel according to the present invention according to claim 4 is the flow-type micro reaction channel according to any one of claims 1 to 3, wherein The cross-sectional area of the portion is set in a range of 0.01 times to 0.8 times the total of the cross-sectional areas of the introduction flow path.

According to a fifth aspect of the present invention, there is provided a flow-type minute reaction channel according to any one of the first to fourth aspects, wherein the cross-sectional area of the enlarged portion is smaller than that of the throttle. It is characterized in that it is set in the range of 30 times to 3000 times the sectional area of the part. The flow-type microreaction channel according to the present invention according to claim 6 is the flow-type microreaction channel according to any one of claims 1 to 5, wherein the enlarged portion is formed substantially in the width direction. It is characterized in that one or more rectifying plates for uniformly dividing are provided.

According to a seventh aspect of the present invention, there is provided the reaction apparatus according to any one of the first to sixth aspects, wherein the flow-type minute reaction channel according to any one of the first to sixth aspects is provided with one flow path.
With equipped above, it is characterized in that it is configured to include a reaction fluid drive for the reaction fluid is circulated to each of the inlet flow path of the flow through type fine reaction flow channel. The reaction method of the present invention according to claim 8 is a reaction method in which a plurality of reaction fluids flowing through a minute introduction flow path are combined / reacted, wherein the plurality of reaction fluids are joined at a junction of the introduction flow paths. Step 1, a second step of narrowing the mixed reaction fluid with a throttle having a cross-sectional area smaller than the total cross-sectional area of the introduction flow path, and a step of narrowing the mixed reaction fluid by the throttle And a third step of causing a reaction in an enlarged portion having a larger cross-sectional area.

According to a ninth aspect of the present invention, there is provided the reaction method of the eighth aspect, wherein a cross-sectional area of the flow passage at the junction of the introduction flow passage is 1 cm ² or less. I have. The reaction method of the present invention described in claim 10 is the reaction method of the present invention described in claim 8 or 9,
It is characterized in that the equivalent diameter of each cross section of the narrowed portion and the enlarged portion is 1 cm or less.

[0014]

Embodiments of the present invention will be described below with reference to the drawings. 1 to 7 are diagrams showing a flow-type micro reaction channel, a reaction apparatus, and a reaction method according to an embodiment of the present invention. The reaction apparatus as an embodiment of the present invention, as shown in FIG. 1, a tank 1A for accommodating a predetermined raw material (reactant fluid) F _A, a tank 1B for housing a predetermined material (reaction fluid) F _B , raw F _a, is reacted with a F _B given substance (product, the desired product) and the reactor (flow type micro-channel) 3 for generating a raw material F _a from the tank 1A, the pipe P a pump (reaction fluid circulating device) 2A for feeding to the reactor 3 through the _a, the raw material F _B from the tank 1B, a pump for delivering the reactor 3 via a pipe P _B (reaction fluid (Drive device) 2B.

[0015] The starting F _A, in the case of a F _B is unlikely to flow causes the previously dissolved in solvent tank 1A, may be supplied to the 1B. Further, etc. using pre filter to prevent the reactor 3 is closed, the raw material F _A, may be previously remove fine dust from F _B. In particular,
For example material F _A, tank F _B through the filter 1A, 1
B or a filter may be interposed in the pipes P _A and P _B.

[0016] Now, plate-shaped heater as a temperature adjustment means and below the reactor 3 (e.g. electric heating plate) 4 are arranged, a raw material F _A, F _B is these heaters 4 which flows through the reactor 3 To adjust the temperature to an optimum temperature for the reaction. In addition, such a temperature adjusting unit is not limited to the electric heating plate, and may be, for example, a constant temperature water tank. Further, the temperature adjustment is not limited to heating, and is appropriately set according to the type of reaction.
_A, sometimes to cool the F _B.

