Micro-distillation device and distillation method using same

Abstract

A micro-distillation device comprises: a distillation unit including a liquid introduction port for introducing a mixed liquid containing at least two components having different boiling points, a vapor introduction port for separately introducing vapors originating from the mixed liquid, a gas-liquid contact flow path in which the mixed liquid introduced from the liquid introduction port and the vapor originating from the mixed liquid introduced from the vapor introduction port are brought into contact with each other in counterflow, a liquid discharge port for discharging the mixed liquid flowing through the gas-liquid contact flow path, and a vapor discharge port for discharging the vapor originating from the mixed liquid flowing through the gas-liquid contact flow path; a first circulation unit in which a condensate obtained by condensing the vapor originating from the mixed liquid discharged from the vapor discharge port is circulated to the liquid introduction port; and a second circulation unit in which a vapor obtained by evaporating the mixed liquid discharged from the liquid discharge port is circulated to the vapor introduction port.

Description

Microdistillation device and distillation method using the same

[0001] The present disclosure relates to a microdistillation device and a distillation method using the same.

[0002] In chemical synthesis, which produces a target compound through a chemical reaction, unwanted by-products are usually also produced. In response to this, a technique is known for separating a target component from other components in a mixture containing at least two components by utilizing gas-liquid contact (see, for example, Patent Document 1).

[0003] Japanese Patent Application Laid-Open No. 2006-198542 Japanese Patent Application Laid-Open No. 2007-136280 Japanese Patent No. 5627837

[0004] However, in the past, the efficiency of separating a specific component contained in a mixed liquid from other components by distillation was not particularly high, and there was room for improvement in this regard. The technology disclosed herein has been made in consideration of this situation, and its purpose is to provide a micro-distillation device that can efficiently separate a specific component contained in a mixed liquid from other components.

[0005] The gist of the present disclosure is as follows: [Aspect 1] A micro-distillation device according to Aspect 1 comprises a distillation unit including: a liquid inlet for introducing a mixed liquid containing at least two components with different boiling points, vapor inlets for introducing vapors derived from the mixed liquid, a gas-liquid contact flow path that brings the mixed liquid introduced from the liquid inlet and the vapor derived from the mixed liquid introduced from the vapor inlet into contact with each other in counterflow, a liquid outlet for discharging the mixed liquid that has flowed through the gas-liquid contact flow path, and a vapor outlet for discharging the vapor derived from the mixed liquid that has flowed through the gas-liquid contact flow path, a first circulation unit that circulates a condensed liquid obtained by condensing the vapor derived from the mixed liquid discharged from the vapor outlet to the liquid inlet, and a second circulation unit that circulates vapor obtained by evaporating the mixed liquid discharged from the liquid outlet to the vapor inlet. [Aspect 2] The micro-distillation device according to Aspect 1, wherein in the distillation unit, the gas-liquid contact channel is configured as a channel extending in one direction, one end side of the gas-liquid contact channel is arranged vertically upward, and the liquid inlet and the vapor outlet are arranged at this end, and the other end side of the gas-liquid contact channel is arranged vertically downward, and the liquid outlet and the vapor inlet are arranged at this other end. [Aspect 3] The micro-distillation device according to Aspect 1 or 2, wherein in the distillation unit, the mixed liquid introduced from the liquid inlet flows down a liquid flow region formed along a channel wall surface that forms the gas-liquid contact channel, and vapor derived from the mixed liquid supplied from the vapor inlet flows in the opposite direction to the mixed liquid along a vapor flow region formed on the central side of a cross section of the gas-liquid contact channel. [Aspect 4] The micro-distillation device according to any of Aspects 1 to 3, wherein the distillation unit has a plurality of the liquid inlets and a plurality of the liquid outlets.[Aspect 5] The micro-distillation device according to Aspect 4, wherein the channel wall surface in the distillation unit includes a first surface and a second surface different from the first surface, the plurality of liquid inlets include first and second liquid inlets arranged on one end side of the gas-liquid contact channel, and the plurality of liquid outlets include first and second liquid outlets arranged on the other end side of the gas-liquid contact channel, wherein the mixed liquid introduced from the first liquid inlet flows down the first surface of the channel wall surface and is then discharged from the first liquid outlet, and the mixed liquid introduced from the second liquid inlet flows down the second surface of the channel wall surface and is then discharged from the second liquid outlet. [Aspect 6] The micro-distillation device according to Aspect 2, wherein the distillation unit further includes an intermediate inlet for introducing the mixed liquid into an intermediate position of the gas-liquid contact channel, in addition to the liquid inlet arranged on one end side of the gas-liquid contact channel. [Aspect 7] The microdistillation device according to any one of Aspects 1 to 6, wherein the first circulation unit has a first storage tank for storing condensed liquid obtained by condensing vapor derived from the mixed liquid discharged from the vapor outlet. [Aspect 8] The microdistillation device according to any one of Aspects 1 to 7, wherein the second circulation unit has a second storage tank for storing the mixed liquid discharged from the liquid outlet of the distillation unit. [Aspect 9] The microdistillation device according to any one of Aspects 1 to 8, wherein the second circulation unit further comprises an evaporation unit having a microchannel through which the mixed liquid discharged from the liquid outlet of the distillation unit circulates, and an evaporation heater for evaporating the mixed liquid flowing through the microchannel. [Aspect 10] The microdistillation device according to any one of Aspects 1 to 9, wherein the distillation unit further comprises a temperature adjustment mechanism for forming a predetermined temperature gradient in which the temperature gradually decreases from the other end side to one end side of the gas-liquid contact channel. [Aspect 11] The micro-distillation device according to Aspect 2, wherein in the distillation unit, a liquid inlet channel connecting one end of the gas-liquid contact channel to the liquid inlet, and a liquid outlet channel connecting the other end of the gas-liquid contact channel to the liquid outlet are each formed as a microchannel.[Aspect 12] The microdistillation device according to Aspect 3, wherein the liquid film thickness of the mixed liquid flowing down along the wall surface of the flow channel is on the order of micrometers. [Aspect 13] A distillation method for distilling a mixed liquid containing at least two components with different boiling points, using the microdistillation device according to Aspect 1. [Aspect 14] The mixed liquid contains a predetermined low-boiling point component and a high-boiling point component having a boiling point higher than that of the low-boiling point component, and in the distillation unit, the mixed liquid introduced from the liquid inlet and the vapor derived from the mixed liquid introduced from the vapor inlet are brought into gas-liquid countercurrent contact in the gas-liquid contact flow path, thereby evaporating the low-boiling point component contained in the mixed liquid, thereby discharging the liquid-phase low-boiling point component from the vapor outlet together with the vapor derived from the mixed liquid introduced from the vapor inlet, and discharging the liquid-phase high-boiling point component from the liquid outlet together with the mixed liquid introduced from the liquid inlet, and the first circulation unit continuously circulates, to the liquid inlet, a condensate obtained by condensing the vapor in which the low-boiling point component is concentrated, which is discharged from the vapor outlet of the distillation unit, the second circulation unit continuously circulates the vapor obtained by evaporating the mixed liquid in which the high-boiling-point component is concentrated, discharged from the liquid outlet of the distillation unit, to the vapor inlet, thereby separating the low-boiling-point component and the high-boiling-point component contained in the mixed liquid.

[0006] The technology disclosed herein can provide a micro-distillation device that can efficiently separate a specific component contained in a mixed liquid from other components.

[0007] FIG. 1 is a schematic diagram showing an example of a micro-distillation device according to embodiment 1. FIG. 2 is a plan view of a distillation unit according to embodiment 1. FIG. 3 is a diagram illustrating a method for producing a distillation unit according to embodiment 1. FIG. 4 is a schematic diagram showing a cross section taken along the line A-A in FIG. 2. FIG. 5 is a diagram illustrating a temperature adjustment mechanism. FIG. 6 is a diagram illustrating temperature measurement points in an example. FIG. 7 is a diagram illustrating an experimental apparatus used in a comparative example. FIG. 8 is a diagram illustrating a micro-distillation device according to embodiment 2.

[0008] Below, a microdistillation device according to an embodiment of the present disclosure will be described with reference to the drawings. Each configuration and their combinations in the embodiments are merely examples, and addition, omission, substitution, and other modifications of the configurations are possible as appropriate without departing from the spirit of the present disclosure. The present disclosure is not limited by the embodiments, but only by the claims. Furthermore, each aspect disclosed in this specification can be combined with any other feature disclosed in this specification.

[0009] First Embodiment Microdistillation Device FIG. 1 is a schematic diagram showing an example of a microdistillation device 1 according to a first embodiment.

[0010] The micro-distillation device 1 is a microfluidic device equipped with a distillation unit 2, a first circulation unit 5, a second circulation unit 6, etc., for performing a distillation operation on a mixed fluid containing at least two components with different boiling points. In this specification, the term "fluid" may include not only liquids and gases, but also mixtures of liquids and gases, and multiphase fluids in which solids are mixed with liquids and / or gases.

[0011] [Distillation Unit] Figure 2 is a plan view of the distillation unit 2 according to embodiment 1. The symbol B in the figure denotes the substrate of the distillation unit 2. Substrate B has the form of a rectangular plate-like chip. As will be described in detail later, the distillation unit 2 is configured so that a mixed liquid containing at least two components with different boiling points (hereinafter simply referred to as the "mixed liquid") is supplied from a first circulation unit 5, and vapor obtained by evaporating the mixed liquid is supplied from a second circulation unit 6. The up, down, left, and right directions shown in Figure 2 are given for convenience in explaining the relative positional relationship of each element with respect to substrate B of the distillation unit 2, and do not indicate the absolute orientation of each element.

[0012] The distillation unit 2 according to this embodiment includes a liquid inlet 21 for introducing the mixed liquid supplied from the first circulation unit 5, a steam inlet 22 for introducing steam derived from the mixed liquid supplied from the second circulation unit 6, a gas-liquid contact flow path 23 for bringing the mixed liquid introduced from the liquid inlet 21 and the steam derived from the mixed liquid introduced from the steam inlet 22 into contact with each other in counterflow, a liquid outlet 24 for discharging the mixed liquid that has flowed through the gas-liquid contact flow path 23, and a steam outlet 25 for discharging the steam derived from the mixed liquid that has flowed through the gas-liquid contact flow path 23. The liquid inlet 21, the steam inlet 22, the gas-liquid contact flow path 23, the liquid outlet 24, the steam outlet 25, etc. are formed on the substrate B.

