Microdistillation apparatus and distillation method using the same

Abstract

The microdistillation apparatus of the present invention comprises: a distillation unit, a first circulation unit, and a second circulation unit. The distillation unit comprises: a liquid inlet for introducing a mixture containing at least two components with different boiling points; a steam inlet for introducing steam from the mixture; a gas-liquid contact flow path for contacting the mixture introduced from the liquid inlet and the steam from the mixture introduced from the steam inlet in a countercurrent manner; a liquid outlet for discharging the mixture flowing through the gas-liquid contact flow path; and a steam outlet for discharging the steam from the mixture flowing through the gas-liquid contact flow path. The first circulation unit circulates condensate to the liquid inlet, the condensate being obtained by condensing the steam from the mixture discharged from the steam outlet. The second circulation unit circulates steam to the steam inlet, the steam being obtained by evaporating the mixture discharged from the liquid outlet.

Description

Technical Field

[0001] This disclosure relates to a microdistillation apparatus and a distillation method using the microdistillation apparatus. Background Technology

[0002] In chemical synthesis that generates a target compound through a chemical reaction, unwanted byproducts are often generated. To address this, techniques are known to separate the target component from other components in a mixture containing at least two components by utilizing gas-liquid contact (e.g., see Patent Document 1, etc.).

[0003] Existing technical documents

[0004] Patent documents

[0005] Patent Document 1: Japanese Patent Application Publication No. 2006-198542

[0006] Patent Document 2: Japanese Patent Application Publication No. 2007-136280

[0007] Patent Document 3: Japanese Patent No. 5627837 Summary of the Invention

[0008] The problem that the invention aims to solve

[0009] However, conventional methods for separating specific components from other components in a mixture via distillation have not been very efficient, and there is still room for improvement in this regard. The technology disclosed herein was developed in view of this reality, and its purpose is to provide a microdistillation apparatus capable of efficiently separating specific components from other components in a mixture.

[0010] Problem Solving Methods

[0011] The main points of this disclosure are as follows.

[0012] [Method 1]

[0013] The microdistillation apparatus of method 1 includes: a distillation unit, a first circulation unit, and a second circulation unit.

[0014] The distillation unit includes:

[0015] A liquid inlet for introducing a mixture containing at least two components with different boiling points.

[0016] Steam inlets from the above mixture are introduced separately.

[0017] A gas-liquid contact flow path in which the mixture introduced from the liquid inlet and the steam derived from the mixture introduced from the steam inlet come into contact in a countercurrent manner.

[0018] The liquid outlet that discharges the mixture flowing through the above-mentioned gas-liquid contact flow path, and

[0019] The vapor outlet discharges the vapor originating from the mixed liquid that has flowed through the above-mentioned gas-liquid contact flow path.

[0020] The first circulation unit circulates the condensate back to the liquid inlet, the condensate being obtained by condensing the vapor derived from the mixture discharged from the steam outlet.

[0021] The second circulation unit circulates steam to the steam inlet, which is obtained by evaporating the mixture discharged from the liquid outlet.

[0022] [Method 2]

[0023] According to the microdistillation apparatus of method 1, wherein...

[0024] In the aforementioned distillation unit, the gas-liquid contact flow path is configured as a flow path extending in one direction.

[0025] One end of the aforementioned gas-liquid contact flow path is positioned on the upper side in the vertical direction, and a liquid inlet and a vapor outlet are provided on this end side.

[0026] The other end of the gas-liquid contact flow path is located on the lower side in the vertical direction, and the liquid outlet and the steam inlet are provided on the other end.

[0027] [Method 3]

[0028] According to the microdistillation apparatus of method 1 or 2, wherein...

[0029] In the distillation unit described above, the mixture introduced from the liquid inlet flows downward in the liquid flow area, and the steam supplied from the steam inlet from the mixture flows in the opposite direction to the mixture along the steam flow area. The liquid flow area is formed along the flow path wall that forms the gas-liquid contact flow path, and the steam flow area is formed at the center side of the cross-section of the gas-liquid contact flow path.

[0030] [Method 4]

[0031] The microdistillation apparatus according to any one of methods 1 to 3, wherein...

[0032] The distillation unit described above has multiple liquid inlets and multiple liquid outlets described above.

[0033] [Method 5]

[0034] According to the microdistillation apparatus of method 4, wherein...

[0035] The flow path wall in the distillation unit includes a first surface and a second surface different from the first surface.

[0036] The plurality of liquid inlets include a first and a second liquid inlet disposed at one end of the gas-liquid contact flow path.

[0037] The plurality of liquid outlets mentioned above include a first and a second liquid outlet disposed at the other end of the gas-liquid contact flow path.

[0038] The mixture introduced through the first liquid inlet flows downwards along the first surface of the flow path wall and is then discharged from the first liquid outlet.

[0039] The mixture introduced from the second liquid inlet flows downward on the second surface of the flow path wall and is then discharged from the second liquid outlet.

[0040] [Method 6]

[0041] According to the microdistillation apparatus of method 2, wherein...

[0042] In addition to the liquid inlet located at one end of the gas-liquid contact flow path, the distillation unit further has an intermediate inlet for introducing the mixture into the middle of the gas-liquid contact flow path.

[0043] [Method 7]

[0044] The microdistillation apparatus according to any one of methods 1 to 6, wherein...

[0045] The first circulation unit described above has a first storage tank for storing condensate, which is obtained by condensing steam from the mixture discharged from the steam outlet described above.

[0046] [Method 8]

[0047] The microdistillation apparatus according to any one of methods 1 to 7, wherein...

[0048] The second circulation unit has a second storage tank for storing the mixture discharged from the liquid outlet of the distillation unit.

[0049] [Method 9]

[0050] The microdistillation apparatus according to any one of methods 1 to 8, wherein...

[0051] The second circulation unit further includes an evaporation unit, which has a microflow path for circulating the mixture discharged from the liquid outlet of the distillation unit and an evaporation heater for evaporating the mixture flowing through the microflow path.

[0052] [Method 10]

[0053] The microdistillation apparatus according to any one of methods 1 to 9, wherein...

[0054] The distillation unit further includes a temperature control mechanism for forming a given temperature gradient that gradually decreases from one end of the gas-liquid contact flow path to the other.

[0055] [Method 11]

[0056] According to the microdistillation apparatus of method 2, wherein...

[0057] In the distillation unit described above, a liquid inlet path and a liquid outlet path are formed in the form of microflow paths. The liquid inlet path connects one end of the gas-liquid contact flow path to the liquid inlet, and the liquid outlet path connects the other end of the gas-liquid contact flow path to the liquid outlet.

[0058] [Method 12]

[0059] According to the microdistillation apparatus of method 3, wherein...

[0060] The liquid film thickness of the mixture flowing downward along the wall of the aforementioned flow path is on the order of micrometers.

[0061] [Method 13]

[0062] A distillation method, the method comprising:

[0063] The microdistillation apparatus described in Method 1 is used to distill a mixture containing at least two components with different boiling points.

[0064] [Method 14]

[0065] According to the distillation method described in method 13, wherein...

[0066] The mixture described above contains a given low-boiling-point component and a high-boiling-point component with a higher boiling point compared to the low-boiling-point component.

[0067] In the distillation unit described above, the mixture introduced from the liquid inlet and the vapor derived from the mixture introduced from the steam inlet are brought into countercurrent contact in the gas-liquid contact flow path, thereby...

[0068] The low-boiling-point component of the liquid phase is discharged from the steam outlet along with the steam from the mixture introduced from the steam inlet. This low-boiling-point component of the liquid phase is obtained by evaporating the low-boiling-point component contained in the mixture.

[0069] The high-boiling-point component of the liquid phase is discharged from the liquid outlet along with the mixture introduced from the liquid inlet. The high-boiling-point component of the liquid phase is obtained by condensing the high-boiling-point component contained in the vapor derived from the mixture in the gas-liquid contact flow path.

[0070] The first circulation unit continuously circulates the condensate to the liquid inlet, which is obtained by condensing the low-boiling-point components from the steam outlet of the distillation unit.

[0071] The second circulation unit continuously circulates steam to the steam inlet, which is obtained by evaporating a concentrated mixture of high-boiling-point components discharged from the liquid outlet of the distillation unit.

[0072] Thus, the low-boiling-point components and high-boiling-point components contained in the above mixture are separated.

[0073] The effects of the invention

[0074] According to the technology disclosed herein, a microdistillation apparatus can be provided that can efficiently separate specific components contained in a mixture from other components. Attached Figure Description

[0075] Figure 1 This is a schematic diagram showing an example of the microdistillation apparatus of Embodiment 1.

[0076] Figure 2 This is a top view of the distillation unit in Embodiment 1.

[0077] Figure 3 This is a diagram illustrating the method for manufacturing the distillation unit of Embodiment 1.

[0078] Figure 4 It is shown schematically. Figure 2 The diagram shows a cross-section viewed along the direction of arrow AA.

[0079] Figure 5 This is a diagram illustrating the temperature control mechanism.

[0080] Figure 6 This is a diagram illustrating the temperature measurement points in the embodiment.

[0081] Figure 7 This is a diagram illustrating the experimental setup used in the comparative example.

[0082] Figure 8 This is a diagram illustrating the microdistillation apparatus of Embodiment 2.