[0017] Fluid F _G from the reactor 3 is sent to an unillustrated purifier via the pipe P _G, in the purifier, the predetermined substance (object from a fluid F _G by a known method such as distillation or extraction Substance) is to be purified. Reactor 3 as one embodiment of a flow-type micro-passage of the present invention,
As shown in FIG. 2 (b), it is configured to include a substrate part 31 and a lid part 32 loaded on the substrate part 31. As shown in FIGS. 2A to 2D, a plurality of (two in this case) introduction flow paths 10 </ b> A and 10 </ b> B and these introduction flow paths 10 </ b> A and 10 </ b> B are formed in the substrate portion 31. that a merging path 20 is provided in a groove shape, respectively, when the lid 32 is loaded, the flow path 10A, 10B, 20 is to be formed as a closed cross section channel. In addition, each flow path 10A, 10
B, 20 is configured as a microchannel having an equivalent diameter of 1 cm or less, has a high specific surface area, and can obtain high heat removal efficiency.

The introduction flow channel 10A, 10B, as shown in FIG. 2 (b), one end (upstream end) 11A, 11B is, lid 3
2 are connected to the above-mentioned external pipes P _A and P _B via flow paths 32A and 32B formed at the other end, and the other end (downstream end) is connected to each other to form a junction 15.
Introducing path 10A, the flow path cross-sectional area S _A in the combined unit 15 of 10B, S _B is small (1 cm ² or less, preferably 0.5 cm ²
Or less, more preferably is set to 1 mm ² or less), thereby, the raw material F _A, is introduced / collision to the confluence section 15 at high speed F _B, the mixture is to be efficiently performed.

The merging channel 20 is formed with the merging portion 15 as a base end (upstream end, inlet). A predetermined area 21 on the upstream side including the base end portion 15 has a cross-sectional area S _{M of the} flow channel. introduction flow path 10A, the flow path cross-sectional area S _a of 10B, is set to be smaller than the sum (introduction path total cross-sectional area) S _T of _{S B (S M <S T} , S T = S a + S _B ). That is, the converging section 20 is provided with the throttle section 21 at the entrance. Thus, the introduction channel 10A, 10B is supplied to the raw material F _A, F _B is throttled at the joining portion 15 (diaphragm portion 21), thereby efficiently mixing under turbulent flow conditions.

The flow path cross-sectional area S _M of the diaphragm portion 21 may be smaller than the introduction channel total sectional area S _T above, but with respect to the introduction path total sectional area S _T, preferably 0.05 to 0.5 The range is twice, more preferably 0.1 to 0.3 times. On the other hand, the region 22 of the downstream side of the throttle portion 21, the flow path cross-sectional area S _R is the channel cross-sectional area S is set larger than _M (region 22 region 21 region 21 is expanded Is formed.) That is, the converging section 20 includes the throttle section 21
Is provided on the downstream side of the
In the raw material solution F _A, it reduces the flow speed of the mixture of F _B, are the reaction so as to efficiently conducted to ensure the residence time or reaction time in the reactor 3 under this mixture.

It is preferable that the cross-sectional area S _R of the flow passage of the enlarged portion 22 is set to be at least larger than the total cross-sectional area S _{T of the} introduction path (S _R > S _T ). Further, the flow path cross-sectional area S _R is
In general, the flow passage cross-sectional area S _{M of the} throttle unit 21 is 10
It is 10 to 10,000 times, preferably 20 to 5,000 times, more preferably 30 to 3,000 times. This reactor 3
In the embodiment, since the merging portion 15 is formed as a throttle portion, the pressure loss at the merging portion 15 is larger than that of the conventional reaction channel, but the enlarged portion 22 having a larger cross-sectional area than the conventional merging channel is provided. since the enlarged portion 22 and later the flow rate is decreasing, even in consideration of the pressure loss due to such diaphragm section 21, the raw material solution F _a in the combined channel 20 and thus the reactor 3, reducing the pressure loss of the F _B It can be made to be.

Further, the downstream end of the merging channel 20 (merging channel outlet)
Region 23 including 23a is here formed by reducing relative enlargement 22, downstream end 23a is connected to an external pipe P _G described above. Incidentally, the combined channel 20, feed F _A, because it is location for mixing the F _B reaction, hereinafter also referred to as the reaction path.