[0013] The shape of the gas-liquid contact channel 23 is not particularly limited. In the example shown in FIGS. 1 and 2 , the gas-liquid contact channel 23 is configured as a channel extending in one direction (straight line). Of the ends of the gas-liquid contact channel 23 in the extension direction (axial direction), one end designated by reference symbol 23A is referred to as the "first end," and the other end designated by reference symbol 23B is referred to as the "second end." In this embodiment, the liquid inlet 21 and the steam outlet 25 are disposed on the first end 23A side of the gas-liquid contact channel 23, and the liquid outlet 24 and the steam inlet 22 are disposed on the second end 23B side. However, these arrangements are merely exemplary. The length of the gas-liquid contact channel 23 in the extension direction (axial direction) (the length from the first end 23A to the second end 23B) can be 10 mm or more and 3000 mm or less, preferably 20 mm or more and 2000 mm or less, and more preferably 30 mm or more and 1000 mm or less.

[0014] The distillation unit 2 further includes a liquid inlet channel 26 connecting the first end 23A (one end) of the gas-liquid contact flow path 23 to the liquid inlet 21, and a liquid outlet channel 27 connecting the second end 23B (the other end) of the gas-liquid contact flow path 23 to the liquid outlet 24. The mixed liquid supplied from the first circulation unit 5 to the liquid inlet 21 of the distillation unit 2 is guided to the first end 23A of the gas-liquid contact flow path 23 through the liquid inlet channel 26. The mixed liquid guided to the first end 23A of the gas-liquid contact flow path 23 flows through the gas-liquid contact flow path 23 along the linearly extending gas-liquid contact flow path 23 (i.e., from the first end 23A toward the second end 23B). The mixed liquid after flowing through the gas-liquid contact flow path 23 then flows through a liquid outlet channel 27 connected to the second end 23B of the gas-liquid contact flow path 23, and is then discharged from the distillation unit 2 through the liquid outlet 24.

[0015] 1 and 2, the distillation unit 2 has two liquid inlets 21, which are referred to as a first liquid inlet 21A and a second liquid inlet 21B when they are to be distinguished from one another. The distillation unit 2 also has two liquid outlets 24, which are referred to as a first liquid outlet 24A and a second liquid outlet 24B when they are to be distinguished from one another. However, the number of liquid inlets 21 and liquid outlets 24 in the distillation unit 2 is not particularly limited.

[0016] 1 and 2, the distillation unit 2 has two liquid inlet channels 26 corresponding to the liquid inlets 21A, 21B, and two liquid outlet channels 27 corresponding to the liquid outlets 24A, 24B. The first liquid inlet channel 26A connects the first liquid inlet channel 21A to the first end 23A of the gas-liquid contact channel 23. The second liquid inlet channel 26B connects the second liquid inlet channel 21B to the first end 23A of the gas-liquid contact channel 23. The first liquid outlet channel 27A connects the second end 23B of the gas-liquid contact channel 23 to the first liquid outlet 24A. The second liquid outlet channel 27B connects the second end 23B of the gas-liquid contact channel 23 to the second liquid outlet 24B. As shown in FIG. 2, the liquid inlet channel 26 and the liquid outlet channel 27 each have a curved shape in a plan view of the distillation unit 2. However, the shapes of the liquid inlet channel 26 and the liquid outlet channel 27 are not particularly limited.

[0017] The distillation unit 2 further includes a steam inlet channel 28 connecting the second end 23B of the gas-liquid contact flow channel 23 to the steam inlet 22, and a steam outlet channel 29 connecting the first end 23A of the gas-liquid contact flow channel 23 to the steam outlet 25. Steam derived from the mixed liquid supplied from the second circulation unit 6 to the steam inlet channel 28 of the distillation unit 2 is guided to the second end 23B of the gas-liquid contact flow channel 23 through the steam inlet channel 28. The steam derived from the mixed liquid guided to the second end 23B of the gas-liquid contact flow channel 23 flows through the gas-liquid contact flow channel 23 along the gas-liquid contact flow channel 23, which extends linearly (i.e., from the second end 23B toward the first end 23A). In other words, the flow direction of the steam derived from the mixed liquid along the gas-liquid contact flow channel 23 is opposite to the flow direction of the mixed liquid flowing from the first end 23A toward the second end 23B. Then, the vapor derived from the mixed liquid after flowing through the gas-liquid contact flow path 23 flows through the vapor discharge path 29 connected to the first end 23A side of the gas-liquid contact flow path 23, and is then discharged outside the distillation unit 2 through the vapor discharge port 25.

[0018] As an example, the distillation unit 2 can be produced by forming the above-mentioned liquid inlet 21, vapor inlet 22, gas-liquid contact flow path 23, liquid outlet 24, vapor outlet 25, liquid inlet path 26, liquid outlet path 27, vapor inlet path 28, vapor outlet path 29, etc. on the substrate B.

[0019] FIG. 3 illustrates a method for fabricating the distillation unit 2 according to the first embodiment. The first substrate B1 shown in FIG. 3 is, for example, a substrate that forms the front side of the distillation unit 2. The third substrate B3 is, for example, a substrate that forms the rear side of the distillation unit 2. The second substrate B2 is, for example, a substrate that forms an intermediate layer sandwiched between the first substrate B1 and the third substrate B3. Each of the substrates B1 to B3 is a plate-like member that is rectangular in plan view and has, for example, a congruent planar shape. However, the shape and size of each of the substrates B1 to B3 are not particularly limited. The material of each of the substrates B1 to B3 is not particularly limited, and examples thereof include glass, silicon, silica, quartz, resin, and silicon carbide. It is preferable to use borosilicate glass, which is resistant to organic chemicals and heat-resistant, as the material for the substrates B1 and B2.

[0020] In a method for fabricating the distillation unit 2, for example, openings for forming the liquid inlet 21, the vapor inlet 22, the liquid outlet 24, the vapor outlet 25, etc. are formed in the first substrate B1 as through-holes penetrating the first substrate B1 in the thickness direction. Furthermore, openings for forming channels such as the gas-liquid contact channel 23, the liquid inlet channel 26, the liquid outlet channel 27, the vapor inlet channel 28, and the vapor outlet channel 29 are formed in the second substrate B2 as through-holes penetrating the second substrate B2. The first substrate B1 may then be bonded to one surface of the second substrate B2, and the third substrate B3 may be bonded to the other surface of the second substrate B2. This allows the various channels described above for circulating the mixed liquid and vapor derived from the mixed liquid within the substrate assembly. The substrates forming the distillation unit 2 may be transparent or translucent. This allows each channel, such as the gas-liquid contact channel 23, the liquid inlet channel 26, the liquid outlet channel 27, the vapor inlet channel 28, and the vapor outlet channel 29, to be visually observed from the outside.

[0021] The method for forming the through holes in the first substrate B1 and the second substrate B2 is not particularly limited, and the through holes may be formed, for example, by etching or micro-cutting the first substrate B1 and the second substrate B2. Of course, the above-described method for fabricating the distillation unit 2 is merely an example, and various other fabrication methods can be employed, and are not particularly limited. For example, the distillation unit 2 may be fabricated by stacking two or more substrates, or by stacking four or more substrates. Note that one-touch joints, such as tube fittings, can be attached to the openings for forming the liquid inlet 21, the vapor inlet 22, the liquid outlet 24, the vapor outlet 25, etc.

[0022] The distillation unit 2 configured as described above is formed, for example, as a chip-type microfluidic device having microscale flow channels. When the distillation unit 2 is in use, the first end 23A of the gas-liquid contact flow channel 23 is arranged vertically upward (facing upward), and the second end 23B is arranged vertically downward (facing downward). Hereinafter, the direction in which the gas-liquid contact flow channel 23 extends in the distillation unit 2 will be referred to as the "vertical direction," and the left-right direction will be referred to as the "width direction."

[0023] Furthermore, in the distillation unit 2, the liquid inlet channel 26 and the liquid outlet channel 27 are each formed as a microchannel. In the present specification, at least one of the channel width and channel height of the liquid inlet channel 26 and the liquid outlet channel 27 formed as microchannels is on the order of micrometers (μm). For example, the channel width of the liquid inlet channel 26 and the liquid outlet channel 27 can be 100 μm or more and 800 μm or less, preferably 150 μm or more and 600 μm or less, and more preferably 200 μm or more and 500 μm or less. The channel height of the liquid inlet channel 26 and the liquid outlet channel 27 can be 100 μm or more and 5000 μm or less, preferably 150 μm or more and 4000 μm or less, and more preferably 200 μm or more and 3000 μm or less.

[0024] Figure 4 is a schematic diagram showing a cross section taken along the line A-A in Figure 2. That is, Figure 4 shows a cross section of the gas-liquid contact flow path 23 in the distillation unit 2. The cross section of the gas-liquid contact flow path 23 is a cross section in a direction perpendicular to the axial direction in which the gas-liquid contact flow path 23 extends. The cross-sectional shape of the gas-liquid contact flow path 23 shown in Figure 4 is one example, and in the example shown in Figure 4, the gas-liquid contact flow path 23 has a rectangular cross section.

[0025] Reference numerals 231 to 234 in FIG. 4 denote first to fourth channel wall surfaces that form the gas-liquid contact channel 23. The distillation unit 2 in this embodiment is configured so that a liquid flow region is formed on all or part of each of the channel wall surfaces 231 to 234, and the mixed liquid flows down along the liquid flow region. In the example shown in FIG. 4, the first channel wall surface 231 and the second channel wall surface 232 are arranged to face each other and extend, for example, along the side surface of the distillation unit 2. Similarly, the third channel wall surface 233 and the fourth channel wall surface 234 are arranged to face each other and extend, for example, along the front surface of the distillation unit 2.