[0083] Symbol Explanation

[0084] 1. Microdistillation apparatus

[0085] 2 Distillation Unit

[0086] 5. First Cyclic Unit

[0087] 6. Second Cycle Unit

[0088] 21 Liquid inlet

[0089] 22 Steam inlet

[0090] 23 Gas-liquid contact flow path

[0091] 24 Liquid discharge outlet

[0092] 25 Steam exhaust port

[0093] 26 Liquid inlet path

[0094] 27 Liquid discharge path

[0095] 28 Steam Inlet Path

[0096] 29 Steam exhaust path

[0097] 100 Control device Detailed Implementation

[0098] The microdistillation apparatus according to embodiments of the present disclosure will now be described with reference to the accompanying drawings. The various components and combinations thereof in the embodiments are examples only; additions, omissions, substitutions, and other modifications to the components may be made as appropriate without departing from the spirit of the present disclosure. The present invention is not limited to the embodiments, but only to the claims. Furthermore, the various methods disclosed in this specification can also be combined with any other features disclosed in this specification.

[0099] <Implementation Method 1>

[0100] Microdistillation apparatus

[0101] Figure 1 This is a schematic diagram showing an example of the microdistillation apparatus 1 according to Embodiment 1.

[0102] The microdistillation apparatus 1 includes a distillation unit 2, a first circulation unit 5, a second circulation unit 6, etc., and is a microfluidic device for distilling a mixed fluid containing at least two components with different boiling points. In this specification, "fluid" may include not only liquids and gases, but also fluids composed of liquids and gases, and mixed-phase fluids in which liquids and / or gases contain solids.

[0103] [Distillation Unit]

[0104] Figure 2This is a top view of the distillation unit 2 according to Embodiment 1. Symbol B in the figure represents the substrate of the distillation unit 2. The substrate B has a rectangular plate-like chip shape. As will be described in detail later, the distillation unit 2 is configured to receive a mixture (hereinafter referred to as "mixture") containing at least two components with different boiling points from the first circulation unit 5, and steam obtained by evaporating the mixture from the second circulation unit 6. Furthermore, Figure 2 The directions shown are for the purpose of conveniently illustrating the relative positional relationship of each element with reference to the substrate B of distillation unit 2, and do not represent the absolute direction of each element.

[0105] The distillation unit 2 in this embodiment includes:

[0106] Liquid inlet 21 is used to introduce the mixture supplied from the first circulation unit 5;

[0107] Steam inlet 22 is used to introduce steam from the mixture supplied from the second circulation unit 6;

[0108] A gas-liquid contact flow path 23 is used to make the mixture introduced from the liquid inlet 21 and the steam from the mixture introduced from the steam inlet 22 come into countercurrent contact with each other.

[0109] Liquid outlet 24 discharges the mixture flowing through the gas-liquid contact flow path 23;

[0110] Steam outlet 25, which discharges the vapor originating from the mixed liquid that flows through the gas-liquid contact flow path 23; etc.

[0111] These liquid inlets 21, steam inlets 22, gas-liquid contact flow paths 23, liquid outlets 24, steam outlets 25, etc., are formed on substrate B.

[0112] The shape of the gas-liquid contact flow path 23 is not particularly limited. Figure 1 and Figure 2 In the example shown, the flow path is configured as a straight line extending in one direction. At the ends of the gas-liquid contact flow path 23 in its extending direction (axial direction), the end indicated by symbol 23A is referred to as the "first end," and the other end indicated by symbol 23B is referred to as the "second end." In this embodiment, a liquid inlet 21 and a steam outlet 25 are provided on the first end 23A side of the gas-liquid contact flow path 23, and a liquid outlet 24 and a steam inlet 22 are provided on the second end 23B side. These configurations are exemplary. Examples of the gas-liquid contact flow path 23 having an axial length (from the first end 23A to the second end 23B) of 10 mm or more and 3000 mm or less are preferred, 20 mm or more and 2000 mm or less are preferred, and 30 mm or more and 1000 mm or less are more desirable.

[0113] The distillation unit 2 further includes a liquid inlet passage 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 passage 27 connecting the second end 23B (the other end) of the gas-liquid contact flow path 23 to the liquid outlet 24. The mixture 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 via the liquid inlet passage 26. The mixture guided to the first end 23A of the gas-liquid contact flow path 23 flows along the gas-liquid contact flow path 23, which extends in a straight line (i.e., from the first end 23A side to the second end 23B side). Then, the mixture after flowing through the gas-liquid contact flow path 23 flows through the liquid outlet passage 27 connected to the second end 23B side of the gas-liquid contact flow path 23, and is then discharged from the liquid outlet 24 to the outside of the distillation unit 2.

[0114] exist Figure 1 and Figure 2 In the example shown, distillation unit 2 has two liquid inlets 21, which are referred to as the first liquid inlet 21A and the second liquid inlet 21B, respectively. Additionally, distillation unit 2 has two liquid outlets 24, which are referred to as the first liquid outlet 24A and the second liquid outlet 24B, respectively. The number of liquid inlets 21 and liquid outlets 24 in distillation unit 2 is not particularly limited.

[0115] In addition, such as Figure 1 and Figure 2 As shown, the distillation unit 2 has two liquid inlet paths 26 corresponding to each liquid inlet 21A, 21B, and two liquid outlet paths 27 corresponding to each liquid outlet 24A, 24B. The first liquid inlet path 26A is connected to the first liquid inlet 21A and the first end 23A of the gas-liquid contact flow path 23. The second liquid inlet path 26B is connected to the second liquid inlet 21B and the first end 23A of the gas-liquid contact flow path 23. Furthermore, the first liquid outlet path 27A is connected to the second end 23B of the gas-liquid contact flow path 23 and the first liquid outlet 24A. The second liquid outlet path 27B is connected to the second end 23B of the gas-liquid contact flow path 23 and the second liquid outlet 24B. It should be noted that, as... Figure 2 As shown in the top view of distillation unit 2, the liquid inlet path 26 and the liquid outlet path 27 are both curved. The shapes of the liquid inlet path 26 and the liquid outlet path 27 are not particularly limited.

[0116] The distillation unit 2 further includes a steam inlet passage 28 connecting the second end 23B of the gas-liquid contact flow path 23 to the steam inlet 22, and a steam outlet passage 29 connecting the first end 23A of the gas-liquid contact flow path 23 to the steam outlet 25. Steam from the mixture supplied to the distillation unit 2 from the second circulation unit 6 via the steam inlet passage 28 is guided to the second end 23B of the gas-liquid contact flow path 23. The steam from the mixture guided to the second end 23B of the gas-liquid contact flow path 23 flows along the linearly extending gas-liquid contact flow path 23 (i.e., from the second end 23B side to the first end 23A side). That is, the direction of the steam from the mixture flowing along the gas-liquid contact flow path 23 is opposite to the direction of the mixture flowing from the first end 23A side to the second end 23B side. Then, the vapor from the mixture 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 from the vapor discharge port 25 to the outside of the distillation unit 2.

[0117] As an example, the distillation unit 2 can be fabricated by forming the liquid inlet 21, steam inlet 22, gas-liquid contact flow path 23, liquid outlet 24, steam outlet 25, liquid inlet path 26, liquid outlet path 27, steam inlet path 28, and steam outlet path 29 on the substrate B.

[0118] Figure 3 This diagram illustrates the method for manufacturing distillation unit 2 according to Embodiment 1. Figure 3 The first substrate B1 shown is, for example, a substrate forming the front side of the distillation unit 2. The third substrate B3 is, for example, a substrate forming the back side of the distillation unit 2. The second substrate B2 is, for example, a substrate forming an intermediate layer sandwiched between the first substrate B1 and the third substrate B3. Each substrate B1 to B3 is a plate-like member having a rectangular shape when viewed from above, and for example, having the same planar shape. The shape and size of each substrate B1 to B3 are not particularly limited. Furthermore, the material of each substrate B1 to B3 is not particularly limited; for example, glass, silicon, silicon dioxide, quartz, resin, silicon carbide, etc., can be used. Moreover, borosilicate glass, which has resistance to organic chemicals and heat resistance, is preferably used as the material for substrates B1 and B2.

[0119] As a method for manufacturing the distillation unit 2, for example, openings for forming liquid inlet 21, vapor inlet 22, liquid outlet 24, vapor outlet 25, etc., are formed on the first substrate B1 in the form of through holes penetrating the first substrate B1 in the thickness direction. Additionally, openings for forming flow paths such as gas-liquid contact flow path 23, liquid inlet path 26, liquid outlet path 27, vapor inlet path 28, and vapor outlet path 29 are formed on the second substrate B2 in the form of through holes penetrating the second substrate B2. Then, the first substrate B1 can be bonded to one side of the second substrate B2, and the third substrate B3 can be bonded to the other side of the second substrate B2. Thus, the aforementioned flow paths for allowing the mixture and vapor derived from the mixture to flow can be formed inside the substrate assembly. It should be noted that the substrate forming the distillation unit 2 can be a transparent or semi-transparent substrate. Therefore, the various flow paths such as the gas-liquid contact flow path 23, liquid inlet path 26, liquid outlet path 27, vapor inlet path 28, and vapor outlet path 29 can be visually identified from the outside.

[0120] There is no particular limitation on the method for forming through holes on the first substrate B1 and the second substrate B2. For example, through holes can be formed by etching or micro-machining of the first substrate B1 and the second substrate B2. Of course, the above-described method for manufacturing the distillation unit 2 is just one example, and various methods can be used without particular limitation. For example, the distillation unit 2 can be manufactured by stacking two or more substrates, or by stacking four or more substrates. It should be noted that the openings used to form the liquid inlet 21, steam inlet 22, liquid outlet 24, steam outlet 25, etc., can be fitted with one-touch connectors such as tube fittings.

[0121] The distillation unit 2 constructed as described above can, for example, be formed as a microfluidic device in the form of a chip with microscale flow paths. In use, the first end 23A of the gas-liquid contact flow path 23 is positioned upwards in the vertical direction, and the second end 23B is positioned downwards in the vertical direction. Hereinafter, in the distillation unit 2, the direction in which the gas-liquid contact flow path 23 extends is referred to as the "vertical direction," and the horizontal direction is referred to as the "width direction."