The material of the walls forming the flow paths 10A, 10B and 20 (ie, the material of the substrate 31 and the material of the lid 32) is, for example, glass or stainless steel.
Material F _A, F _B and feedstock F _A, as long as it does not affect the reaction of F _B, it may be used various resins. Resin in terms of ease of fabrication is a preferred embodiment. The chemical reaction performed using the present flow-type micro reaction channel, reaction apparatus and reaction method is not limited at all, and examples thereof include an esterification reaction, a transesterification reaction, an amidation reaction, a transamidation reaction, and an acid anhydride. Product synthesis reaction, acid chloride synthesis reaction, hydrolysis reaction, dehydration reaction, reduction reaction, reductive amination reaction, oxidation reaction, dehydrogenation reaction, nitro group synthesis reaction, nitration reaction, electrolytic oxidation reaction, electrolytic reduction reaction, Electrolytic coupling reaction, Hoffman rearrangement reaction, Schmidt reaction, Curtius reaction, Rosen reaction, alkene oxide rearrangement reaction, ether rearrangement reaction, other rearrangement reaction, Diels Alder reaction, hetero Diels Alder reaction, other concerted reaction, hydrogen cyanide reaction, Hoffman elimination reaction of quaternary ammonium salt, dealcoholation reaction of ether, decarboxylation reaction, desorption O ₂ reaction, nucleophilic substitution reaction, halogenation reaction, halogen addition reaction, hydrogen halide addition reaction Michael addition reaction, hydrate hydroboration, hydroformylation, cyanohydrin reaction, the acetal reaction, hemiacetal reaction, aldol reaction, Wittig reaction, Examples include an alkylation reaction, an addition reaction, an acylation reaction, a Suzuki coupling reaction, a diazotization reaction, a diazo coupling reaction, an addition reaction of an organic metal, and a metal exchange reaction of an organic metal.

[0024] As the halogenation reaction, chlorination, bromination, fluorination include iodinated, but not limited to reaction substrate in question, aromatic compounds, heterocyclic compounds, carbonyl-containing compounds, include sugar Can be Examples of the addition reaction of an organic metal include an addition reaction of an organolithium compound to an organic functional group and an addition reaction of a Grignard reagent to an organic functional group. Specific examples of the functional group used in the reaction include a cyano group, an alkylcarbonyl group, an arylcarbonyl group,
Examples include an alkoxycarbonyl group, an aryloxycarbonyl group, and an aminocarbonyl group, specifically, an acyl group, a methoxycarbonyl group, an ethoxycarbonyl group,
Propyloxy carbonyl group, an aminocarbonyl group, dimethylaminocarbonyl group. Specific examples of Grignard reagents include methyl magnesium bromide, ethyl magnesium bromide, propyl magnesium bromide, phenyl magnesium bromide, methyl magnesium chloride, ethyl magnesium chloride, propyl magnesium chloride, and phenyl magnesium chloride.

In the reduction reaction, it is possible to use metals, alloys and metal hydrides. Specific examples of the metal hydride include lithium aluminum hydride, sodium aluminum hydride, lithium borohydride and borohydride. It is possible to use sodium and their deuterium substitutes. The metal-exchange reaction of an organic metal includes a reaction between an organic metal compound and a compound having active hydrogen, and a reaction between an organic metal compound and a compound having a halogen atom. Examples of the reaction between the organometallic compound and the compound having active hydrogen include a lithiation reaction of a secondary amine, and specifically, a synthesis reaction of lithium diisopropylamide from butyllithium and diisopropylamine.

Further, if the reaction substrate and reaction agents is a liquid,
The use of a reaction solvent is not essential, it may be present if desired. Specific examples of preferred solvents include water, liquid ammonia, organic solvents, supercritical solvents, and ionic liquids. As the organic solvent, aliphatic hydrocarbons, aromatic hydrocarbons, ketones, aldehydes, et -
Examples include ters, esters, amines, sulfoxides, alcohols, nitriles, heteroaromatic compounds, halogen solvents, carboxylic acids, and mineral acids include sulfonic acids and phosphoric acids. As the supercritical solvent, supercritical water, supercritical carbon dioxide and the like can be used.
Further, a mixture of these at an arbitrary ratio, the reaction substrate itself, a reactant, a target substance, or a reaction solution can be used as a solvent.

The reaction fluid may be a fluid between miscible with each other, it may be a fluid between immiscible. Fluids that are mixed are solutions that use the same or relatively similar organic solvents, or solutions that use a highly polar organic solvent such as methanol and water, and fluids that are not mixed are hexane. And a solution using a highly polar solvent such as methanol.