[0026] For example, the first flow path wall surface 231 in the gas-liquid contact flow path 23 is connected flush with the flow path wall surface 26A1 (see FIG. 2) in the first liquid inlet path 26A. Here, "flush" refers to a mode in which the wall surfaces are connected without forming a step at the connection point. Furthermore, the second flow path wall surface 232 in the gas-liquid contact flow path 23 is connected flush with the flow path wall surface 26B1 (see FIG. 2) in the second liquid inlet path 26B. In this mode, when the mixed liquid introduced from the first liquid inlet 21A in the distillation unit 2 flows into the gas-liquid contact flow path 23 through the first liquid inlet path 26A, the mixed liquid is easily allowed to flow down along the first flow path wall surface 231 (first surface) that is connected flush with the flow path wall surface 26A1 of the first liquid inlet path 26A. In this way, after the mixed liquid flows downward along the first flow path wall surface 231, the mixed liquid is discharged from the first liquid outlet 24A through the first liquid discharge path 27A. Similarly, when the mixed liquid introduced from the second liquid inlet 21B in the distillation unit 2 flows into the gas-liquid contact flow path 23 through the second liquid inlet path 26B, the mixed liquid is more likely to flow downward along the second flow path wall surface 232 (a second surface different from the first surface) that is connected flush with the flow path wall surface 26B1 of the second liquid inlet path 26B. In this way, after the mixed liquid flows downward along the second flow path wall surface 232, the mixed liquid is discharged from the second liquid outlet 24B through the second liquid discharge path 27B. In this way, the mixed liquid is introduced into two different flow path walls 231, 232 in the gas-liquid contact flow path 23 of the distillation unit 2 through two systems, and the mixed liquid that has flowed down the flow path walls 231, 232 is discharged through two systems, so that the mixed liquid can flow smoothly along the flow path walls 231, 232. Moreover, the flow rate of the mixed liquid can be easily ensured while preventing the gas-liquid contact flow path 23 from being blocked by the mixed liquid.

[0027] As described above, the gas-liquid contact flow path 23 in the distillation unit 2 can cause all or part of the vertically extending flow path wall surfaces 231 to 234 (for example, the first flow path wall surface 231 and the second flow path wall surface 232) to function as wetted walls through which the mixed liquid flows in the form of a thin film. This allows the mixed liquid to flow down along the flow path wall surfaces that form the gas-liquid contact flow path 23, while forming a hollow vapor flow region, through which vapor derived from the mixed liquid flows, at the center of the cross section of the gas-liquid contact flow path 23.

[0028] In the exemplary embodiment shown in FIG. 4 , the mixed liquid (designated by Lq in FIG. 4 ) flows down along the liquid flow region RL formed on the first flow path wall surface 231 and the second flow path wall surface 232. Furthermore, in the hollow vapor flow region RG formed at the center of the cross section of the gas-liquid contact flow path 23, vapor derived from the mixed liquid flows along the vapor flow region RG in the opposite direction to the mixed liquid. This prevents the gas-liquid contact flow path 23 from being clogged by the mixed liquid. As a result, the mixed liquid introduced through the liquid inlet 21 and the vapor derived from the mixed liquid introduced through the vapor inlet 22 can be brought into counterflow contact with each other in the gas-liquid contact flow path 23. This allows efficient heat and mass exchange between the vapor derived from the mixed liquid and the mixed liquid, resulting in an efficient distillation operation. In particular, the distillation unit 2 of this embodiment utilizes gravity to allow the mixed liquid to flow down along the flow path wall surface of the gas-liquid contact flow path 23. That is, the channel wall surface extending in the vertical direction of the gas-liquid contact channel 23 can function as a wetted wall, allowing the mixed liquid to flow down suitably along the channel wall surface. Note that the action of gravity and the wettability of the substrate (wall material) forming the channel wall surface may be related to allowing the mixed liquid to flow down suitably on the channel wall surface (liquid flow region RL) of the gas-liquid contact channel 23. Therefore, it is preferable to design the channel wall surface as a wetted wall such that the contact angle (θ) between the channel wall surface (substrate) of the gas-liquid contact channel 23 and the mixed liquid (liquid) is less than 90°.

[0029] In the present embodiment, the liquid film thickness of the mixed liquid flowing down along the liquid flow region RL in the gas-liquid contact flow channel 23 may be on the order of micrometers (scale). For example, the liquid film thickness may be 10 μm or more and 1000 μm or less, preferably 50 μm or more and 800 μm or less, and more preferably 100 μm or more and 600 μm or less. This makes it possible to suitably prevent the cross section of the gas-liquid contact flow channel 23 from being blocked by the mixed liquid flowing down along the liquid flow region RL of the gas-liquid contact flow channel 23. Furthermore, by causing the mixed liquid to flow down along the multiple different flow channel walls 231, 232 that form the gas-liquid contact flow channel 23 as described above, it is possible to suitably prevent the cross section of the gas-liquid contact flow channel 23 from being blocked by the mixed liquid while ensuring the total flow rate of the mixed liquid flowing down along the liquid flow region RL. From the above viewpoint, the shape of the cross section of the gas-liquid contact channel 23 is not particularly limited, but may be, for example, a square, in which case the length of each side of the square (corresponding to the channel width) is 0.1 mm or more and 5 mm or less, preferably 0.2 mm or more and 4 mm or less, and more preferably 0.5 mm or more and 3 mm or less. By doing so, the total flow rate of the mixed liquid flowing down along the liquid flow region RL can be ensured, while the cross section of the gas-liquid contact channel 23 can be suitably prevented from being blocked by the mixed liquid.

[0030] Furthermore, the distillation unit 2 according to this embodiment is provided with a temperature adjustment mechanism 3 for forming a predetermined temperature gradient in which the temperature gradually decreases from the second end 23B toward the first end 23A of the gas-liquid contact channel 23. Fig. 5 is a diagram illustrating the temperature adjustment mechanism 3. The temperature adjustment mechanism 3 includes a temperature adjustment heater and a heat conduction member for conducting heat from the temperature adjustment heater.

[0031] In the example shown in Figure 5, a first heat conduction member 31 and a second heat conduction member 32 are attached to the front of the distillation unit 2, and a third heat conduction member 33 and a fourth heat conduction member 34 are attached to the back of the distillation unit 2. Each of the heat conduction members 31 to 34 has a plate shape and is made of a thermal conductor such as a copper plate. In the example shown in Figure 5, each of the heat conduction members 31 to 34 has the same shape, but this is not limited to this. Of course, the heat conduction members 31 to 34 may also be made of other metals with excellent thermal conductivity.

[0032] On the front side of the distillation unit 2, a gap (visualization slit) SL extending in the vertical direction is formed between the first heat conduction member 31 and the second heat conduction member 32, and the gas-liquid contact flow path 23 can be seen through this gap SL. The same applies to the arrangement of the third heat conduction member 33 and the fourth heat conduction member 34 arranged on the back side of the distillation unit 2. That is, a gap (visualization slit) SL extending in the vertical direction is formed between the third heat conduction member 33 and the fourth heat conduction member 34, and the gas-liquid contact flow path 23 can be seen through this gap SL.

[0033] For example, as shown in FIG. 5 , each heat-conducting member 31-34 extends in the vertical direction of the distillation unit 2 so as to cover a height from the first end 23A of the gas-liquid contact flow path 23 to the height corresponding to the second end 23B. Reference numeral 35 in FIG. 5 denotes a temperature control heater. The temperature control heater 35 is, for example, a film heater, and is attached to the lower region of each heat-conducting member 31-34. When the temperature control heater 35 attached to each heat-conducting member 31-34 is activated, heat is transmitted to the gas-liquid contact flow path 23 in the distillation unit 2 through each heat-conducting member 31-34. At this time, the heat of the temperature control heater 35 is more easily transmitted the closer the distance from the temperature control heater 35 is, and is less easily transmitted the farther the distance from the temperature control heater 35 is. As a result, an appropriate temperature gradient (temperature distribution) is generated along the extension direction (longitudinal direction) of the gas-liquid contact flow path 23, and more specifically, it is possible to form a predetermined temperature gradient (temperature distribution) in which the temperature gradually decreases from the second end 23B side toward the first end 23A side of the gas-liquid contact flow path 23. The set temperature of the temperature adjustment heater 35 depends on the boiling points of the components contained in the mixed liquid, but can be set to 30°C or more and 400°C or less, preferably 40°C or more and 350°C or less, and more preferably 50°C or more and 300°C or less.

[0034] [First Circulation Unit] Next, the first circulation unit 5 in the micro-distillation device 1 will be described with reference to Figure 1. The first circulation unit 5 is a unit for circulating the condensed liquid obtained by condensing the vapor derived from the mixed liquid discharged from the vapor outlet 25 of the distillation unit 2 back to the liquid inlet 21 of the distillation unit 2.

[0035] The first circulation unit 5 is configured to include a first circulation conduit 50, a first storage tank 51, a first circulation pump 52, a distributor 54, etc. The first circulation conduit 50 includes a return pipe 55 and a forward pipe 56. The return pipe 55 condenses the vapor derived from the mixed liquid discharged from the vapor outlet 25 of the distillation unit 2 during the transfer process, and transfers the resulting condensate to the first storage tank 51. For example, one end of the return pipe 55 is connected to the vapor outlet 25 of the distillation unit 2 via a fitting FT, and the other end is connected to the first storage tank 51. The vapor derived from the mixed liquid discharged from the vapor outlet 25 of the distillation unit 2 is cooled and condensed while flowing through the return pipe 55. The mixed liquid (condensate) that has changed phase from gas phase to liquid phase while flowing through the return pipe 55 is stored in the first storage tank 51. The joint FT is a one-touch joint such as a tube fitting, and connects the steam outlet 25 of the distillation unit 2 and the return pipe 55 in an airtight manner.

[0036] The supply pipe 56 is a pipe for transferring (supplying) the mixed liquid (condensate) stored in the first storage tank 51 to the liquid inlet 21 of the distillation unit 2. Here, the distillation unit 2 in this embodiment has two liquid inlets 21 (first liquid inlet 21A and second liquid inlet 21B). Therefore, a distributor 54 is disposed midway along the supply pipe 56, and a configuration is adopted in which the supply pipe 56 is branched into two branch pipes.