[0122] Furthermore, for distillation unit 2, the liquid inlet path 26 and liquid outlet path 27 described above are each formed as a microfluidic path. In this specification, at least one of the flow path width and flow path height of the liquid inlet path 26 and liquid outlet path 27 formed in the form of microfluidic paths is at the micrometer (μm) level. For example, it is possible to set the flow path width of the liquid inlet path 26 and liquid outlet path 27 to 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. It is possible to set the flow path height of the liquid inlet path 26 and liquid outlet path 27 to 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.

[0123] Figure 4 It is shown schematically. Figure 2 The diagram shows a cross-section viewed along the direction of arrow AA. That is, Figure 4 The cross-section of the gas-liquid contact flow path 23 in distillation unit 2 is shown. The cross-section of the gas-liquid contact flow path 23 is a section in a direction orthogonal to the axial direction in which the gas-liquid contact flow path 23 extends. Figure 4 The cross-sectional shape of the gas-liquid contact flow path 23 shown is an example. Figure 4 In the example shown, the gas-liquid contact flow path 23 has a square cross-section.

[0124] Figure 4 The symbols 231-234 shown represent the first to fourth flow path walls forming the gas-liquid contact flow path 23. In this embodiment, the distillation unit 2 is configured such that a liquid flow area is formed in all or part of each flow path wall 231-234, and the mixture flows downward along the liquid flow area. Figure 4 In the example shown, the first flow path wall 231 and the second flow path wall 232 are arranged opposite each other, for example, extending along the side of the distillation unit 2. Similarly, the third flow path wall 233 and the fourth flow path wall 234 are arranged opposite each other, for example, extending along the front of the distillation unit 2.

[0125] For example, the first flow path wall 231 in the gas-liquid contact flow path 23 and the flow path wall 26A1 in the first liquid inlet path 26A (see reference) Figure 2 The walls are connected flush. "Flush" here means that the connection points between the walls are connected in a manner that does not create a height difference. Furthermore, the second flow path wall 232 in the gas-liquid contact flow path 23 and the flow path wall 26B1 in the second liquid inlet path 26B (see reference...) Figure 2The mixture is flush with the first liquid inlet 21A in the distillation unit 2. In this manner, when the mixture is introduced into the gas-liquid contact flow path 23 through the first liquid inlet 26A, it easily flows downward along the first flow path wall 231 (first surface), which is flush with the flow path wall 26A1 of the first liquid inlet 26A. After flowing downward along the first flow path wall 231, the mixture is discharged from the first liquid outlet 24A through the first liquid outlet 27A. Similarly, when the mixture is introduced into the gas-liquid contact flow path 23 through the second liquid inlet 21B in the distillation unit 2, it easily flows downward along the second flow path wall 232 (second surface different from the first surface), which is flush with the flow path wall 26B1 of the second liquid inlet 26B. Thus, after the mixture flows downward along the second flow path wall 232, it is discharged from the second liquid outlet 24B through the second liquid outlet 27B. By introducing the mixture as two separate systems into the two different flow path walls 231 and 232 of the gas-liquid contact flow path 23 of the distillation unit 2, and discharging the mixture flowing down along the flow path walls 231 and 232 as two separate systems, the mixture can flow smoothly along the flow path walls 231 and 232. Furthermore, it can prevent the gas-liquid contact flow path 23 from being blocked by the mixture, and easily ensure the flow rate of the mixture.

[0126] As described above, the gas-liquid contact flow path 23 in the distillation unit 2 can function as a wetting wall for the mixture to flow downward in a thin film, with all or part of the flow path walls 231-234 extending in the vertical direction (e.g., the first flow path wall 231 and the second flow path wall 232) serving as the wetting wall for the mixture to flow downward in a thin film. Thus, a hollow vapor flow region is formed at the center of the cross-section of the gas-liquid contact flow path 23, allowing vapor from the mixture to flow through, and the mixture flows downward along the flow path walls forming the gas-liquid contact flow path 23.

[0127] As an example, Figure 4 The mixture is shown in the method illustrated. Figure 4The liquid flows downward along the liquid flow area RL formed on the first flow path wall 231 and the second flow path wall 232. Furthermore, in the hollow steam flow area RG formed at the center of the cross-section of the gas-liquid contact flow path 23, the steam originating from the mixture flows in the opposite direction to the mixture along this steam flow area RG. In this way, the gas-liquid contact flow path 23 is not blocked by the mixture. As a result, the mixture introduced from the liquid inlet 21 and the steam originating from the mixture introduced from the steam inlet 22 can be appropriately contacted in the gas-liquid contact flow path 23 in a counter-current manner. Therefore, efficient heat transfer and mass transfer can be achieved between the steam originating from the mixture and the mixture, resulting in a highly efficient distillation operation. In particular, according to the distillation unit 2 of this embodiment, gravity can be used to appropriately cause the mixture to flow downward along the flow path wall of the gas-liquid contact flow path 23. That is, the flow path wall extending vertically in the gas-liquid contact flow path 23 can function as a wetting wall, allowing the mixture to flow appropriately downwards along the flow path wall. It should be noted that, for the mixture to flow appropriately downwards on the flow path wall (liquid flow area RL) of the gas-liquid contact flow path 23, the effect of gravity and the wettability of the substrate (wall material) forming the flow path wall may be relevant. Therefore, it is preferable to design the flow path wall as a wetting wall such that the contact angle (θ) between the mixture (liquid) and the flow path wall (substrate) of the gas-liquid contact flow path 23 is less than 90°.

[0128] It should be noted that, in this embodiment, the liquid film thickness of the mixed liquid flowing downward along the liquid flow area RL in the gas-liquid contact flow path 23 can be described as being on the micrometer scale. For example, the liquid film thickness can be described as being 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 appropriately prevents the cross-section of the gas-liquid contact flow path 23 from being blocked by the mixed liquid flowing downward along the liquid flow area RL of the gas-liquid contact flow path 23. Furthermore, as described above, by causing the mixed liquid to flow downward along the multiple different flow path walls 231, 232 forming the gas-liquid contact flow path 23, the total flow rate of the mixed liquid flowing downward along the liquid flow area RL can be ensured, and the blockage of the cross-section of the gas-liquid contact flow path 23 by the mixed liquid can be appropriately prevented. From the above perspective, the shape of the cross-section of the gas-liquid contact flow path 23 is not particularly limited. For example, it can be a square. In this case, the length of each side of the square (corresponding to the flow path 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. In this way, the total flow rate of the mixture flowing downward along the liquid flow area RL can be ensured, and the blockage of the cross-section of the gas-liquid contact flow path 23 by the mixture can be appropriately suppressed.

[0129] Furthermore, the distillation unit 2 of this embodiment includes a temperature regulating mechanism 3, which is used to form a given temperature gradient in which the temperature gradually decreases from the second end 23B side of the gas-liquid contact flow path 23 toward the first end 23A side. Figure 5 This diagram illustrates the temperature regulating mechanism 3. The temperature regulating mechanism 3 comprises a temperature regulating heater and a heat-conducting member for conducting heat from the temperature regulating heater.

[0130] exist Figure 5 In the example shown, a first heat-conducting member 31 and a second heat-conducting member 32 are mounted on the front side of the distillation unit 2, and a third heat-conducting member 33 and a fourth heat-conducting member 34 are mounted on the back side of the distillation unit 2. Each heat-conducting member 31-34 has a plate shape, for example, formed of a heat-conducting material such as a copper plate. Figure 5 In the example shown, all heat-conducting components 31-34 have the same shape, but are not limited to this. Of course, heat-conducting components 31-34 can also be formed of other metals with excellent thermal conductivity.

[0131] On the front side of the distillation unit 2, a gap (visual identification slit) SL is formed between the first heat-conducting member 31 and the second heat-conducting member 32 in the vertical direction, through which the gas-liquid contact flow path 23 can be visually identified. The third heat-conducting member 33 and the fourth heat-conducting member 34, which are located on the back side of the distillation unit 2, are arranged in the same manner. That is, a gap (visual identification slit) SL is formed between the third heat-conducting member 33 and the fourth heat-conducting member 34 in the vertical direction, through which the gas-liquid contact flow path 23 can be visually identified.

[0132] For example, such as Figure 5 As shown, each heat-conducting component 31 to 34 extends in the vertical direction of the distillation unit 2, covering the distance from the height of the first end 23A corresponding to the gas-liquid contact flow path 23 to the height of the second end 23B. Figure 5 The symbol 35 shown represents a temperature regulating heater. The temperature regulating heater 35, for example, is a film heater, attached to the lower region of each heat-conducting member 31-34. During operation, the heat released by the temperature regulating heater 35 installed on each heat-conducting member 31-34 is transferred 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 from the temperature regulating heater 35 is more easily transferred the closer it is to the temperature regulating heater 35, and less easily transferred the farther it is from the temperature regulating heater 35. As a result, a suitable temperature gradient (temperature distribution) can be generated along the extension direction (long axis direction) of the gas-liquid contact flow path 23; more specifically, a given temperature gradient (temperature distribution) can be formed where the temperature gradually decreases from the second end 23B side of the gas-liquid contact flow path 23 towards the first end 23A side. The set temperature of the heater 35 for temperature regulation depends on the boiling point of the components contained in the mixture. Examples of such temperatures are 30°C or higher and 400°C or lower, preferably 40°C or higher and 350°C or lower, and more preferably 50°C or higher and 300°C or lower.

[0133] [First Loop Unit]

[0134] Next, refer to Figure 1 The first circulation unit 5 in the microdistillation apparatus 1 will be described. The first circulation unit 5 is a unit for recirculating the condensate to the liquid inlet 21 of the distillation unit 2, the condensate being obtained by condensing the vapor from the mixture discharged from the vapor outlet 25 of the distillation unit 2.