The products produced by the flow-type minute reaction channel, the reaction apparatus and the reaction method are not limited. If they are solids, for example, metals, alloys, metal oxides,
Quaternary ammonium salts, quaternary pyridinium salts, alkali metal halide salts, alkaline earth metal halide salts, alkali metal hydroxides, alkaline earth metal hydroxides, boron-containing compounds, aluminum alkoxides, polymers, condensates and the like Is a mixture containing

The flow-type minute reaction channel and the reaction apparatus as one embodiment of the present invention are configured as described above, and are carried out by the following method (reaction method as one embodiment of the present invention). [Hereinafter, a description will be given with reference to FIGS. 1 and 2]. That is, the raw materials F are pumped by the pumps 2A and 2B.
_A, when the F _B introduction path 10A, is fed to 10B, feed F
_A, F _B, the introduction channel 10A having a small cross-sectional area, 10B
The liquid is introduced into the mixing unit 15 at a high speed and merges / collides with each other (first step), and is further throttled by the throttle unit 21 (second step) to promote and mix the turbulent state. Therefore,
As in the prior art described above, the raw material F _A, compared to mixing by molecular diffusion through the interface F _B, can be a mixing efficiency extremely high, thereby, the raw material F _A, the reaction of F _B Efficiency, and thus the production efficiency of the target substance, can be improved.

Then, the raw materials F _A ,
Mixed fluid F _B reacts while flowing through the enlarged portion 22 (third step), this time, the residence in the raw material F _A, the reaction channel 20 of the F _B since the flow rate is reduced by the expansion of the channel cross-section I can secure time. Reactor 3 is adjusted to the optimum temperature for the reaction by the heater 4, thus, such residence time ensured, i.e., the raw material F _A, becomes possible to secure the reaction time F _B, also in this respect, material F _a, it is possible to improve the production efficiency of the reaction efficiency and thus the target substance F _B.

Further, since the enlarged portion 22 is provided as described above, even if the pressure loss due to the throttle portion 21 is considered,
Compared to the prior art, the raw material solution F _A in the reactor 3, has to be able to reduce the pressure loss of the F _B. Therefore,
According to the flow-type micro reaction channel, the reaction apparatus and the reaction method,
There is an advantage that the productivity of the target substance can be improved without increasing the pressure loss.

[0032] Incidentally, if it is necessary, the raw material F _A, F _B reactor 3 to passed through to the the prior channel 10A, to 10B, 20 in, by circulating an inert gas in a solvent or reaction If necessary, the reactor 3 itself may be dried. The flow-type minute reaction channel and the reaction apparatus of the present invention are not limited to the above-described embodiments, and various modifications can be made without departing from the spirit of the present invention.

For example, in the above-described embodiment,
Predetermined area 2 including junction 15 of introduction flow paths 10A and 10B
1 is shown, but the converging section is connected to the merging section 15.
In order to mix the raw material F _A, the F _B effectively by introducing flow channel 10
It is sufficient that the flow path is narrowed with respect to A and 10B. For example, as shown in FIGS. 3A and 3B, the flow path may be formed by the merging portion 15 itself (that is, as shown in FIG. ),
(In the plan view shown in (b), the aperture portion may be formed not as an area but as a spot.) Figure 3 (a), the feed F
_A, the flow path along the flow direction of F _B are the degree of expansion of the (enlarged portion) 22 is fixed, in FIG. 3 (b), the degree of such expansion, gradually increases along the flow direction It is set as follows.

As shown in FIGS. 4A to 4E,
One or more rectifications are provided in the enlarged portion 22 of the merged channel 20 so as to substantially uniformly divide the merged channel 20 along the width direction of the merged channel 20 (the direction perpendicular to the direction of travel of the raw material flowing through the merged channel 20). A plate (rectifying means) 5 may be provided. By providing the rectifying plates 5, when the raw material F _A, is F _B flows through the confluence passage 20, it is possible to prevent the may flow in the width direction,
Material F _A, a reduction in the production efficiency of the target substance due to variation in the residence time of the F _B can be suppressed.