[0037] The section of the supply pipe 56 that starts at the first storage tank 51 and reaches the distributor 54 is called the main pipe 56A, and the two branch pipes that branch off from the main pipe 56A via the distributor 54 are called the first branch pipe 56B and the second branch pipe 56C, respectively. One end of the first branch pipe 56B is connected to the distributor 54, and the other end is connected to the first liquid inlet 21A of the distillation unit 2. One end of the second branch pipe 56C is connected to the distributor 54, and the other end is connected to the second liquid inlet 21B of the distillation unit 2. The distributor 54 may be made of borosilicate glass, which is resistant to organic chemicals and heat-resistant.

[0038] A first circulation pump 52 is connected to the main pipe 56A of the supply pipe 56. When the first circulation pump 52 is operated, the mixed liquid (condensate) LqA stored in the first storage tank 51 is pumped (e.g., sent) to the supply pipe 56 (main pipe 56A), and the mixed liquid (condensate) LqA flows through the supply pipe 56 from upstream to downstream. That is, the mixed liquid (condensate) LqA sent by the first circulation pump 52 is supplied to the distillation unit 2 through the supply pipe 56. At this time, the mixed liquid (condensate) LqA is introduced into the first liquid inlet 21A through the first branch pipe 56B of the supply pipe 56 and into the second liquid inlet 21B through the second branch pipe 56C. The type of the first circulation pump 52 is not particularly limited, and examples thereof include a syringe pump and a diaphragm pump.

[0039] The return pipe 55 and the supply pipe 56 of the first circulation conduit 50 may be, for example, thin-diameter flexible tubes. For example, a PEEK tube made of PEEK (polyether ether ketone) resin, which is a material resistant to organic chemicals, can be suitably used. The inner diameter of the first circulation conduit 50 (PEEK tube) may be on the order of micrometers (scale), for example, 60 μm to 1000 μm, preferably 80 μm to 700 μm, and more preferably 100 μm to 500 μm. In particular, by making the inner diameter of the return pipe 55 on the order of micrometers as in the above embodiment, the heat transfer area for the vapor discharged from the vapor outlet 25 of the distillation unit 2 can be increased. As a result, the vapor discharged from the vapor outlet 25 can be condensed solely by the cooling effect of the outside air temperature, without using a condenser or a special refrigerant for condensing the vapor.

[0040] [Second Circulation Unit] Next, the second circulation unit 6 in the micro-distillation device 1 will be described with reference to Figure 1. The second circulation unit 6 is a unit for evaporating the mixed liquid discharged from the distillation unit 2, thereby circulating the vapor of the mixed liquid back to the vapor inlet 22 of the distillation unit 2.

[0041] The second circulation unit 6 includes a second circulation conduit 60, a second storage tank 61, a second circulation pump 62, an evaporation unit 70, etc. The second circulation conduit 60 includes a return pipe 65 and a supply pipe 66.

[0042] The return pipe 65 is a pipe for transferring the mixed liquid discharged from the liquid outlet 24 of the distillation unit 2 to the second storage tank 61. The distillation unit 2 in this embodiment has two liquid outlets 24 (a first liquid outlet 24A and a second liquid outlet 24B). Therefore, the return pipe 65 is configured to include a first branch pipe 65A and a second branch pipe 65B, and transfers the mixed liquid discharged from each liquid outlet 24A, 24B to the second storage tank 61. The first branch pipe 65A of the return pipe 65 is liquid-tightly connected to the first liquid outlet 24A of the distillation unit 2 via a joint FT. The second branch pipe 65B is liquid-tightly connected to the second liquid outlet 24B of the distillation unit 2 via a joint FT. The mixed liquid transferred from the liquid outlet 24 of the distillation unit 2 by the return pipe 65 is stored in the second storage tank 61.

[0043] The supply piping 66 is composed of a liquid supply piping 66A that transfers the mixed liquid stored in the second storage tank 61 to the evaporation unit 70, and an air supply piping 66B that transfers steam derived from the mixed liquid generated by the evaporation unit 70 to the steam inlet 22 of the distillation unit 2.

[0044] A second circulation pump 62 is connected to the liquid supply pipe 66A in the feed pipe 66. When the second circulation pump 62 is activated, the mixed liquid LqB stored in the second storage tank 61 is pressure-fed (e.g., pumped) to the liquid supply pipe 66A, and the mixed liquid LqB is transferred through the liquid supply pipe 66A to the evaporation unit 70. The type of the second circulation pump 62 is not particularly limited, and examples thereof include a syringe pump and a diaphragm pump.

[0045] The evaporation unit 70 is formed, for example, as a chip-type microfluidic device in which micrometer-scale microchannels 71 are formed on a substrate 72. The shape of the substrate 72 in the evaporation unit 70 is not particularly limited, and may be, for example, a chip-type device with a rectangular plane. The substrate 72 in the evaporation unit 70 may be made of borosilicate glass, which is resistant to organic chemicals and heat-resistant. A plurality of linear microchannels 71 are arranged in parallel on the substrate 72 of the evaporation unit 70. The upstream and downstream ends of each microchannel 71 merge at an upstream junction 73 and a downstream junction 74. The substrate 72 of the evaporation unit 70 is formed with a liquid inlet 75 communicating with the upstream junction 73 and a vapor outlet 76 communicating with the downstream junction 74. The number and arrangement of the microchannels 71 in the evaporation unit 70 are not particularly limited. For example, the evaporation unit 70 may have microchannels 71 extending in a serpentine shape.

[0046] The channel width of the microchannel 71 in the evaporation unit 70 can be 60 μm or more and 1000 μm or less, preferably 80 μm or more and 700 μm or less, and more preferably 100 μm or more and 500 μm or less. The channel height of the microchannel 71 can be 60 μm or more and 1000 μm or less, preferably 80 μm or more and 700 μm or less, and more preferably 100 μm or more and 500 μm or less. The channel length of the microchannel 71 can be 1 mm or more and 1000 mm or less, preferably 5 mm or more and 500 mm or less, and more preferably 10 mm or more and 100 mm or less.

[0047] A liquid supply pipe 66A is liquid-tightly connected to a liquid inlet 75 of the evaporation unit 70 via a joint FT. One end of an air supply pipe 66B is airtightly connected to a steam outlet 76 of the evaporation unit 70 via a joint FT. The other end of the air supply pipe 66B is airtightly connected to the steam inlet 22 of the distillation unit 2 via a joint FT. The evaporation unit 70 configured as described above introduces the mixed liquid LqB supplied through the liquid supply pipe 66A from the liquid inlet 75, and distributes the mixed liquid LqB to each microchannel 71 via the upstream junction 73.

[0048] The evaporation unit 70 includes an evaporation heater 77 for heating and evaporating the mixed liquid LqB flowing along each microchannel 71 (see FIG. 1 ). The evaporation heater 77 may be any heater capable of evaporating the mixed liquid LqB flowing through each microchannel 71, but may also be a planar heater provided on a substrate so as to cover the upper or lower surface of each microchannel 71. In this manner, the mixed liquid LqB flowing into each microchannel 71 of the evaporation unit 70 evaporates as it flows through each microchannel 71. The vapor derived from the mixed liquid generated in each microchannel 71 merges at a downstream junction 74 and is discharged from a vapor outlet 76 to the air supply pipe 66B. The evaporation unit 70 allows the mixed liquid flowing through the microchannel 71 to be suitably evaporated by heating the mixed liquid with the heater. The set temperature of the evaporation heater 77 can be set to be higher than the boiling point of the lowest boiling point component contained in the mixed liquid LqB, for example, 30°C or higher and 400°C or lower, with 40°C or higher and 350°C or lower being preferred, and 50°C or higher and 300°C or lower being more preferred.

[0049] The vapor derived from the mixed liquid discharged into the air supply pipe 66B is supplied to the vapor inlet 22 of the distillation unit 2 through the air supply pipe 66B. Here, the air supply pipe 66B preferably has a heat-insulating function that can keep the vapor derived from the mixed liquid flowing therethrough warm and prevent condensation during transfer. Alternatively, the second circulation unit 6 may be provided with a heat-insulating member 67 for keeping the air supply pipe 66B warm (see FIG. 1 ). The heat-insulating member 67 is not particularly limited as long as it is a member that can prevent re-condensation of the vapor transferred by the air supply pipe 66B by keeping the air supply pipe 66B warm.

[0050] The micro-distillation device 1 is controlled by a control device 100 (see Figure 1) which controls the temperature control heater 35 in the distillation unit 2, the first circulation pump 52 in the first circulation unit 5, the second circulation pump 62 in the second circulation unit 6, the evaporation heater 77, etc.

[0051] The control device 100 may be a general-purpose computer. The control device 100 includes a communication interface (I / F), a storage device, an input / output device, a processor, and the like. The communication I / F may be, for example, a network card or a communication module, and communicates with other computers based on a predetermined protocol. The storage device may be a main storage device such as a random access memory (RAM) or a read-only memory (ROM), or an auxiliary storage device (secondary storage device) such as a hard-disk drive (HDD), a solid-state drive (SSD), or a flash memory. The main storage device temporarily stores programs read by the processor and information exchanged with other computers, and secures a working area for the processor. The auxiliary storage device stores programs executed by the processor and information exchanged with other computers. The input / output device is, for example, a user interface such as an input device (e.g., a keyboard or a mouse), an output device (e.g., a monitor), or an input / output device (e.g., a touch panel). The processor is an arithmetic processing device such as a central processing unit (CPU) that executes programs. It should be noted that the various devices of the micro-distillation device 1 do not necessarily need to be controlled by the control device 100, and in that respect the control device 100 is an optional element.

[0052] In the micro-distillation device 1 configured as described above, in a preparation step prior to the start of operation (operation), the mixed liquids LqA and LqB to be distilled are stored in the first storage tank 51 and the second storage tank 61. Note that although the mixed liquids are denoted here using different symbols "LqA, LqB," this is to distinguish between the locations where the mixed liquids are stored, and it goes without saying that the mixed liquids LqA and LqB may have the same composition.

[0053] Next, we will explain the operating status (driving status) of the micro-distillation device 1. The operation (driving status) of the micro-distillation device 1 is performed by the control device 100 controlling the operation of various components of the micro-distillation device 1 (first circulation pump 52, second circulation pump 62, temperature control heater 35, and evaporation heater 77).