[0135] The first circulation unit 5 comprises 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 destination pipe 56. The return pipe 55 is used to condense the vapor from the mixture discharged from the steam outlet 25 of the distillation unit 2 during transport, and to transport the resulting condensate to the first storage tank 51. For example, one end of the return pipe 55 is connected to the steam outlet 25 of the distillation unit 2 via a connector FT, and the other end is connected to the first storage tank 51. The vapor from the mixture discharged from the steam outlet 25 of the distillation unit 2 is cooled and condensed as it flows through the return pipe 55. The mixture (condensate) that undergoes a phase change from the gas phase to the liquid phase during its flow through the return pipe 55 is stored in the first storage tank 51. The connector FT is, for example, a tube fitting or other one-touch connector that airtightly connects the steam outlet 25 of the distillation unit 2 to the loop piping 55.

[0136] The outgoing pipe 56 is used to transport (supply) the mixture (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 arranged in the middle of the outgoing pipe 56 to branch the outgoing pipe 56 into two branches.

[0137] In the outgoing piping 56, the section from the first storage tank 51 to the distributor 54 is referred to as the main piping 56A. The two branch pipes branching off from the main piping 56A via the distributor 54 are referred to as 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 in 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 in the distillation unit 2. Borosilicate glass, which is resistant to organic chemicals and has heat resistance, can be used as the material for the distributor 54.

[0138] A first circulation pump 52 is connected to the main pipe 56A in the outgoing pipe 56. When the first circulation pump 52 operates, the mixture (condensate) LqA stored in the first storage tank 51 is pressurized (e.g., pumped) to the outgoing pipe 56 (main pipe 56A), and the mixture (condensate) LqA flows from upstream to downstream in the outgoing pipe 56. That is, the mixture (condensate) LqA pumped by the first circulation pump 52 is supplied to the distillation unit 2 through the outgoing pipe 56. At this time, the mixture (condensate) LqA is introduced to the first liquid inlet 21A through the first branch pipe 56B in the outgoing pipe 56, and to 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 include syringe pumps, diaphragm pumps, etc.

[0139] Furthermore, the return pipe 55 and the outgoing pipe 56 in the first circulation conduit 50 can be, for example, small-diameter flexible pipes. For example, PEEK pipes utilizing PEEK (polyether ether ketone) resin can be suitably used as materials with resistance to organic chemicals. The inner diameter of the first circulation conduit 50 (PEEK pipe) can be in the micrometer range, for example, 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. In particular, by setting the inner diameter of the return pipe 55 to the micrometer range as described above, the heat transfer area for the steam discharged from the steam outlet 25 of the distillation unit 2 can be increased. As a result, the steam can be condensed solely by utilizing the cooling effect of the external temperature without using a condenser or a special refrigerant for condensing the steam discharged from the steam outlet 25.

[0140] [Second Cycle Unit]

[0141] Next, refer to Figure 1 The second circulation unit 6 in the microdistillation apparatus 1 will be described. The second circulation unit 6 is a unit for evaporating the mixture discharged from the distillation unit 2 and thereby recirculating the vapor of the mixture to the steam inlet 22 of the distillation unit 2.

[0142] The second circulation unit 6 comprises 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 destination pipe 66.

[0143] The loop piping 65 is used to transport the mixture discharged from the liquid outlet 24 of the distillation unit 2 to the second storage tank 61. In this embodiment, the distillation unit 2 has two liquid outlets 24 (first liquid outlet 24A and second liquid outlet 24B). Therefore, the loop piping 65 is configured to include a first branch pipe 65A and a second branch pipe 65B, such that the mixture discharged from each liquid outlet 24A, 24B is transported to the second storage tank 61. The first branch pipe 65A of the loop piping 65 is liquid-tightly connected to the first liquid outlet 24A of the distillation unit 2 via a connector FT. The second branch pipe 65B is liquid-tightly connected to the second liquid outlet 24B of the distillation unit 2 via a connector FT. The mixture transported from the liquid outlet 24 of the distillation unit 2 through the loop piping 65 is stored in the second storage tank 61.

[0144] The outgoing piping 66 comprises a liquid delivery piping 66A for transporting the mixture stored in the second storage tank 61 to the evaporation unit 70, and a gas delivery piping 66B for transporting the vapor generated by the evaporation unit 70 from the mixture to the steam inlet 22 of the distillation unit 2.

[0145] A second circulation pump 62 is connected to a liquid delivery pipe 66A in the outgoing pipe 66. When the second circulation pump 62 is operating, the mixture LqB stored in the second storage tank 61 is pressurized (e.g., delivered) to the liquid delivery pipe 66A, and the mixture LqB is transported to the evaporation unit 70 through the liquid delivery pipe 66A. The type of second circulation pump 62 is not particularly limited, and examples include syringe pumps, diaphragm pumps, etc.

[0146] The evaporation unit 70 is, for example, a microfluidic device in the form of a chip with micrometer-scale microflow paths 71 formed on a substrate 72. The shape of the substrate 72 in the evaporation unit 70 is not particularly limited; for example, it can be a chip with a rectangular planar shape. Borosilicate glass, which is resistant to organic chemicals and has heat resistance, can be used as the material for the substrate 72 in the evaporation unit 70. Multiple linear microflow paths 71 are arranged side-by-side on the substrate 72 of the evaporation unit 70. The upstream and downstream ends of each microflow path 71 merge at an upstream confluence 73 and a downstream confluence 74. Furthermore, a liquid inlet 75 is formed on the substrate 72 of the evaporation unit 70 in communication with the upstream confluence 73, and a vapor outlet 76 is formed in communication with the downstream confluence 74. The number and arrangement of the microflow paths 71 in the evaporation unit 70 are not particularly limited; for example, the evaporation unit 70 may also have microflow paths 71 extending in a meandering manner.

[0147] The flow path width of the microflow path 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 flow path height of the microflow path 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 flow path length of the microflow path 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.

[0148] The liquid inlet 75 of the evaporation unit 70 is liquid-tightly connected to the liquid delivery pipe 66A via connector FT. Additionally, one end of the gas delivery pipe 66B is airtightly connected to the steam outlet 76 of the evaporation unit 70 via connector FT. The other end of the gas delivery pipe 66B is airtightly connected to the steam inlet 22 of the distillation unit 2 via connector FT. For the evaporation unit 70 configured as described above, the mixed liquid LqB supplied via the liquid delivery pipe 66A is introduced through the liquid inlet 75, and distributed to each microchannel 71 via the upstream confluence section 73.

[0149] Evaporation unit 70 includes an evaporation heater 77, which is used to heat and evaporate the mixture LqB flowing along each microflow path 71 (see reference). Figure 1 The evaporation heater 77 can be any heater capable of evaporating the mixture LqB flowing through each microfluidic path 71; there is no particular limitation. For example, it can be a surface heater disposed on the substrate to cover the top or bottom of each microfluidic path 71. In this way, the mixture LqB flowing into each microfluidic path 71 of the evaporation unit 70 evaporates as it flows through each microfluidic path 71. The vapor generated in each microfluidic path 71 from the mixture merges at the downstream confluence section 74 and is discharged from the vapor outlet 76 to the gas supply pipe 66B. According to the evaporation unit 70, by heating the mixture flowing through the microfluidic path 71 with the heater, the mixture can be appropriately evaporated. It should be noted that the set temperature of the evaporation heater 77 can be set to a temperature higher than the boiling point of the lowest boiling point component contained in the mixture LqB. For example, a temperature of 30°C or higher and 400°C or lower is acceptable, preferably 40°C or higher and 350°C or lower, and more preferably 50°C or higher and 300°C or lower.

[0150] The vapor from the mixture discharged to the gas supply pipe 66B is supplied to the steam inlet 22 of the distillation unit 2 via the gas supply pipe 66B. Here, the gas supply pipe 66B preferably has a heat-insulating function that can keep the vapor from the mixture flowing through it warm and prevent its condensation during transport. Alternatively, the second circulation unit 6 may also have a heat-insulating member 67 for keeping the gas supply pipe 66B warm (see reference). Figure 1 The insulation component 67 is not particularly limited as long as it can suppress the recondensation of the steam transported by the gas supply pipe 66B by insulating the gas supply pipe 66B.

[0151] Microdistillation apparatus 1 is controlled by control device 100 (refer to...) Figure 1 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, and the evaporation heater 77 are all included.

[0152] The control device 100 can be a conventional computer. The control device 100 includes a communication interface (I / F), storage devices, input / output devices, a processor, etc. The communication I / F can be, for example, a network interface card (NIC) or a communication module, which communicates with other computers based on a given protocol. The storage devices can be main storage devices such as RAM (Random Access Memory) and ROM (Read Only Memory), and auxiliary storage devices (secondary storage devices) such as HDD (Hard-Disk Drive), SSD (Solid State Drive), and flash memory. The main storage device temporarily stores programs read by the processor, information sent and received with other computers, or ensures the processor's working area. The auxiliary storage device stores programs executed by the processor, information sent and received with other computers, etc. The input / output devices are, for example, user interfaces such as keyboards, mice, monitors, touch panels, etc. The processor is an arithmetic processing unit such as a CPU (Central Processing Unit) that executes programs. It should be noted that the various devices of the microdistillation apparatus 1 do not need to be controlled by the control device 100; therefore, the control device 100 is an optional element.

[0153] In the microdistillation apparatus 1 configured as described above, during the preparation process before its operation begins, the first storage tank 51 and the second storage tank 61 respectively store the mixture LqA and LqB, which are the objects of distillation. It should be noted that different symbols "LqA" and "LqB" are used here to represent the mixture, which is to distinguish the meaning of the storage location of the mixture. Of course, the composition of the mixture LqA and LqB can be the same.