As shown in FIG. 4 (e), the rectifying means has a relatively high height and both the lid 32 and the merging channel 20 (the enlarged portion 2).
It predetermined range of 2) may be those resulting partitions completely, as shown in FIG. 5 (a), the combined channel 20 (enlarged portion 22) may be one which does not completely partitioned. Alternatively, a predetermined area of the merging channel 20 (the enlarged portion 22) is
As shown in (b), a plurality of cylindrical branch channels 25 may be arranged along the width direction of the merging channel 20. In this case, a portion which forms between the respective mutual branch channel 25 in the substrate 31 'functions as a rectifying means. The branch channel 25 is formed by, for example, penetrating the substrate portion 31 'with a drill or the like.

In the above embodiment, the introduction flow path 10
A, 10B and the merging channel 20 are the substrate portions 31, 3 respectively.
An example is shown which is formed in a groove shape at the 1 ', for example, as shown in FIG. 6, each passage 10A, 10B, 20 and may be constituted by a pipe. Further, in the above-described embodiment, the example in which the two introduction flow paths are merged has been described.
The number is not limited to one and may be any number.

In the above-described embodiment, the reactor is constituted by one flow-type reaction passage 3. However, as shown in FIG. 7, a plurality of flow-type reaction passages 3 are stacked to form a reactor 3 '. May be formed to increase the production amount of the target substance. Although FIG. 7 shows the reactor (reactor 3 ′) as having a configuration in which seven flow-type micro reaction channels are provided, the number of flow-type micro reaction channels is not limited to this and may be set as appropriate. can do.

[0038]

EXAMPLES (A) Example Hereinafter, micro-flow-type reaction channel as an embodiment of the invention with reference to FIGS. 8 and 9, will be described reactor and the reaction method, an embodiment of the present invention reactor as is substantially similar to the embodiment described above, as shown in FIG. 8, a predetermined raw material (reactant fluid) F _a, the tank for accommodating the F _B 1A, 1B
, A reactor (flow-type microreaction channel) 3 ″, raw material F _A ,
Container 1C which houses F _B pipe P _A, a pump (reaction fluid circulating device) for feeding to the reactor 3 "via the P _B 2A, and 2B, the fluid which has passed through the reactor 3 containing a target substance
It is configured with and. Further, the reactor 3 'is placed in a thermostat bath 5 which is maintained at 0 ° C, the ambient temperature, the raw material F _A, it is adjusted to the optimum temperature for the reaction of F _B.

As shown in the sectional view of FIG. 9 (b), the reactor 3 ″ as one embodiment of the micro flow type reaction channel of the present invention has inlet channels 60A and 60B and inlet channels 60A and 60A.
B is formed with a merging channel 70 formed by merging. The introduction flow paths 60A and 60B are connected to the raw material supply ports 61A and 61B of FIG. 9A, respectively, and the raw material supply ports 61A and 61B are connected to the pipe P shown in FIG.
_A, are connected to the P _B. In addition, the combined channel 70
Communicates with a discharge port 75 connected to a pipe P _G (see FIG. 8).

The flow paths 60A, 60B, 70 are
It is provided at a depth of 0.5mm to. 60A of the introduction flow channel in the immediate upstream side of the mixing portion 65, the width b ₁ of the 60B is set to 0.5 mm. Therefore, the cross-sectional shape of the introduction flow channels 60A and 60B is a square having a side length of 0.5 mm, and each of the cross-sectional areas S _A and S _B is 0.25 mm ² . Further, the mixing section 65 of the merging channel 70
Immediately downstream, the cross-sectional area of the introduction channel 60A, 60B of
Is formed as a constricted portion 71 smaller than the sum S _T (= S _A + S _B = 0.5) of the cross-sectional areas of.

In this case, the restricting section 71 is connected to the inlet channel 60.
The width dimension is set to 0.5 mm as in A and 60B, the cross-sectional shape is a square with a side length of 0.5 mm, and the cross-sectional area S _M is 0.25 mm ² . Also,
Length L ₁ of the throttle portion 71 is set to 1 mm. Each dimension of the enlarged portion 72 is b ₂ = 5.
0 mm, L ₂ = 10 mm, is set in L ₃ = 106 mm, the equivalent diameter of the channel cross-sectional area and flow path cross section, respectively, 25 mm ² at most, about 1 mm. In addition, the volume of the reaction section (merging flow path) 70 involved in the reaction on the downstream side of the mixing section 65 of the reactor 3 is set to 2.7 due to the above dimension setting.
It becomes 8 mL (milliliter).