[0054] The micro-distillation device 1 separates a specific target component from other components by performing a distillation operation on a mixed liquid containing at least two components with different boiling points.

[0055] When the micro-distillation device 1 is activated, the mixed liquids LqA and LqB stored in the first storage tank 51 in the first circulation unit 5 are transferred to the liquid inlet 21 of the distillation unit 2 through the forward piping 56 in the first circulation unit 5.

[0056] Furthermore, the mixed liquid LqB stored in the second storage tank 61 in the second circulation unit 6 is transferred to the evaporation unit 70 through the liquid transfer pipe 66A. The mixed liquid LqB transferred to the evaporation unit 70 is heated by the evaporation heater 77 while flowing through each microchannel 71, and is thereby evaporated, becoming vapor derived from the mixed liquid. The vapor derived from the mixed liquid generated by the evaporation unit 70 is transferred, while being kept warm, to the vapor inlet 22 of the distillation unit 2 through the gas transfer pipe 66B.

[0057] The mixed liquid LqA introduced from the first liquid inlet 21A and the second liquid inlet 21B in the distillation unit 2 is guided through the first liquid inlet channel 26A and the second liquid inlet channel 26B, respectively, to the first end 23A side of the gas-liquid contact channel 23. Then, this mixed liquid flows along the liquid flow region RL formed on the channel wall surface of the gas-liquid contact channel 23, and flows downward toward the second end 23B of the gas-liquid contact channel 23 located vertically below.

[0058] More specifically, the mixed liquid LqA introduced from the first liquid inlet 21A is guided through the first liquid introduction path 26A to the first flow path wall surface 231 at the first end 23A of the gas-liquid contact flow path 23. Furthermore, the mixed liquid LqA introduced from the second liquid inlet 21B is guided through the second liquid introduction path 26B to the second flow path wall surface 232 at the first end 23A of the gas-liquid contact flow path 23. As described above, when the distillation unit 2 is in use, the first end 23A side of the gas-liquid contact flow path 23 is disposed vertically upward (facing upward), and the second end 23B side is disposed vertically downward (facing downward). Therefore, the mixed liquid LqA guided to the first flow path wall surface 231 and the second flow path wall surface 232 can be caused to flow vertically downward along the surfaces of these flow path wall surfaces 231, 232 by gravity.

[0059] In this embodiment, the cross-sectional area of ​​the gas-liquid contact channel 23 is determined so that the mixed liquid LqA flowing through the gas-liquid contact channel 23 does not block the entire cross section of the channel 23; in other words, so that a hollow vapor flow region RG remains at the center of the cross section of the gas-liquid contact channel 23. In one aspect, the liquid inlet channel 26 and the liquid outlet channel 27 in the distillation unit 2 are designed to have a channel width of approximately 400 μm and a channel height of approximately 2000 μm. The liquid film thickness TH1 (see FIG. 4 ) of the mixed liquid flowing down along each channel wall surface 231, 232 in the gas-liquid contact channel 23 is designed to be, for example, several tens of μm to several hundreds of μm, thereby ensuring excellent discharge of the mixed liquid. Under such design conditions, in order to ensure a sufficient vapor flow region RG for flowing the vapor as a countercurrent in the vertically upward direction opposite to the flow direction of the mixed liquid, it is possible to suitably adopt, for example, an embodiment in which the cross section of the gas-liquid contact flow path 23 is a square with one side measuring 2 mm.

[0060] On the other hand, the vapor derived from the mixed liquid transferred to the vapor inlet 22 of the distillation unit 2 by the second circulation unit 6 flows through the vapor inlet path 28 into the gas-liquid contact flow path 23 from the second end 23B side located on the vertically lower side. The vapor derived from the mixed liquid that has flowed into the gas-liquid contact flow path 23 flows along the gas-liquid contact flow path 23 toward the first end 23A side of the gas-liquid contact flow path 23 (i.e., vertically upward). In other words, the vapor derived from the mixed liquid supplied to the distillation unit 2 by the second circulation unit 6 flows through the gas-liquid contact flow path 23 as a counterflow opposite to the mixed liquid LqA supplied to the distillation unit 2 by the first circulation unit 5.

[0061] As described above, gravity is utilized to cause gas-liquid countercurrent contact between the mixed liquid LqA and the vapor derived from the mixed liquid in the gas-liquid contact flow path 23, thereby enabling efficient heat exchange and mass transfer between the mixed liquid LqA and the vapor derived from the mixed liquid. Furthermore, as described above, the distillation unit 2 is equipped with a temperature control mechanism 3 for forming a predetermined temperature gradient in which the temperature gradually decreases from the second end 23B side toward the first end 23A side of the gas-liquid contact flow path 23. The control device 100 controls the temperature control heater 35 in the temperature control mechanism 3, thereby forming an appropriate temperature distribution in which the temperature gradually decreases from the second end 23B (lower end) side toward the first end 23A (upper end) side of the gas-liquid contact flow path 23. For example, the temperature of the gas-liquid contact flow path 23 may be controlled to remain in a temperature range higher than the boiling point of the target component to be separated in the distillation operation and lower than the boiling points of the other components.

[0062] As a result, the vapor derived from the mixed liquid flowing through the vapor flow region RG of the gas-liquid contact flow channel 23 from the second end 23B side toward the first end 23A side (vertically upward) is gradually cooled, and other components having a boiling point higher than that of the target component contained in the vapor derived from the mixed liquid are condensed. The condensed other components flow downward along the liquid flow region RL (flow channel walls 231, 232) together with the mixed liquid LqA flowing from the first end 23A side of the gas-liquid contact flow channel 23. Meanwhile, the target component contained in the vapor derived from the mixed liquid is discharged from the vapor outlet 25 through the vapor discharge channel 29 while maintained in the vapor phase.

[0063] Furthermore, the temperature of the mixed liquid LqA flowing down along the liquid flow region RL (flow path wall surfaces 231, 232) of the gas-liquid contact flow path 23 gradually increases as it approaches the second end 23B of the gas-liquid contact flow path 23, and in this process, the target component contained in the mixed liquid LqA undergoes a phase change to vapor. In this manner, the vapor of the target component flows through the vapor flow region RG and is discharged from the vapor outlet 25 via the vapor discharge path 29. Furthermore, other components of the mixed liquid LqA flowing down the liquid flow region RL (flow path wall surfaces 231, 232) that have higher boiling points than the target component are concentrated and reach the second end 23B of the gas-liquid contact flow path 23, where they are discharged from the liquid outlets 24 (first liquid outlet 24A, second liquid outlet 24B) via the liquid discharge path 27.

[0064] The vapor derived from the mixed liquid discharged from the vapor outlet 25 of the distillation unit 2 (vapor in which the target component is concentrated) is cooled and condensed while flowing through the return pipe 55 of the first circulation unit 5. The condensate thus obtained is stored in the first storage tank 51. That is, the condensate transferred through the return pipe 55 of the first circulation unit 5 is mixed with the mixed liquid LqA stored in the first storage tank 51, and then circulated again to the liquid inlet 21 of the distillation unit 2 through the feed pipe 56.

[0065] Furthermore, the mixed liquid discharged from the liquid outlet 24 of the distillation unit 2 (a mixed liquid in which components other than the target component are concentrated) is stored in the second storage tank 61 through the return pipe 65 of the second circulation unit 6. That is, the mixed liquid discharged from the liquid outlet 24 of the distillation unit 2 (a mixed liquid in which components other than the target component are concentrated) is mixed with the mixed liquid LqB stored in the second storage tank 61, and then transferred to the evaporation unit 70 through the liquid delivery pipe 66A, where it is converted into vapor and then circulated again to the vapor inlet 22 of the distillation unit 2.

[0066] In its steady-state operation, the micro-distillation device 1 continuously (continuously) circulates using the first circulation unit 5 and the second circulation unit 6. As a result, a mixed liquid in which the target component is concentrated can be stored in the first storage tank 51 (which can also be referred to as a reflux tank) of the micro-distillation device 1. That is, the mixed liquid in which the target component is concentrated can be suitably recovered from the first storage tank 51 (reflux tank). Furthermore, the second storage tank 61 (which can also be referred to as a bottom tank) can store a mixed liquid in which components other than the target component are concentrated. Therefore, the mixed liquid in which components other than the target component are concentrated can be suitably recovered from the second storage tank 61 (bottom tank). Here, the higher the concentration of the target component in the mixed liquid recovered from the first storage tank 51 and the lower the concentration of the target component (the higher the concentration of components other than the target component) in the mixed liquid recovered from the second storage tank 61, the more efficient the separation operation by distillation using the micro-distillation device 1. Furthermore, the micro-distillation device 1 according to this embodiment realizes countercurrent gas-liquid contact utilizing gravity in the gas-liquid contact channel 23, thereby efficiently bringing the vapor rising vertically upward in the vapor flow region RG into contact with the mixed liquid flowing vertically downward in the liquid flow region RL using the channel walls 231, 232 as wetted walls, thereby facilitating heat and mass transfer between the gas and liquid. As a result, it becomes possible to efficiently separate the target component from other components contained in the mixed fluid (mixed liquid and vapor).

[0067] The micro-distillation device 1 continuously circulates the mixed liquid in which the target component has been concentrated by the first circulation unit 5 to the distillation unit 2. The second circulation unit 6 also continuously circulates the mixed liquid in which components other than the target component have been concentrated to the distillation unit 2. The micro-distillation device 1 is capable of continuous distillation using these two circulation units 5, 6. In other words, the mixed liquid in which the target component has been concentrated and the vapor obtained by evaporating the mixed liquid in which the other components have been concentrated are continuously and repeatedly circulated to the distillation unit 2 and brought into gas-liquid contact in the gas-liquid contact flow path 23, thereby enhancing the degree of separation between the target component and the other components contained in the mixed fluid (mixed liquid and vapor).