[0154] Next, the working status (operation status) of the microdistillation apparatus 1 will be described. The operation (running) of the microdistillation apparatus 1 is carried out by the control device 100 controlling the operation of various devices of the microdistillation apparatus 1 (first circulation pump 52, second circulation pump 62, temperature regulating heater 35, evaporation heater 77).

[0155] The microdistillation apparatus 1 separates a specific target component from other components by performing a distillation operation on a mixture containing at least two components with different boiling points.

[0156] When the microdistillation apparatus 1 is in operation, the mixed liquids LqA and LqB stored in the first storage tank 51 in the first circulation unit 5 are transported to the liquid inlet 21 of the distillation unit 2 through the outgoing pipe 56 in the first circulation unit 5.

[0157] Additionally, the mixture LqB stored in the second storage tank 61 of the second circulation unit 6 is transported to the evaporation unit 70 via the liquid delivery pipe 66A. The mixture LqB transported to the evaporation unit 70 is heated by the evaporation heater 77 as it flows through each microfluidic path 71, thus evaporating into vapor derived from the mixture. The vapor derived from the mixture generated by the evaporation unit 70 is then transported to the steam inlet 22 of the distillation unit 2 via the gas delivery pipe 66B while being kept at a constant temperature.

[0158] The mixture LqA introduced from the first liquid inlet 21A and the second liquid inlet 21B in the distillation unit 2 is guided to the first end 23A side of the gas-liquid contact flow path 23 through the first liquid inlet 26A and the second liquid inlet 26B, respectively. Moreover, the mixture flows downward along the liquid flow area RL formed on the flow path wall of the gas-liquid contact flow path 23 toward the second end 23B of the gas-liquid contact flow path 23, which is located vertically downward.

[0159] More specifically, the mixture LqA introduced from the first liquid inlet 21A is guided to the first flow path wall 231 at the first end 23A in the gas-liquid contact flow path 23 via the first liquid inlet 26A. Similarly, the mixture LqA introduced from the second liquid inlet 21B is guided to the second flow path wall 232 at the first end 23A in the gas-liquid contact flow path 23 via the second liquid inlet 26B. 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 positioned vertically upwards, and the second end 23B side is positioned vertically downwards. Therefore, gravity allows the mixture LqA guided to the first flow path wall 231 and the second flow path wall 232 to flow downwards along the surfaces of these flow path walls 231 and 232.

[0160] In this embodiment, the cross-sectional area of ​​the gas-liquid contact flow path 23 is determined such that the entire cross-section of the flow path 23 is not blocked by the mixed liquid LqA flowing through it; in other words, the cross-sectional area of ​​the gas-liquid contact flow path 23 is determined such that a hollow vapor flow area RG remains at the center of its cross-section. As an example, the width of the liquid inlet path 26 and the liquid outlet path 27 in the distillation unit 2 is designed to be approximately 400 μm, and the height is designed to be approximately 2000 μm. Furthermore, the liquid film thickness TH1 of the mixed liquid flowing downwards along the flow path walls 231 and 232 of the gas-liquid contact flow path 23 (refer to...) Figure 4 For example, the design can be made to be tens to hundreds of μm, resulting in excellent discharge of the mixture. Under such design conditions, in order to ensure that the steam flow area RG for the steam to flow in the countercurrent direction toward the vertical direction opposite to the flow direction of the mixture is sufficiently guaranteed, for example, the cross-section of the gas-liquid contact flow path 23 can be suitably set to a square cross-section with a side length of 2 mm.

[0161] On the other hand, the steam from the mixture, which is transported from the second circulation unit 6 to the steam inlet 22 of the distillation unit 2, flows into the gas-liquid contact flow path 23 from the second end 23B side located vertically downward through the steam inlet 28. The steam from the mixture flowing into the gas-liquid contact flow path 23 flows along the gas-liquid contact flow path 23 toward the first end 23A side (i.e., vertically upward) of the gas-liquid contact flow path 23. That is, the steam from the mixture supplied to the distillation unit 2 from the second circulation unit 6 flows through the gas-liquid contact flow path 23 as a countercurrent to the mixture LqA supplied to the distillation unit 2 from the first circulation unit 5.

[0162] As described above, by utilizing gravity to bring the mixture LqA and the vapor from the mixture into countercurrent contact in the gas-liquid contact flow path 23, efficient heat and mass transfer can be achieved between the mixture LqA and the vapor from the mixture. Furthermore, as described above, the distillation unit 2 includes a temperature regulating mechanism 3, which is used to create a given temperature gradient from the second end 23B side of the gas-liquid contact flow path 23 towards the first end 23A side. The control device 100 can create an appropriate temperature distribution from the second end 23B (lower end) side of the gas-liquid contact flow path 23 towards the first end 23A (upper end) side by controlling the temperature regulating heater 35 in the temperature regulating mechanism 3. For example, the temperature of the gas-liquid contact flow path 23 can be controlled such that it is higher than the boiling point of the target component to be separated in the distillation operation and lower than the boiling points of other components.

[0163] As a result, the vapor originating from the mixed liquid flowing from the second end 23B side to the first end 23A side (vertically upward) through the vapor flow area RG of the gas-liquid contact flow path 23 is gradually cooled, and other components in the vapor originating from the mixed liquid with boiling points higher than the target component are condensed. These condensed components, together with the mixed liquid LqA flowing from the first end 23A side of the gas-liquid contact flow path 23, flow downwards along the liquid flow area RL (flow path walls 231, 232). On the other hand, the target component contained in the vapor originating from the mixed liquid is discharged from the vapor outlet 25 through the vapor outlet path 29 while remaining in the vapor phase.

[0164] Furthermore, for the mixture LqA flowing downward along the liquid flow region RL (flow path walls 231, 232) of the gas-liquid contact flow path 23, the temperature gradually increases as it approaches the second end 23B of the gas-liquid contact flow path 23. Therefore, during this process, the target component contained in the mixture LqA undergoes a phase change to vapor. Thus, the vapor of the target component flows through the vapor flow region RG and is discharged from the vapor outlet 25 through the vapor outlet 29. In addition, in the mixture LqA flowing downward along the liquid flow region RL (flow path walls 231, 232), other components with boiling points higher than the target component concentrate and reach the second end 23B of the gas-liquid contact flow path 23, and are discharged from the liquid outlet 24 (first liquid outlet 24A, second liquid outlet 24B) through the liquid outlet 27.

[0165] The steam (concentrated steam of the target component) from the steam outlet 25 of the distillation unit 2, originating from the mixture, is cooled and condensed as it flows through the loop piping 55 of the first circulation unit 5. The resulting condensate is stored in the first storage tank 51. That is, the condensate transported through the loop piping 55 of the first circulation unit 5 is mixed with the mixture LqA stored in the first storage tank 51 and then recirculated to the liquid inlet 21 of the distillation unit 2 through the outgoing piping 56.

[0166] Additionally, the mixture discharged from the liquid outlet 24 of the distillation unit 2 (a concentrated mixture of components other than the target component) is stored in the second storage tank 61 via the loop piping 65 of the second circulation unit 6. That is, after the mixture discharged from the liquid outlet 24 of the distillation unit 2 (a concentrated mixture of components other than the target component) is mixed with the mixture LqB stored in the second storage tank 61, it is transported to the evaporation unit 70 via the liquid delivery piping 66A, and after phase transformation into steam, it is recycled back to the steam inlet 22 of the distillation unit 2.

[0167] The microdistillation apparatus 1 continuously (persistently) performs cycles using the first circulation unit 5 and the second circulation unit 6 under its steady-state operation. As a result, a concentrated mixture of the target component can be stored in the first storage tank 51 (also called a reflux tank) of the microdistillation apparatus 1. That is, the concentrated mixture of the target component can be suitably recovered from the first storage tank 51 (reflux tank). Furthermore, a concentrated mixture of components other than the target component can be stored in the second storage tank 61 (also called a bottom discharge tank). Therefore, a concentrated mixture of components other than the target component can be suitably recovered from the second storage tank 61 (bottom discharge tank). Here, the higher the concentration of the target component in the mixture recovered from the first storage tank 51 and the lower the concentration of the target component in the mixture recovered from the second storage tank 61 (the higher the concentration of components other than the target component), the more efficient the distillation-based separation operation using the microdistillation apparatus 1 is considered. Furthermore, the microdistillation apparatus 1 of this embodiment achieves countercurrent gas-liquid contact utilizing gravity in the gas-liquid contact flow path 23, thereby enabling efficient and good contact between the steam rising vertically upward in the steam flow region RG and the mixed liquid flowing vertically downward in the liquid flow region RL, with the flow path walls 231 and 232 serving as wetting walls. This promotes heat and mass transfer between the gas and liquid. As a result, the target component and other components contained in the mixed fluid (mixture and steam) can be efficiently separated.

[0168] Furthermore, the microdistillation apparatus 1 continuously circulates the concentrated mixture of the target component to the distillation unit 2 via the first circulation unit 5. Additionally, the concentrated mixture of other components besides the target component is continuously circulated to the distillation unit 2 via the second circulation unit 6. The microdistillation apparatus 1 can perform continuous distillation using circulation units 5 and 6, which utilize these two systems. That is, the vapor obtained by evaporating the concentrated mixture of the target component and the concentrated mixture of other components can be continuously and repeatedly circulated to the distillation unit 2, and gas-liquid contact occurs in the gas-liquid contact flow path 23, thus improving the separation degree of the target component from other components in the mixed fluid (mixture and vapor).