In such an apparatus, a Grignard reagent (methylmagnesium bromide) in a THF solution [3.0 mol
l / l (mol / liter)] and ketone (4-Phenyl-2buta
a THF solution of none) [1.0 mol / l (mol / l)], but each said feedstock F _A, is supplied in the reactor as F _B 0.5 L (liters) / h, alcohols (2-
Methyl, 4-Phenyl, 2-butanol) was produced.
From the above conditions, these mixed liquids are supplied to the reaction section (combined flow path) 7.
For 0, 1 L (liter) / h (about 10
mm / sec) and stayed in the reaction section 70 for about 10 seconds. As a result, a conversion of about 80% was obtained.

This reaction is an exothermic reaction (heat of reaction: about 300 k
A J / mol), to produce a target substance by suppressing the generation of by-products efficiently, the heat generated by the reaction is removed with high efficiency, the liquid in the reactor 3 in "warm (feed F _a, it is necessary to maintain the temperature) as possible to a low temperature of F _B. in this reactor 3 ', as described above it, the equivalent diameter of the cross section of the joining path (reaction section) 70 is 1mm at most As a result, the rise in liquid temperature could be suppressed within 1 ° C., and a high conversion rate was obtained as described above. (B) Comparative Example In the conventional structure as shown in FIG. 10 described above, like the reactor 3 ″ as one embodiment of the present invention, the cross-sectional shape of the merging flow path (reaction path) 102 is one side. 0.5 mm square (cross-sectional area 0.25 mm ² )
Was set to be 2.78 mL (milliliter), and the length of the reaction path 102 was 11,200 mm.

[0044] Further, similarly to the above embodiment, and a THF solution of the THF solution with a ketone of the Grignard reagent was fed at 0.5 L (liters) / h, respectively reactor as a starting material F _A, F _B. Thus, the raw material F _A in the reaction path within 102, F _B
Of the mixed fluid was about 1,000 mm / sec. That is, in order to obtain the same heat removal performance and the same production time as in the above-mentioned example with the same heat removal performance and the same residence time of the raw material in the reaction section, the equivalent diameter and the reaction path volume are made the same. , raw F _a in the reaction channel 102., the flow velocity of the mixed fluid F _B, it became about 100 times the above-described embodiment. (C) Results pressure loss in the reaction path of the fluid (raw material) is proportional to the square of the flow rate, the reaction in the apparatus and reactor 3 'of this embodiment, if you try to produce the same amount of the desired product Such a flow rate can be reduced to about 1/100 of that in the related art, and the pressure loss of the entire reaction path can be reduced even in consideration of the pressure loss due to the throttle section 71.

[0045]

As described above in detail, according to the flow-type minute reaction channel, the reaction apparatus and the reaction method of the present invention, a plurality of reaction fluids are introduced into the junction via the introduction passage having a minute cross-sectional area. It flows in and collides at high speed, and is further throttled by a throttle having a smaller cross-sectional area than the total cross-sectional area of the introduction path. Since the gas flows through the enlarged portion having a larger cross-sectional area, the flow velocity is suppressed, and therefore, while suppressing an increase in pressure loss, the reaction fluid is effectively mixed, and the reaction time at the junction is secured. There is an advantage that the productivity of the substance can be improved.

[Brief description of the drawings]

FIG. 1 is a schematic perspective view showing the entire configuration of a reaction apparatus as one embodiment of the present invention.

FIGS. 2A and 2B are diagrams showing a configuration of a micro-flow-type reaction channel as one embodiment of the present invention, wherein FIG. 2A is a plan view thereof, and FIG.
Is a cross-sectional view taken along line X1-X1 of (a), and FIG.
X2 sectional view, (d) is an X3-X3 sectional view of (a),
(E) is a X4-X4 sectional view of (a).

FIGS. 3 (a) and 3 (b) are schematic plan views showing a main configuration of a modified example of the micro flow channel as one embodiment of the present invention.

4A and 4B are diagrams showing a configuration of a modified example of the micro flow type reaction channel as one embodiment of the present invention, wherein FIG. 4A is a plan view thereof, and FIG. 4B is a sectional view taken along line Y1-Y1 of FIG. (C) is a sectional view taken along line Y2-Y2 of (a), and (d) is a sectional view taken along Y3-Y of (a).
3 is a cross-sectional view, and (e) is a Y4-Y4 cross-sectional view of (a).