[0068] Furthermore, the distillation unit 2 according to this embodiment has a plurality of liquid inlets 21A, 21B as described above. The mixed liquid can be introduced into the liquid flow region RL of the gas-liquid contact flow channel 23 via a plurality of liquid inlet channels 26A, 26B corresponding to the liquid inlets 21A, 21B. This makes it possible to suitably ensure the flow rate of the mixed liquid in the gas-liquid contact flow channel 23. In this case, by configuring the mixed liquid introduced from each of the liquid inlet channels 26A, 26B to be introduced into different flow channel wall surfaces 231, 232 that form the gas-liquid contact flow channel 23, it is possible to ensure the flow rate of the mixed liquid while suppressing the obstruction of the flow of steam in the vapor flow region RG of the gas-liquid contact flow channel 23.

[0069] Furthermore, in the distillation unit 2, the liquid inlet channel 26 is formed as a microchannel, so that the mixed liquid can be supplied at an appropriate flow rate to the gas-liquid contact channel 23 through the liquid inlet channel 26. As a result, it is easy to control the liquid film thickness of the mixed liquid flowing down along the channel wall surfaces 231, 232 (liquid flow region RL) in the gas-liquid contact channel 23 to the micrometer scale. Furthermore, in the distillation unit 2, the liquid outlet channel 27 is formed as a microchannel, so that the channel for discharging the mixed liquid flowing down the channel wall surfaces 231, 232 (liquid flow region RL) with a liquid film thickness on the micrometer scale can be made to an appropriate size.

[0070] The distillation unit 2 also includes a temperature control mechanism 3 including a temperature control heater 35 and heat conduction members 31-34 for conducting heat from the temperature control heater 35 to the substrate B. This allows a predetermined temperature gradient (temperature distribution) to be formed in the gas-liquid contact flow path 23, in which the temperature gradually decreases from the second end 23B (lower end) of the gas-liquid contact flow path 23 toward the first end 23A (upper end) of the gas-liquid contact flow path 23. This allows an appropriate thermal environment to be formed in the gas-liquid contact flow path 23, even under conditions where the thermal environment of the gas-liquid contact flow path 23 is easily affected by the outside air temperature due to the small volume of the gas-liquid contact flow path 23 in the distillation unit 2, thereby enabling the distillation operation to be performed suitably. More specifically, separation of low-boiling-point components and high-boiling-point components by gas-liquid countercurrent contact can be suitably performed without completely condensing the vapor flowing through the vapor flow region RG in the gas-liquid contact flow path 23. In this embodiment, it is preferable to use the temperature adjustment mechanism 3 to control the temperature so that the temperature at each point set in advance along the axial direction (extension direction) of the gas-liquid contact flow path 23 becomes a predetermined temperature.

[0071] Furthermore, conventional distillation columns have complex structures, which can make it difficult to check the internal flow conditions and check for malfunctions (such as drift in the packed column, blockage by polymers, flooding, weeping, etc.). In contrast, the temperature control mechanism 3 according to this embodiment has vertically extending gaps (visualization slits) SL formed between the first heat conduction member 31 and the second heat conduction member 32, and between the third heat conduction member 33 and the fourth heat conduction member 34. This makes it possible to visually check the status of the gas-liquid contact flow path 23 in real time through the gaps SL, even during operation of the micro-distillation device 1, and visualize the flow rates of the mixed liquid and vapor flowing through the gas-liquid contact flow path 23.

[0072] The operating time (driving time) of the micro-distillation device 1 is not particularly limited and can be set freely.

[0073] Furthermore, in the microdistillation device 1, the container capacities of the first storage tank 51 and the second storage tank 61 are such that if the container capacities are too large, it will take a long time for the concentration of the mixed solution stored in each tank 51, 61 to stabilize (reach the final state), while if the container capacities are too small, it may be difficult to achieve stable continuous operation. From these perspectives, it is preferable to design the container capacities of the first storage tank 51 and the second storage tank 61. For example, the capacity of the first storage tank 51 may be 30 μL or more and 3000 μL or less, preferably 40 μL or more and 2000 μL or less, and more preferably 50 μL or more and 1000 μL or less. The capacity of the second storage tank 61 can be 30 μL or more and 3000 μL or less, preferably 40 μL or more and 2000 μL or less, and more preferably 50 μL or more and 1000 μL or less.

[0074] Furthermore, regarding the amount of the mixed liquid delivered by the first circulation pump 52 and the second circulation pump 62, if the amount is too small, it may take a long time for the concentration of the mixed liquid stored in each storage tank 51, 61 to reach its final state. Furthermore, the amount of liquid delivered by the first circulation pump 52 and the second circulation pump 62 should be determined so that the liquid levels in each storage tank 51, 61 remain stable and do not change significantly during operation of the micro-distillation device 1. Furthermore, if the amount of liquid delivered by the second circulation pump 62 is too large (if the liquid delivery rate is too fast), the vaporization and evaporation capacity of the mixed liquid in the evaporation unit 70 may be exceeded, and the liquid may be introduced into the vapor inlet 22 of the distillation unit 2. It is preferable to design the amount of liquid delivered by the first circulation pump 52 and the second circulation pump 62 taking these points into consideration. For example, the flow rate of the mixed solution delivered by the first circulation pump 52 may be 5 μL / min or more and 1000 μL / min or less, preferably 8 μL / min or more and 500 μL / min or less, and more preferably 10 μL / min or more and 300 μL / min or less. The flow rate of the mixed solution delivered by the second circulation pump 62 may be 5 μL / min or more and 1000 μL / min or less, preferably 8 μL / min or more and 500 μL / min or less, and more preferably 10 μL / min or more and 300 μL / min or less.

[0075] Although the microdistillation device 1 according to this embodiment is capable of distilling (rectifying) a mixture of three or more components with different boiling points, this embodiment describes a distillation operation for a mixture of two components (a low-boiling component and a high-boiling component). In this case, the vapor derived from the mixture containing the low-boiling component and the high-boiling component supplied to the distillation unit 2 by the second circulation unit 6 flows through the vapor flow region RG of the gas-liquid contact flow channel 23 from the second end 23B toward the first end 23A (vertically upward), condensing the high-boiling component. The condensed liquid of the high-boiling component flows down the liquid flow region RL (channel walls 231, 232) together with the mixture flowing from the first end 23A of the gas-liquid contact flow channel 23 and is finally discharged from the liquid outlet 24. The vapor, with an increased concentration of the low-boiling component due to separation from the high-boiling component, is discharged from the vapor outlet 25 via the vapor outlet 29.

[0076] Furthermore, the mixed liquid containing low-boiling-point and high-boiling-point components supplied to the distillation unit 2 by the first circulation unit 5 undergoes a phase change in which the low-boiling-point components change into vapor as they flow down the liquid flow region RL (flow path wall surfaces 231, 232) of the gas-liquid contact flow path 23. This vapor of the low-boiling-point components is discharged from the vapor outlet 25 through the vapor discharge path 29 together with the vapor flowing upward through the vapor flow region RG. On the other hand, the high-boiling-point components contained in the mixed liquid supplied to the distillation unit 2 by the first circulation unit 5 are concentrated as they flow down the liquid flow region RL (flow path wall surfaces 231, 232), reach the second end 23B of the gas-liquid contact flow path 23, and are then discharged from the liquid outlet 24 through the liquid discharge path 27. By continuously performing such a distillation operation, a mixture having an increased concentration of low-boiling-point components is stored in the first storage tank 51 (reflux tank), and a mixture having an increased concentration of high-boiling-point components is stored in the second storage tank 61 (bottom tank). In other words, mixtures having increased purities of low-boiling-point components and high-boiling-point components can be stored in the storage tanks 51 and 61 and recovered.

[0077] EXAMPLES The present disclosure will be specifically described below with reference to examples, although the present disclosure is not limited to the aspects of the following examples.

[0078] In the examples, total reflux distillation was performed on a mixed liquid containing acetic acid and ethyl acetate using the micro-distillation device 1 described with reference to Figures 1 to 5. The micro-distillation device 1 was operated (operated) with the distillation unit 2 installed so that the first end 23A of the gas-liquid contact channel 23 in the distillation unit 2 was positioned vertically upward (facing upward) and the second end 23B was positioned vertically downward (facing downward).

[0079] The apparatus used in the examples is as follows:・Circulation pump (liquid delivery pump): Smoothflow Pump Q Model Q1-5-KR-UP-S-IMTT (manufactured by Takumina Corporation) ・Distributor: Standard Tip ICC-SY500 (manufactured by Micro Chemical Engineering Co., Ltd.) ・Circulation conduit: Polyether ether ketone tube (inner diameter 260 μm, manufactured by Micro Chemical Engineering Co., Ltd.) ・First storage tank (reflux tank): Capacity 0.6 mL (manufactured by Nichiden Rika Glass Co., Ltd.) ・Second storage tank (bottle tank): Capacity 0.6 mL (manufactured by Nichiden Rika Glass Co., Ltd.) ・Temperature control heater, evaporation heater: 2 cm x 2 cm type (manufactured by Miyo Technology Co., Ltd.) ・Evaporation heater: IACF-THT03050 (manufactured by TAIYA International Technology Co., Ltd.)

[0080] [Evaporation Unit] The evaporation unit 70 used had ten microchannels 71 arranged in parallel on a substrate 72. Each microchannel 71 had a channel width of 150 μm, a channel height (depth) of 50 μm, and a channel length of 60 mm, and the substrate 72 was made of borosilicate glass.

[0081] [Distillation Unit] Borosilicate glass was used for the substrate B of the distillation unit 2. The distillation unit 2 used a substrate B measuring 30 mm in width and 70 mm in height. The cross section of the gas-liquid contact channel 23 was a square with sides of 2 mm, and the channel length (reference symbol LT in Figure 6) was 50 mm. The liquid inlet channel 26 and the liquid outlet channel 27 were formed as microchannels with a channel width of 400 μm and a channel height (depth) of 2000 μm (2 mm). The liquid film thickness of the mixed liquid flowing down the channel wall surface of the gas-liquid contact channel 23 was adjusted to be in the range of several tens to several hundreds of μm.