[0169] Furthermore, the distillation unit 2 of this embodiment, as described above, has multiple liquid inlets 21A and 21B. Moreover, the mixture can be guided to the liquid flow area RL of the gas-liquid contact flow path 23 via multiple liquid inlet paths 26A and 26B corresponding to each liquid inlet 21A and 21B. This appropriately ensures the flow rate of the mixture in the gas-liquid contact flow path 23. At this time, by configuring the mixture introduced from each liquid inlet path 26A and 26B to different flow path walls 231 and 232 forming the gas-liquid contact flow path 23, obstruction of steam flow in the steam flow area RG of the gas-liquid contact flow path 23 can be suppressed, and the flow rate of the mixture can also be ensured.

[0170] Furthermore, since the liquid inlet path 26 of the distillation unit 2 is formed as a microflow path, a suitable flow rate of the mixture can be supplied to the gas-liquid contact flow path 23 through the liquid inlet path 26. As a result, the liquid film thickness of the mixture flowing downward along the flow path walls 231, 232 (liquid flow area RL) in the gas-liquid contact flow path 23 can be easily controlled to the micrometer scale. In addition, since the liquid outlet path 27 of the distillation unit 2 is formed as a microflow path, the flow path for discharging the mixture flowing downward along the flow path walls 231, 232 (liquid flow area RL) with a liquid film thickness on the micrometer scale can be set to an appropriate size.

[0171] Furthermore, the distillation unit 2 includes a temperature control mechanism 3, which comprises a temperature control heater 35 and heat-conducting members 31-34 for transferring heat from the temperature control heater 35 to the substrate B. This mechanism enables the formation of a given temperature gradient (temperature distribution) in the gas-liquid contact flow path 23, with the temperature gradually decreasing from the second end 23B (lower end) to the first end 23A (upper end). Therefore, even under conditions where the temperature environment of the gas-liquid contact flow path 23 is easily affected by external air temperature due to its small volume, a suitable temperature environment can be formed in the gas-liquid contact flow path 23, allowing for appropriate distillation operations to be performed in the distillation unit 2. More specifically, it allows for the separation of low-boiling-point and high-boiling-point components without condensing all the vapor flowing through the vapor flow area RG in the gas-liquid contact flow path 23, and is suitable for separation based on countercurrent gas-liquid contact. In this embodiment, a temperature regulating mechanism 3 is preferably used to control the temperature in such a way that the temperature at each point pre-set along the axial direction (extension direction) of the gas-liquid contact flow path 23 becomes a given temperature.

[0172] Furthermore, conventional distillation columns, due to their complex structures, sometimes make it difficult to ascertain the internal flow state and the occurrence of adverse conditions (such as flow deviation in packed columns, polymer-induced blockage, flooding, and weeping). In contrast, the temperature control mechanism 3 of this embodiment forms gaps (visual identification slits) SL extending in the vertical direction between the first heat-conducting member 31 and the second heat-conducting member 32, and between the third heat-conducting member 33 and the fourth heat-conducting member 34. Therefore, even during the operation of the microdistillation apparatus 1, the condition of the gas-liquid contact flow path 23 can be observed visually in real time through the aforementioned gaps SL, enabling visualization of the flow rate of the mixture and vapor flowing through the gas-liquid contact flow path 23.

[0173] It should be noted that the working time (running time) of the microdistillation device 1 is not particularly limited and can be set freely.

[0174] Furthermore, it can be considered that in the microdistillation apparatus 1, regarding the container capacities of the first storage tank 51 and the second storage tank 61, if these container capacities are too large, the time required for the concentration of the mixture stored in each storage tank 51, 61 to stabilize (reach its final state) will be longer. On the other hand, if the container capacities are too small, it will be difficult to operate stably and continuously. It is preferable to design the container capacities of the first storage tank 51 and the second storage tank 61 from these perspectives. For example, the capacity of the first storage tank 51 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. 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.

[0175] Furthermore, regarding the delivery volume of the mixture supplied by the first circulation pump 52 and the second circulation pump 62, if the delivery volume is too low, there is a risk that the time required for the concentration of the mixture stored in each storage tank 51 and 61 to reach its final state will be prolonged. Additionally, the delivery volume of the first circulation pump 52 and the second circulation pump 62 is preferably determined in a way that keeps the liquid level in each storage tank 51 and 61 essentially unchanged and stable during the operation of the microdistillation apparatus 1. Furthermore, if the delivery volume of the second circulation pump 62 is too high (the delivery rate is too fast), it will exceed the vaporization / evaporation capacity of the mixture in the evaporation unit 70, posing a risk that liquid may be introduced into the steam inlet 22 of the distillation unit 2. The delivery volumes of the first circulation pump 52 and the second circulation pump 62 are preferably designed with these considerations in mind. For example, an example is a method in which the flow rate of the mixture delivered by the first circulation pump 52 is 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. Similarly, an example is a method in which the flow rate of the mixture delivered by the second circulation pump 62 is 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.

[0176] Furthermore, the microdistillation apparatus 1 of this embodiment can perform distillation (rectification) operations on mixtures of three or more components with different boiling points. The following description describes the distillation operation on a mixture of two components (a low-boiling-point component and a high-boiling-point component). In this case, for the vapor supplied to the distillation unit 2 via the second circulation unit 6 from the mixture containing both low-boiling-point and high-boiling-point components, as the vapor flows from the second end 23B side to the first end 23A side (vertically upward) in the vapor flow area RG of the gas-liquid contact flow path 23, the high-boiling-point component is condensed. The condensate of the high-boiling-point component, together with the mixture flowing from the first end 23A side of the gas-liquid contact flow path 23, flows downward along the liquid flow area RL (flow path walls 231, 232) and is finally discharged from the liquid outlet 24. Moreover, the vapor, whose concentration of the low-boiling-point component has been increased by separating it from the high-boiling-point component, is discharged from the steam outlet 25 via the steam outlet path 29.

[0177] Furthermore, for the mixture containing low-boiling-point and high-boiling-point components supplied to the distillation unit 2 via the first circulation unit 5, the low-boiling-point components transform into vapor as they flow downwards along the liquid flow area RL (flow path walls 231, 232) of the gas-liquid contact flow path 23. This low-boiling-point vapor, along with the vapor flowing upwards through the vapor flow area RG, is discharged from the steam outlet 25 via the steam outlet path 29. On the other hand, the high-boiling-point components contained in the mixture supplied to the distillation unit 2 via the first circulation unit 5 are concentrated as they flow downwards along the liquid flow area RL (flow path walls 231, 232). After reaching the second end 23B of the gas-liquid contact flow path 23 in this state, they are discharged from the liquid outlet 24 via the liquid outlet path 27. By continuously performing this distillation operation, a mixture with increased low-boiling-point component concentration is stored in the first storage tank 51 (reflux tank), and a mixture with increased high-boiling-point component concentration is stored in the second storage tank 61 (bottom discharge tank). That is, the mixture with improved purity of both low-boiling-point and high-boiling-point components can be stored in storage tanks 51 and 61 for recycling.

[0178] <Example>

[0179] The present disclosure will now be described in detail with reference to the embodiments. However, the present disclosure is not limited to the embodiments described below.

[0180] In the embodiments, references are used. Figures 1-5 The microdistillation apparatus 1, as described, was used to perform total reflux distillation on a mixture containing acetic acid and ethyl acetate.

[0181] The operation of the microdistillation apparatus 1 is carried out in the following state: the distillation unit 2 is arranged such that the first end 23A side of the gas-liquid contact flow path 23 in the distillation unit 2 is arranged on the upper side (upward) in the vertical direction and the second end 23B side is arranged on the lower side (downward) in the vertical direction.

[0182] The apparatus used in the embodiments is described below.

[0183] • Circulation pump (liquid delivery pump): Smoothflow Pump Q model Q1-5-KR-UP-S-IMTT (manufactured by TACMINA)

[0184] Distributor: Standard chip ICC-SY500 (manufactured by Microchemical Technology Co., Ltd.)

[0185] • Circulation tubing: Polyetheretherketone tubing (inner diameter 260 μm, manufactured by Microchemical Technology Co., Ltd.)

[0186] • Storage Tank 1 (Reflux Tank): Capacity 0.6 mL (manufactured by Nippon Rikka Glass Co., Ltd.)

[0187] • Second storage tank (bottom discharge tank): Capacity 0.6 mL (manufactured by Nippon Electric Industrial Co., Ltd.)

[0188] • Temperature control heater, evaporation heater: 2cm×2cm type (manufactured by Miyo Technology Co., Ltd.)

[0189] • Evaporation heater: IACF-THT03050 (manufactured by TAIYA International Technology Co., Ltd.)

[0190] [Evaporation Unit]

[0191] The evaporation unit 70 uses a device in which 10 microchannels 71 are arranged side by side on a substrate 72. Each microchannel 71 is configured with a channel width of 150 μm, a channel height (depth) of 50 μm, and a channel length of 60 mm. The substrate 72 is made of borosilicate glass.

[0192] [Distillation Unit]

[0193] The substrate B of distillation unit 2 is made of borosilicate glass. In addition, the substrate B of distillation unit 2 has a width of 30 mm and a height of 70 mm.

[0194] The cross-section of the gas-liquid contact flow path 23 is set as a square cross-section with a side length of 2mm, and the flow path length ( Figure 6 The symbol LT in the figure is set to 50 mm. In addition, the liquid inlet path 26 and the liquid outlet path 27 are formed as microflow paths with a flow path width of 400 μm and a flow path height (depth) of 2000 μm (2 mm).

[0195] The thickness of the liquid film of the mixture flowing downward on the flow path wall of the gas-liquid contact flow path 23 is adjusted to be in the range of tens to hundreds of μm.

[0196] [Operating and Distillation Conditions]

[0197] The specific operations and distillation conditions in the examples are shown in Table 1.

[0198] As a preparatory step before starting the distillation operation based on the microdistillation device 1, the mixture is contained in the first storage tank 51 (reflux tank) and the second storage tank 61 (bottom discharge tank).