[Figure 5] is a diagram showing a configuration of a variation of the micro flow type reaction channel according to an embodiment of the present invention, (a), (b) is a schematic sectional view corresponding to FIG. 4 (e) It is.

6 is a schematic perspective view showing a main part of a modification of the micro flow type reaction channel structure of an embodiment of the present invention.

FIG. 7 is a schematic perspective view showing the overall configuration of a modified example of the reactor as one embodiment of the present invention.

FIG. 8 is a schematic diagram showing the overall configuration of a reaction apparatus as one embodiment of the present invention.

[Figure 9] is a diagram showing an entire configuration of a micro-flow-type reaction channel as an embodiment of the present invention, (a) is its schematic perspective view, A-A cross section of (b) is (a) FIG.

FIG. 10 is a schematic plan view showing the entire configuration of a conventional micro flow reaction channel.

[Explanation of symbols]

1A~1C tanks 2A, 2B pump (reaction fluid circulating device) 3,3 "flow-through micro-channel 3 'reactor 4 electrothermal board 5 rectifying means (rectification plate) 10A, 10B, 60A, 60B introduction channel 15, 65 merging portion 20, 70 joining path 21 and 71 stop portion 22 and 72 expanding portion 31 substrate 32 lid P _A, P _B, P _G pipe F _A, F _B material (reactant fluid) S _A, S _B introduction flow Cross-sectional area of road S _T Sum of cross-sectional areas of introduction flow path S _M Cross-sectional area of merge flow path

 ────────────────────────────────────────────────── ─── front page of continued F-term (reference) 4G075 AA63 BD15 BD22 EA06 EB01

Claims (10)

[Claims] A reaction fluid having a plurality of introduction channels each having a minute cross-sectional area, and a joining channel formed by joining the introduction channels at a junction, and flowing through each of the introduction channels. Wherein the converging flow path is formed in the merging section and has a cross-sectional area smaller than the sum of the cross-sectional areas of the introduction flow paths; A flow-type micro reaction channel, comprising: an enlarged portion provided downstream of the throttle portion and having a cross-sectional area larger than the cross-sectional area of the throttle portion. 2. The flow-type micro reaction channel according to claim 1, wherein a cross-sectional area of the flow channel at the junction of the introduction flow channel is 1 cm ² or less. 3. The flow-type micro reaction channel according to claim 1, wherein an equivalent diameter of a cross section of the junction channel is 1 cm or less. Sectional area of 4. the narrowed portion, characterized in that it is set in 0.01 to 0.8 times greater than the sum of the cross-sectional area of the introduction flow path, claim 1 4. The flow-type minute reaction channel according to any one of items 3 to 5. 5. The cross-sectional area of the enlarged portion is set in a range of 30 times to 3000 times the cross-sectional area of the narrowed portion. Flow type micro reaction channel. 6. The device according to claim 1, wherein one or more rectifying plates for partitioning the enlarged portion substantially uniformly in the width direction are provided in the enlarged portion. Flow type micro reaction channel. 7. A flow-type minute reaction channel according to any one of claims 1 to 6, further comprising one or more flow-type minute reaction channels, and a reaction fluid is supplied to each of the introduction flow paths of the flow-type minute reaction channel. A reaction device characterized by comprising a reaction fluid drive device for flowing the same. 8. A reaction method for joining / reacting a plurality of reaction fluids flowing through a minute introduction flow path, wherein the first step of joining the plurality of reaction fluids at a junction of the introduction flow paths; A second step of squeezing the mixed reaction fluid with a throttle having a smaller cross-sectional area than the sum of the cross-sectional areas of the introduction flow paths; and having the mixed reaction fluid having a larger cross-sectional area than the throttle. A reaction method, comprising: a third step of causing a reaction in an enlarged portion. 9. The reaction method according to claim 8, wherein a cross-sectional area of the flow path at the junction of the introduction flow path is 1 cm ² or less. 10. The reaction method according to claim 8, wherein an equivalent diameter of each cross section of the narrowed portion and the enlarged portion is 1 cm or less.