[0082] [Operation and Distillation Conditions] Specific operation and distillation conditions in the examples are shown in Table 1. As a preparation step before starting the distillation operation using the micro-distillation device 1, a mixed liquid was placed in the first storage tank 51 (reflux tank) and the second storage tank 61 (bottom tank). The first storage tank 51 (reflux tank) contained 100 μL of a mixed liquid of acetic acid and ethyl acetate, in which ethyl acetate was mixed so that the acetic acid concentration was 30.0% by mass. The second storage tank 61 (bottom tank) contained 100 μL of a mixed liquid of acetic acid and ethyl acetate, in which ethyl acetate was mixed so that the acetic acid concentration was 30.0% by mass. Note that acetic acid and ethyl acetate manufactured by Honeywell Corporation were used in the examples.

[0083] In the distillation operation of the example, the first circulation pump 52, the second circulation pump 62, the temperature control heater 35, and the evaporation heater 77 in the micro-distillation device 1 were operated, and each mixed liquid stored in the first storage tank 51 (reflux tank) and the second storage tank 61 (bottom tank) was sent to the distillation unit 2 at the flow rates shown in Table 1, and the operation of the micro-distillation device 1 was stopped after the operating time (experimental time) shown in Table 1 had elapsed since the start of operation.

[0084] Table 1 shows the results of measuring the temperatures at temperature measurement points T1 to T5 of the gas-liquid contact flow channel 23 in the distillation unit 2 during operation of the micro-distillation device 1 (specifically, the surface temperatures of the substrate (glass) at each of the temperature measurement points T1 to T5). FIG. 6 is a diagram illustrating the temperature measurement points T1 to T5. The temperature measurement points T1 to T5 are set at intervals along the axial direction of the gas-liquid contact flow channel 23. The temperature measurement points T1 to T5 are set on the axis of the gas-liquid contact flow channel 23. The temperature measurement point T1 is located at the first end 23A (upper end) of the gas-liquid contact flow channel 23, i.e., at the point where the gas-liquid contact flow channel 23 merges with the liquid inlet channel 26 (26A, 26B). The temperature measurement point T5 is located at the second end 23B (lower end) of the gas-liquid contact flow channel 23, i.e., at the point where the gas-liquid contact flow channel 23 branches off from the liquid outlet channel 27 (27A, 27B). The temperature measurement point T3 is a measurement point set exactly midway between the temperature measurement points T1 and T5 on the axis of the gas-liquid contact flow path 23. The temperature measurement point T2 is a measurement point set between the temperature measurement points T1 and T3, and is set 10 mm away from the temperature measurement point T1 toward the T3 side. The temperature measurement point T4 is a measurement point set between the temperature measurement points T5 and T3, and is set 10 mm away from the temperature measurement point T5 toward the T3 side. The symbols L1 to L4 in FIG. 6 indicate the distance between each temperature measurement point along the axial direction of the gas-liquid contact flow path 23. In the example, L1 and L4 are set to 10 mm, and L2 and L3 are set to 15 mm. The sum of L1 to L4 is represented by the symbol LT, and its length of 50 mm is equal to the total length of the gas-liquid contact flow path 23.

[0085] Distillation operations were carried out for each of Examples 1 to 3 under different distillation conditions, and the ethyl acetate concentration and acetic acid concentration of the mixture recovered in the first storage tank 51 (reflux tank), the ethyl acetate concentration and acetic acid concentration of the mixture recovered in the second storage tank 61 (bottom tank), the number of theoretical plates, and the height equivalent of one theoretical plate (HETP) were determined. The results for each Example are shown in Table 2.

[0086] The methods for measuring the acetic acid concentration and ethyl acetate concentration in the reflux liquid and bottoms obtained in each example are as follows. [Method for measuring acetic acid concentration] The acetic acid concentration was measured by titration analysis using a 0.05 mol / L aqueous sodium hydroxide solution, and calculated from the neutralization point due to pH change. The measurement conditions were as follows: Titration reagent: 0.05 mol / L aqueous sodium hydroxide solution (manufactured by Honeywell Corporation) Measuring instrument: pH meter Model PB-10 (manufactured by Sartorius Corporation) Measurement temperature: 25°C (room temperature) [Method for measuring ethyl acetate concentration] The ethyl acetate concentration was calculated as the difference between 100% by mass and the acetic acid concentration.

[0087]

[0088]

[0089] [Comparative Example] Next, a comparative example will be described. In the comparative example, total reflux distillation of acetic acid (99.7 wt %; Fujifilm Wako Pure Chemical Industries, Ltd.) and ethyl acetate (99.9 GC area %; Daicel Corporation) was carried out using an experimental apparatus using a flask as shown in Fig. 7 .

[0090] The equipment used in the comparative example is as follows: Flask, capacity 3 L (manufactured by Asahi Seisakusho Co., Ltd.) Packed tower (manufactured by Asahi Seisakusho Co., Ltd.) Condenser (manufactured by Asahi Seisakusho Co., Ltd.)

[0091] The flask used in the distillation operation according to the comparative example was connected to a packed tower located at the top. The packed tower had structured packing (Sulzer EX laboratory packing, inner diameter 50 mm, packing length 55 mm; Sulzer Chemtech Ltd) and a dispersion plate. A gas flow pipe for circulating gas was connected to the top of the packed tower, and a condenser was connected to the top of the gas flow pipe. In the distillation operation according to the comparative example, the flask was heated using an oil bath to vaporize the mixed liquid in the flask, and the gas flowing through the gas flow pipe was condensed by cooling it using a condenser.

[0092] [Operation and Distillation Conditions] Specific operation and distillation conditions for the comparative examples are shown in Table 3. As a preparation step before starting the distillation operation for the comparative examples, a mixed solution containing ethyl acetate was mixed to a concentration of 30.0% by mass of acetic acid, and the resulting mixture was filled into a 2.9 L flask. Then, for Comparative Examples 1 to 3 (see Table 3), which had different distillation conditions, total reflux distillation was performed on the mixed solution of acetic acid and ethyl acetate, and the oil bath temperature was adjusted so that the reflux flow rate was a predetermined flow rate. The reflux solution and the mixed solution in the flask were then sampled, and the ethyl acetate and acetic acid concentrations of the reflux solution, the ethyl acetate and acetic acid concentrations of the mixed solution in the flask, the number of theoretical plates, and the height equivalent to a theoretical plate (HETP) were determined. The results for each comparative example are shown in Table 4.

[0093] The methods for measuring the acetic acid concentration and ethyl acetate concentration in the reflux liquid and the mixed liquid in the flask obtained in each Comparative Example are as follows. The ethyl acetate concentration was calculated as the difference between 100% by mass and the acetic acid concentration.

[0094] [Method for measuring acetic acid concentration in reflux liquid] The acetic acid concentration was measured by titration analysis using a 0.1 mol / L potassium hydroxide aqueous solution (manufactured by FUJIFILM Wako Pure Chemical Industries, Ltd.) and calculated from the neutralization point due to color change. The measurement conditions were as follows: Titration reagent: 0.1 mol / L potassium hydroxide aqueous solution (manufactured by FUJIFILM Wako Pure Chemical Industries, Ltd.) Indicator: 1.0 w / v% phenolphthalein-ethanol (90) solution (FUJIFILM Wako Pure Chemical Industries, Ltd.) Solvent: 99.7 wt% 2-propanol (FUJIFILM Wako Pure Chemical Industries, Ltd.) Measurement temperature: 25°C (room temperature) [Method for measuring acetic acid concentration in the mixed liquid in the flask] The measurement conditions for gas chromatography (GC) were as follows: Apparatus: Gas chromatograph (manufactured by Agilent Technologies Inc.) Detector: Thermal conductivity detector (manufactured by Agilent Technologies Inc.) Column: DB-WAX (column size: length 60 m, inner diameter: 0.53 mm, film thickness: 1.0 μm, manufactured by Agilent Technologies Inc.) Vaporization chamber temperature: 180°C Heating: 100°C, held for 10 minutes → 10°C / min → 200°C, held for 10 minutes Carrier gas: He Split ratio: 20:1 Total flow rate: 87 ml / min Injection volume: 1 μL Internal standard substance: 1,4-dioxane Analysis time: 30 minutes

[0095]

[0096]

[0097] Comparing the results of the Examples (Table 2) and Comparative Examples (Table 4), it can be seen that the Examples have a larger number of theoretical plates than the Comparative Examples. This indicates that the Examples have a higher separation efficiency than the Comparative Examples. Furthermore, the Examples have a smaller height equivalent to a theoretical plate (HETP) than the Comparative Examples, which indicates that the Examples have a higher separation performance than the Comparative Examples.

[0098] <Embodiment 2> Next, embodiment 2 of the micro-distillation device will be described. Figure 8 is a diagram illustrating a micro-distillation device 1A according to embodiment 2. In the micro-distillation device 1A shown in Figure 8, the structure of the distillation unit 2A differs from the distillation unit 2 shown in Figure 1. The following description will focus on the differences between embodiments 1 and 2, and common structures will be denoted by the same reference numerals and will not be described in detail.

[0099] The distillation unit 2A according to the second embodiment further includes an intermediate inlet 80 for introducing an additional mixed liquid into the intermediate position of the gas-liquid contact flow path 23, in addition to the liquid inlet 21 disposed at the first end 23A of the gas-liquid contact flow path 23. In the example shown in FIG. 8, the distillation unit 2A is provided with a first intermediate inlet 80A and a second intermediate inlet 80B. The distillation unit 2A is further provided with an intermediate inlet path 81 connecting the intermediate inlet 80 and the gas-liquid contact flow path 23. In the example shown in FIG. 8, the first intermediate inlet path 81A connects the first intermediate inlet 80A and the gas-liquid contact flow path 23, and the second intermediate inlet path 81B connects the second intermediate inlet 80B and the gas-liquid contact flow path 23. The first intermediate inlet path 81A opens into the first flow path wall surface 231, and the second intermediate inlet path 81B opens into the second flow path wall surface 232.

[0100] As shown in Figure 8, the microdistillation device 1A is equipped with an additional supply unit 90 for supplying an additional mixed liquid to an intermediate position of the gas-liquid contact channel 23. The additional supply unit 90 is configured to include a liquid feed conduit 91, a third storage tank 92, a liquid feed pump 93, a distributor 94, etc. The liquid feed conduit 91 is a pipe for transferring (supplying) the additional mixed liquid stored in the third storage tank 92 to the intermediate inlet 80 of the distillation unit 2A. The type of the liquid feed pump 93 is not particularly limited, and examples include a syringe pump and a diaphragm pump.