[0199] The first storage tank 51 (reflux tank) contains 100 μL of a mixture, which is a mixture of acetic acid and ethyl acetate mixed with ethyl acetate in such a way that the acetic acid concentration is 30.0% by mass.

[0200] The second storage tank 61 (bottom discharge tank) contains 100 μL of a mixture of acetic acid and ethyl acetate mixed in such a manner that the acetic acid concentration is 30.0% by mass.

[0201] It should be noted that acetic acid and ethyl acetate manufactured by Honeywell were used in the examples.

[0202] In the distillation operation of this embodiment, the first circulation pump 52, the second circulation pump 62, the temperature control heater 35, and the evaporation heater 77 in the microdistillation apparatus 1 are operated to deliver the mixtures stored in the first storage tank 51 (reflux tank) and the second storage tank 61 (bottom discharge tank) to the distillation unit 2 at the flow rates shown in Table 1. After the operating time (experimental time) shown in Table 1 has elapsed since the start of operation, the operation of the microdistillation apparatus 1 is stopped.

[0203] It should be noted that during the operation of the microdistillation apparatus 1, the temperatures at each temperature measurement point T1 to T5 in the gas-liquid contact flow path 23 of the distillation unit 2 were measured (specifically, the surface temperatures of the substrate (glass) at each temperature measurement point T1 to T5), and the measured results are shown in Table 1. Figure 6 This diagram illustrates temperature measurement points T1 to T5. Each temperature measurement point T1 to T5 is spaced apart along the axial direction of the gas-liquid contact flow path 23. Each temperature measurement point T1 to T5 is located on the axis of the gas-liquid contact flow path 23. Temperature measurement point T1 is located at the first end 23A (upper end) of the gas-liquid contact flow path 23, where the gas-liquid contact flow path 23 merges with the liquid inlet path 26 (26A, 26B). Temperature measurement point T5 is located at the second end 23B (lower end) of the gas-liquid contact flow path 23, where the gas-liquid contact flow path 23 branches off from the liquid outlet path 27 (27A, 27B). Temperature measurement point T3 is located on the axis of the gas-liquid contact flow path 23, precisely at the center of temperature measurement points T1 and T5. Temperature measurement point T2 is set between temperature measurement points T1 and T3, and is located 10 mm away from temperature measurement point T1 towards T3. Temperature measurement point T4 is set between temperature measurement points T5 and T3, and is located 10 mm away from temperature measurement point T5 towards T3. Figure 6 The symbols L1 to L4 represent the spacing between temperature measurement points along the axial direction of the gas-liquid contact flow path 23. In this embodiment, L1 and L4 are set to 10 mm, and L2 and L3 are set to 15 mm. It should be noted that 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.

[0204] For Examples 1-3 with different distillation conditions, distillation operations were performed respectively, and the concentrations of ethyl acetate and acetic acid in the recovered mixture in the first storage tank 51 (reflux tank), the concentrations of ethyl acetate and acetic acid in the recovered mixture in the second storage tank 61 (bottom discharge tank), the number of theoretical plates, and the height equivalent of one theoretical plate (HETP) were determined respectively. The results of each example are shown in Table 2.

[0205] The methods for determining the concentrations of acetic acid and ethyl acetate in the reflux liquid and bottom discharge liquid obtained in each embodiment are as follows.

[0206] [Method for determining acetic acid concentration]

[0207] The acetic acid concentration was determined by titration analysis based on a 0.05 mol / L sodium hydroxide aqueous solution, calculated according to the neutralization point of pH change. The determination conditions are as follows.

[0208] • Titration reagent: 0.05 mol / L sodium hydroxide aqueous solution (Honeywell Corporation)

[0209] • Measuring instrument: pH meter model PB-10 (manufactured by Sartorius)

[0210] • Measurement temperature: 25℃ (room temperature)

[0211] [Method for determining the concentration of ethyl acetate]

[0212] The ethyl acetate concentration is calculated as the difference between 100% by mass and the acetic acid concentration.

[0213]

[0214]

[0215] [Comparative Example]

[0216] Next, the comparative examples will be explained. The comparative examples use... Figure 7 The experimental setup shown in the flask was used to perform total reflux distillation of acetic acid (99.7 wt; manufactured by Fujifilm and Kohden Chemical Co., Ltd.) and ethyl acetate (99.9 GC area; manufactured by Daicel Co., Ltd.).

[0217] The apparatus used in the comparative example is described below.

[0218] • Flask capacity 3L (manufactured by Asahi Manufacturing Co., Ltd.)

[0219] • Filling tower (manufactured by Asahi Manufacturing Co., Ltd.)

[0220] • Condenser (manufactured by Asahi Manufacturing Co., Ltd.)

[0221] In the comparative distillation operation, the flask was connected to a packed column located at the top. The packed column had structured packing (Sulzer EX laboratory packing, 50 mm inner diameter, 55 mm packing length; Sulzer Chemtech Ltd.) and a dispersion plate. The upper part of the packed column was connected to a gas flow tube, the upper part of which was connected to a condenser. Furthermore, in the comparative distillation operation, the flask was heated by an oil bath to vaporize the mixture inside, and the gas flowing through the gas flow tube was cooled by the condenser, thus condensing the mixture.

[0222] [Operating and Distillation Conditions]

[0223] The specific operations and distillation conditions in the comparative examples are shown in Table 3.

[0224] As a preparatory step before starting the distillation operation of the comparative example, a mixture of ethyl acetate was filled into a 2.9L flask to make the acetic acid concentration 30.0% by mass.

[0225] Then, for Comparative Examples 1-3 (refer to Table 3) with different distillation conditions, total reflux distillation was performed on the mixture of acetic acid and ethyl acetate, and the oil bath temperature was adjusted to achieve a given reflux flow rate. Samples were then taken from the reflux and the mixture in the flask, and the concentrations of ethyl acetate and acetic acid in the reflux, the concentrations of ethyl acetate and acetic acid in the mixture in the flask, the theoretical plate number, and the height of equal plates (HETP) were determined. The results for each comparative example are shown in Table 4.

[0226] The methods for determining the concentrations of acetic acid and ethyl acetate in the reflux liquid and the mixture in the flask obtained in each comparative example are described below. It should be noted that the ethyl acetate concentration is calculated as the difference between 100% by mass and the acetic acid concentration.

[0227] [Method for determining the concentration of acetic acid in reflux solution]

[0228] The acetic acid concentration was determined by titration analysis based on a 0.1 mol / L potassium hydroxide aqueous solution (manufactured by Fujifilm and Kojun Chemical Co., Ltd.), and calculated based on the neutralization point of the color change. The determination conditions are as follows.

[0229] • Titration reagent: 0.1 mol / L potassium hydroxide aqueous solution (manufactured by Fujifilm and Wako Pure Chemical Industries, Ltd.)

[0230] • Indicator: 1.0 w / v phenolphthalein / ethanol (90) solution (Fujifilm and Waku Pure Chemical Industries, Ltd.)

[0231] Solvent: 99.7% by weight 2-propanol (Fujifilm and Wako Pure Chemical Industries, Ltd.)

[0232] • Measurement temperature: 25℃ (room temperature)

[0233] [Method for determining the concentration of acetic acid in the mixture within the flask]

[0234] The determination conditions for gas chromatography (GC) are as follows.

[0235] • Apparatus: Gas chromatograph (manufactured by Agilent Technologies)

[0236] • Detector: Thermal conductivity detector (manufactured by Agilent Technologies)

[0237] • Column: DB-WAX (Column dimensions: length 60m, inner diameter: 0.53mm, film thickness: 1.0μm, manufactured by Agilent Technologies)

[0238] • Vaporization chamber temperature: 180℃

[0239] • Temperature increase: 100℃, hold for 10 minutes → 10℃ / min → 200℃, hold for 10 minutes

[0240] Carrier gas: He

[0241] • Flow split ratio: 20:1

[0242] Total flow rate: 87 ml / min

[0243] Injection volume: 1 μL

[0244] Internal standard: 1,4-dioxane

[0245] Analysis time: 30 minutes

[0246]

[0247]

[0248] Then, comparing the results of the Examples (Table 2) and Comparative Examples (Table 4), it can be seen that the Examples have a larger theoretical plate number than the Comparative Examples. Therefore, it can be concluded that the Examples have superior separation efficiency compared to the Comparative Examples. Furthermore, compared to the Comparative Examples, the Examples can reduce the height-to-plate (HETP), indicating that the Examples have higher separation performance than the Comparative Examples.

[0249] <Implementation Method 2>

[0250] Next, Embodiment 2 of the microdistillation apparatus will be described.

[0251] Figure 8 This is a diagram illustrating the microdistillation apparatus 1A of Embodiment 2. For Figure 8 Regarding the microdistillation apparatus 1A shown, the structure of the distillation unit 2A is similar to... Figure 1 The distillation unit 2 shown is different. Hereinafter, the description will focus on the differences between embodiments 1 and 2, with the same reference numerals used for common structures, and detailed descriptions will be omitted.

[0252] In addition to the liquid inlet 21 located at the first end 23A of the gas-liquid contact flow path 23, the distillation unit 2A of embodiment 2 further has an intermediate inlet 80 for introducing additional mixed liquid at the middle position of the gas-liquid contact flow path 23. Figure 8 In the example shown, the first intermediate inlet 80A and the second intermediate inlet 80B are located in the distillation unit 2A. Furthermore, the distillation unit 2A is provided with an intermediate inlet path 81 connecting the intermediate inlet 80 and the gas-liquid contact flow path 23. Figure 8 In the example shown, the first intermediate inlet path 81A connects the first intermediate inlet port 80A to the gas-liquid contact flow path 23, and the second intermediate inlet path 81B connects the second intermediate inlet port 80B to the gas-liquid contact flow path 23. Furthermore, the first intermediate inlet path 81A opens onto the wall 231 of the first flow path, and the second intermediate inlet path 81B opens onto the wall 232 of the second flow path.

[0253] like Figure 8 As shown, the microdistillation apparatus 1A includes an additional supply unit 90 for supplying an additional mixture to the intermediate position of the gas-liquid contact flow path 23. The additional supply unit 90 comprises a delivery conduit 91, a third storage tank 92, a delivery pump 93, a distributor 94, etc. The delivery conduit 91 is a pipe used to transport (supply) the additional mixture stored in the third storage tank 92 to the intermediate inlet 80 of the distillation unit 2A. The type of delivery pump 93 is not particularly limited; examples include syringe pumps and diaphragm pumps.

[0254] The liquid delivery 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 branching off 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 in the distillation unit 2A. One end of the second branch pipe 91C is connected to the distributor 54, and the other end is connected to the second intermediate inlet 80B in the distillation unit 2A.

[0255] A liquid delivery pump 93 is connected to the main pipe 91A in the liquid delivery conduit 91. When the liquid delivery pump 93 is working, the mixture stored in the third storage tank 92 is pressurized and delivered to the main pipe 91A. The mixture is supplied to the first intermediate inlet 80A in the distillation unit 2A through the first branch pipe 91B, and to the second intermediate inlet 80B in the distillation unit 2A through the second branch pipe 91C.

[0256] In addition, such as Figure 8 As shown, the microdistillation apparatus 1A includes a first mixture discharge unit 200 and a second mixture discharge unit 300. The first mixture discharge unit 200 includes a first delivery conduit 210, a first delivery pump 220, and a first recovery tank 230. The first delivery conduit 210 connects the first storage tank 51 and the first recovery tank 230, and the first delivery pump 220 is connected midway through the first delivery conduit 210. Similarly, the second mixture discharge unit 300 includes a second delivery conduit 310, a second delivery pump 320, and a second recovery tank 330. The second delivery conduit 310 connects the second storage tank 61 and the second recovery tank 330, and the second delivery pump 320 is connected midway through the second delivery conduit 310. When the first delivery pump 220 operates, the mixture stored in the first storage tank 51 is delivered to the first recovery tank 230 through the first delivery conduit 210 and stored therein. Similarly, when the second delivery pump 320 operates, the mixture stored in the second storage tank 61 is delivered to the second recovery tank 330 through the second delivery conduit 310 and stored therein. In this embodiment, for example, the first delivery pump 220 and the second delivery pump 320 can operate continuously.

[0257] The types of the first liquid delivery conduit 210 and the second liquid delivery conduit 310 are not particularly limited; for example, PEEK tubing may be preferred. Furthermore, the types of the first liquid delivery pump 220 and the second liquid delivery pump 320 are not particularly limited; examples include syringe pumps and diaphragm pumps.

[0258] As described above, since the first intermediate inlet channel 81A opens onto the first flow path wall 231 and the second intermediate inlet channel 81B opens onto the second flow path wall 232, the mixture transported by the additional supply unit 90 can be continuously supplied from the side to the gas-liquid contact flow path 23. That is, the additional mixture introduced from the first intermediate inlet channel 81A can be merged with the mixture flowing down from the first end 23A side of the gas-liquid contact flow path 23 along the first flow path wall 231. Similarly, the additional mixture introduced from the second intermediate inlet channel 81B can be merged with the mixture flowing down from the first end 23A side of the gas-liquid contact flow path 23 along the second flow path wall 232. Furthermore, since the continuous supply of the mixture via the additional supply unit 90 increases the liquid capacity of the first storage tank 51, the mixture can be continuously discharged from the first storage tank 51 via the first mixture discharge unit 200 in a manner that keeps the liquid level in the first storage tank 51 constant. Similarly, since the continuous supply of the mixture via the additional supply unit 90 increases the liquid capacity of the second storage tank 61, the mixture can be continuously discharged from the second storage tank 61 via the second mixture discharge unit 300 in a manner that keeps the liquid level in the second storage tank 61 constant. That is, by continuously supplying the mixture using the additional supply unit 90 and continuously discharging the mixture using the first mixture discharge unit 200 and the second mixture discharge unit 300, a mixture with concentrated low-boiling-point components and a mixture with concentrated high-boiling-point components can be continuously obtained, respectively. Of course, in the microdistillation apparatus 1A of Embodiment 2, the first circulation pump 52 and the second circulation pump 62 are operated continuously, just as in the microdistillation apparatus 1 described in Embodiment 1.

Claims

1. A microdistillation apparatus, comprising: a distillation unit, a first circulation unit, and a second circulation unit, The distillation unit includes: A liquid inlet for introducing a mixture containing at least two components with different boiling points. Steam inlets from the mixture are introduced separately. A gas-liquid contact flow path in which the mixture introduced from the liquid inlet and the vapor derived from the mixture introduced from the steam inlet come into contact in a countercurrent manner. The liquid outlet that discharges the mixture flowing through the gas-liquid contact flow path, and The vapor outlet discharges the vapor originating from the mixed liquid that flows through the gas-liquid contact flow path. The first circulation unit circulates condensate to the liquid inlet, the condensate being obtained by condensing steam originating from the mixture discharged from the steam outlet. The second circulation unit circulates steam to the steam inlet, the steam being obtained by evaporating the mixture discharged from the liquid outlet.

2. The microdistillation apparatus according to 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 of the gas-liquid contact flow path is positioned on the upper side in the vertical direction, and the liquid inlet and the vapor outlet are disposed on this end side. The other end of the gas-liquid contact flow path is located on the lower side in the vertical direction, and the liquid outlet and the steam inlet are provided on this other end.

3. The microdistillation apparatus according to claim 1 or 2, wherein, In the distillation unit, the mixture introduced from the liquid inlet flows downward in the liquid flow area, and the steam supplied from the mixture from the steam inlet flows in the opposite direction to the mixture along the steam flow area. The liquid flow area is formed along the flow path wall that forms the gas-liquid contact flow path, and the steam flow area is formed on the central side of the cross-section of the gas-liquid contact flow path.

4. The microdistillation apparatus according to claim 3, wherein, The distillation unit has multiple liquid inlets and multiple liquid outlets.

5. The microdistillation apparatus according to claim 4, wherein, The flow path wall in the distillation unit includes a first surface and a second surface that is different from the first surface. The plurality of liquid inlets include a first and a second liquid inlet disposed at one end of the gas-liquid contact flow path. The plurality of liquid outlets include a first and a second liquid outlet disposed at the other end of the gas-liquid contact flow path. The mixture introduced from the first liquid inlet flows downwards along the first surface of the flow path wall and is then discharged from the first liquid outlet. The mixture introduced from the second liquid inlet flows downward on the second surface of the flow path wall and is then discharged from the second liquid outlet.

6. The microdistillation apparatus according to claim 2, wherein, In addition to the liquid inlet located at one end of the gas-liquid contact flow path, the distillation unit further has an intermediate inlet for introducing the mixture into the middle of the gas-liquid contact flow path.

7. The microdistillation apparatus according to claim 1 or 2, wherein, The first circulation unit has a first storage tank for storing condensate, which is obtained by condensing steam derived from the mixture discharged from the steam outlet.

8. The microdistillation apparatus according to claim 1 or 2, wherein, The second circulation unit has a second storage tank for storing a mixture discharged from the liquid outlet of the distillation unit.

9. The microdistillation apparatus according to claim 1 or 2, wherein, The second circulation unit further includes an evaporation unit having: a microflow path for circulating the mixture discharged from the liquid outlet of the distillation unit, and an evaporation heater for evaporating the mixture flowing through the microflow path.

10. The microdistillation apparatus according to claim 1 or 2, wherein, The distillation unit further includes a temperature regulation mechanism for forming a given temperature gradient in which the temperature gradually decreases from one end of the gas-liquid contact flow path to the other.

11. The microdistillation apparatus according to claim 2, wherein, In the distillation unit, a liquid inlet path and a liquid outlet path are formed in the form of microflow paths. The liquid inlet path connects one end of the gas-liquid contact flow path to the liquid inlet, and the liquid outlet path connects the other end of the gas-liquid contact flow path to the liquid outlet.

12. The microdistillation apparatus according to claim 3, wherein, The liquid film thickness of the mixture flowing downward along the wall of the flow path is on the order of micrometers.

13. A distillation method, the method comprising: The microdistillation apparatus of claim 1 is used to distill a mixture containing at least two components with different boiling points.

14. The distillation method according to claim 13, wherein, The mixture contains a given low-boiling-point component and a high-boiling-point component with a higher boiling point compared to the low-boiling-point component. In the distillation unit, the mixture introduced from the liquid inlet and the vapor derived from the mixture introduced from the vapor inlet are brought into countercurrent contact in the gas-liquid contact flow path, thereby achieving [the desired effect]. The low-boiling-point component of the liquid phase is discharged from the steam outlet together with steam from the mixture introduced from the steam inlet. The low-boiling-point component of the liquid phase is obtained by evaporating the low-boiling-point component contained in the mixture. The high-boiling-point component of the liquid phase is discharged from the liquid outlet together with the mixture introduced from the liquid inlet. The high-boiling-point component of the liquid phase is obtained by condensing the high-boiling-point component contained in the vapor derived from the mixture in the gas-liquid contact flow path. The first circulation unit continuously circulates condensate to the liquid inlet, which is obtained by condensing concentrated steam containing the low-boiling-point components discharged from the steam outlet of the distillation unit. The second circulation unit continuously circulates steam to the steam inlet, which is obtained by evaporating a concentrated mixture of high-boiling-point components discharged from the liquid outlet of the distillation unit. Thus, the low-boiling-point components and the high-boiling-point components contained in the mixture are separated.

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