[0101] The liquid supply conduit 91 includes a main pipe 91A located between the third storage tank 92 and the distributor 94, and a first branch pipe 91B and a second branch pipe 91C branched from the main pipe 91A via the distributor 94. One end of the first branch pipe 91B is connected to the distributor 94, and the other end is connected to the first intermediate inlet 80A of the distillation unit 2A. One end of the second branch pipe 91C is connected to the distributor 94, and the other end is connected to the second intermediate inlet 80B of the distillation unit 2A.

[0102] A liquid feed pump 93 is connected to the main pipe 91A of the liquid feed conduit 91. When the liquid feed pump 93 is operated, the mixed liquid stored in the third storage tank 92 is pumped (liquid fed) to the main pipe 91A. This mixed liquid is supplied to the first intermediate inlet 80A of the distillation unit 2A through the first branch pipe 91B, and is supplied to the second intermediate inlet 80B of the distillation unit 2A through the second branch pipe 91C.

[0103] 8, the micro-distillation device 1A includes a first mixed liquid discharge unit 200 and a second mixed liquid discharge unit 300. The first mixed liquid discharge unit 200 includes a first liquid supply conduit 210, a first liquid supply pump 220, a first recovery tank 230, and the like. The first liquid supply conduit 210 is a conduit connecting the first storage tank 51 and the first recovery tank 230, and the first liquid supply pump 220 is connected to the first liquid supply conduit 210. The second mixed liquid discharge unit 300 includes a second liquid supply conduit 310, a second liquid supply pump 320, a second recovery tank 330, and the like. The second liquid feed conduit 310 is a conduit connecting the second storage tank 61 and the second recovery tank 330, and a second liquid feed pump 320 is connected to the second storage conduit 310. When the first liquid feed pump 220 is operated, the mixed liquid stored in the first storage tank 51 is sent to the first recovery tank 230 through the first liquid feed conduit 210 and is stored in the first recovery tank 230. Similarly, when the second liquid feed pump 320 is operated, the mixed liquid stored in the second storage tank 61 is sent to the second recovery tank 330 through the second liquid feed conduit 310 and is stored in the second recovery tank 330. In the present embodiment, for example, the first liquid feed pump 220 and the second liquid feed pump 320 are operated continuously (continuously).

[0104] There are no particular limitations on the types of the first liquid supply conduit 210 and the second liquid supply conduit 310, but for example, a PEEK tube can be suitably used. There are also no particular limitations on the types of the first liquid supply pump 220 and the second liquid supply pump 320, but for example, a syringe pump, a diaphragm pump, etc. can be used.

[0105] As described above, the first intermediate inlet path 81A opens to the first flow path wall surface 231, and the second intermediate inlet path 81B opens to the second flow path wall surface 232, so that the mixed liquid transferred by the additional supply unit 90 can be continuously supplied from the side to the gas-liquid contact flow path 23. In other words, the additional mixed liquid introduced from the first intermediate inlet path 81A can be merged with the mixed liquid flowing down from the first end 23A side of the gas-liquid contact flow path 23 along the first flow path wall surface 231. Similarly, the additional mixed liquid introduced from the second intermediate inlet path 81B can be merged with the mixed liquid flowing down from the first end 23A side of the gas-liquid contact flow path 23 along the second flow path wall surface 232. Furthermore, since the amount of liquid stored in the first storage tank 51 increases due to the mixed liquid continuously supplied by the additional supply unit 90, the first mixed liquid discharge unit 200 may continuously discharge the mixed liquid from the first storage tank 51 so as to maintain a constant liquid level in the first storage tank 51. Similarly, since the amount of liquid stored in the second storage tank 61 increases due to the mixed liquid continuously supplied by the additional supply unit 90, the second mixed liquid discharge unit 300 may continuously discharge the mixed liquid from the second storage tank 61 so as to maintain a constant liquid level in the second storage tank 61. In other words, by continuously supplying the mixed liquid by the additional supply unit 90 and continuously discharging the mixed liquid by the first mixed liquid discharge unit 200 and the second mixed liquid discharge unit 300, a mixed liquid in which the low-boiling point components are concentrated and a mixed liquid in which the high-boiling point components are concentrated can each be continuously obtained. Of course, in the micro-distillation device 1A of embodiment 2, the first circulation pump 52 and the second circulation pump 62 are operated continuously, similar to the micro-distillation device 1 described in embodiment 1.

[0106] REFERENCE SIGNS LIST 1 Micro-distillation device 2 Distillation unit 5 First circulation unit 6 Second circulation unit 21 Liquid inlet 22 Vapor inlet 23 Gas-liquid contact channel 24 Liquid outlet 25 Vapor outlet 26 Liquid inlet channel 27 Liquid outlet channel 28 Vapor inlet channel 29 Vapor outlet channel 100 Control device

Claims

1. A distillation unit comprising: a liquid inlet for introducing a mixed liquid containing at least two components having different boiling points; a steam inlet for introducing vapor derived from the mixed liquid; a gas-liquid contact flow path for contacting the mixed liquid introduced from the liquid inlet and the vapor derived from the mixed liquid introduced from the vapor inlet in counterflow with each other; a liquid outlet for discharging the mixed liquid that has flowed through the gas-liquid contact flow path; and a steam outlet for discharging the vapor derived from the mixed liquid that has flowed through the gas-liquid contact flow path; a first circulation unit for circulating a condensate obtained by condensing the vapor derived from the mixed liquid discharged from the steam outlet to the liquid inlet; and a second circulation unit for circulating the vapor obtained by evaporating the mixed liquid discharged from the liquid outlet to the vapor inlet.

2. The micro-distillation device described in claim 1, wherein in the distillation unit, the gas-liquid contact flow path is configured as a flow path extending in one direction, one end side of the gas-liquid contact flow path is arranged vertically upward and the liquid inlet and the vapor outlet are arranged on said one end side, and the other end side of the gas-liquid contact flow path is arranged vertically downward and the liquid outlet and the vapor inlet are arranged on said other end side.

3. The micro-distillation device according to claim 1 or 2, wherein in the distillation unit, the mixed liquid introduced from the liquid inlet flows down a liquid flow area formed along a flow path wall surface that forms the gas-liquid contact flow path, and the vapor derived from the mixed liquid supplied from the vapor inlet flows in the opposite direction to the mixed liquid along a vapor flow area formed on the central side of the cross section of the gas-liquid contact flow path.

4. The micro-distillation device according to claim 3, wherein the distillation unit has a plurality of the liquid inlets and a plurality of the liquid outlets.

5. The micro-distillation device described in claim 4, wherein the flow path wall surface in the distillation unit includes a first surface and a second surface different from the first surface, the multiple liquid inlets include first and second liquid inlets arranged on one end side of the gas-liquid contact flow path, and the multiple liquid outlets include first and second liquid outlets arranged on the other end side of the gas-liquid contact flow path, the mixed liquid introduced from the first liquid inlet flows down the first surface of the flow path wall surface and is then discharged from the first liquid outlet, and the mixed liquid introduced from the second liquid inlet flows down the second surface of the flow path wall surface and is then discharged from the second liquid outlet.

6. The micro-distillation device according to claim 2, wherein the distillation unit further has an intermediate inlet for introducing the mixed liquid into an intermediate position of the gas-liquid contact flow path, in addition to the liquid inlet arranged on one end side of the gas-liquid contact flow path.

7. A micro-distillation device as described in claim 1 or 2, wherein the first circulation unit has a first storage tank for storing condensed liquid obtained by condensing vapor derived from the mixed liquid discharged from the vapor outlet.

8. The micro-distillation device according to claim 1 or 2, wherein the second circulation unit has a second storage tank for storing the mixed liquid discharged from the liquid outlet of the distillation unit.

9. The micro-distillation device according to claim 1 or 2, wherein the second circulation unit further comprises an evaporation unit having a micro-flow path for circulating the mixed liquid discharged from the liquid outlet of the distillation unit, and an evaporation heater for evaporating the mixed liquid flowing through the micro-flow path.

10. The micro-distillation device according to claim 1 or 2, wherein the distillation unit further comprises a temperature control mechanism for forming a predetermined temperature gradient in which the temperature gradually decreases from the other end side to the one end side of the gas-liquid contact flow path.

11. The micro-distillation device according to claim 2, wherein in the distillation unit, a liquid inlet channel connecting one end side of the gas-liquid contact channel to the liquid inlet, and a liquid outlet channel connecting the other end side of the gas-liquid contact channel to the liquid outlet are each formed as a micro-channel.

12. The microdistillation device according to claim 3, wherein the liquid film thickness of the mixed liquid flowing down along the wall surface of the flow channel is on the order of micrometers.

13. A distillation method for distilling a mixed liquid containing at least two components having different boiling points, using the microdistillation device described in claim 1.

14. The mixed liquid contains a predetermined low boiling point component and a high boiling point component having a boiling point higher than that of the low boiling point component, and in the distillation unit, the mixed liquid introduced from the liquid inlet and the steam derived from the mixed liquid introduced from the steam inlet are brought into gas-liquid countercurrent contact in the gas-liquid contact flow path, thereby discharging the low boiling point component in a liquid phase obtained by evaporating the low boiling point component contained in the mixed liquid from the steam outlet together with the steam derived from the mixed liquid introduced from the steam inlet, and discharging the high boiling point component in a liquid phase obtained by condensing the high boiling point component contained in the steam derived from the mixed liquid in the gas-liquid contact flow path from the liquid outlet together with the mixed liquid introduced from the liquid inlet, and the first circulation unit continuously circulates the condensate obtained by condensing the steam in which the low boiling point component is concentrated, discharged from the steam outlet of the distillation unit, to the liquid inlet, The distillation method according to claim 13, wherein the second circulation unit continuously circulates the vapor obtained by evaporating the mixed liquid in which the high boiling point component is concentrated, discharged from the liquid discharge port of the distillation unit, to the vapor inlet, thereby separating the low boiling point component and the high boiling point component contained in the mixed liquid.

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