Washing device and extraction device

By using a pressurized gas supply component and a small-diameter device design in a microreactor, the problems of high cost and low extraction efficiency of the microreactor when the production volume is expanded are solved, and low-cost and simple extraction of the extraction target substance and pollution control are achieved.

CN120603632APending Publication Date: 2025-09-05USHIO CHEMIX CORP
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Patent Information

Application Number
CN202480009904.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Priority Date
2023-01-31
Filing Date
2024-01-30
Publication Date
2025-09-05

AI Technical Summary

Technical Problem

Existing microreactors have problems such as high manufacturing cost, low extraction efficiency and high pollution risk when expanding production volume. In particular, the plug flow is unstable when using a pulsating pump, making it difficult to achieve low-cost scale-up.

Method used

The device design combines a pressurized gas supply component with a small-diameter portion. By connecting the extraction units in series or parallel, the pressurized gas supply component is used instead of an expensive pump. Combined with the small-diameter portion to control the flow rate, efficient mixing and extraction of the liquid raw material and the solvent is achieved.

Benefits of technology

The invention realizes low-cost and simple extraction of the extraction target substance from the liquid raw material, reduces the manufacturing cost and pollution risk of the device, and improves the extraction efficiency and stability.

✦ Generated by Eureka AI based on patent content.

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Abstract

Provided is a device capable of more easily extracting a substance to be extracted contained in a liquid starting material. The apparatus for extracting a substance to be extracted dissolved in a liquid raw material includes a raw material tank, a solvent tank, a pressurized gas supply means for supplying a pressurized gas to the solvent tank, a small-diameter portion, an extraction unit including a mixer, an extraction portion, and a separation portion, a first recovery tank, and a second recovery tank.
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Description

Technical Field

[0001] The present invention relates to an apparatus for extracting a substance to be extracted dissolved in a liquid raw material, and more particularly to a washing apparatus for extracting a pollutant dissolved in the liquid raw material and an extraction apparatus for extracting a target substance dissolved in the liquid raw material. Background Art

[0002] As an apparatus for performing reactions such as chemical and biochemical reactions, for example, a microreactor can be used.

[0003] Microreactors have attracted attention as a replacement for conventional batch reactors, and various research projects are underway. A microreactor is a general term for flow-type reaction devices in which the spatial scale of a reaction system for performing chemical / biochemical reactions is, for example, on the order of micrometers. A microreactor has a transport path for the substances being reacted. The inner diameter of this transport path is, for example, on the order of micrometers. Microreactors enable efficient mixing and reaction of multiple substances. Furthermore, reactions can be carried out uniformly at a constant temperature. Consequently, microreactors can improve reaction selectivity and increase reaction rate. Furthermore, microreactors are generally considered easier to transition from laboratory-level to production processes than conventional batch reactors. However, microreactors have high manufacturing costs and numerous technical challenges. Consequently, few microchemical equipment for production purposes has been realized.

[0004] Generally speaking, microreactors have lower production capacity than conventional batch reactors. To increase production capacity in microchemical equipment, research is underway into scaling up. Scaling up involves connecting multiple microreactors in parallel.

[0005] Scale-up can be achieved by connecting multiple identical devices, including pumps, in parallel. This scale-up approach has the disadvantage of increasing device manufacturing costs. However, this method can be easily transferred from the laboratory to the production process without changing reaction conditions, making it easy to industrialize.

[0006] Patent Document 1 describes a method for increasing the number of branched flow paths. This method involves distributing a liquid raw material fed from a pump to a plurality of branched flow paths and arranging mixers in parallel.

[0007] Patent Document 2 describes a method for uniformly distributing a liquid to a plurality of microreactors without using branched pipes.

[0008] Patent Document 3 describes a microchannel reactor composed of a plurality of stacked flow channel units.

[0009] Patent Document 4 describes a microreactor aimed at reducing the cost and miniaturization of microchemical equipment.

[0010] Patent Document 5 describes a micro-chemical equipment including a transfer unit that transfers a liquid raw material using gas pressure.

[0011] Patent Document 6 describes a mixer-settler including a mixing section for mixing a plurality of liquids and a separation tank for storing and separating the plurality of liquids mixed in the mixing section.

[0012] Prior art literature

[0013] Patent Literature

[0014] Patent Document 1: Japanese Patent Application Laid-Open No. 2007-136253

[0015] Patent Document 2: Japanese Patent Application Laid-Open No. 2011-36773

[0016] Patent Document 3: Japanese Patent Application Laid-Open No. 2014-217823

[0017] Patent Document 4: Japanese Patent Application Laid-Open No. 2010-94660

[0018] Patent Document 5: Japanese Patent No. 6618997

[0019] Patent Document 6: Japanese Patent Application Laid-Open No. 2022-41098 Summary of the Invention

[0020] When using chemical reaction etc. to manufacture a substance, sometimes the substance (target substance) manufactured exists in a solvent. In addition, sometimes contaminants are included in the target substance or the solvent containing the target substance. In this manual, the solvent containing the target substance is referred to as "liquid raw material".

[0021] When contaminants are present in the liquid raw material, the liquid raw material can be cleaned by extracting the contaminants from the liquid raw material. Furthermore, when recovering a target substance contained in the liquid raw material, the target substance can be recovered by extracting the target substance from the liquid raw material. As described later, in this specification, the target substance and contaminants extracted from the liquid raw material are referred to as "extraction target substances."

[0022] Examples of flow-type reaction devices in which the spatial scale of a reaction system for performing chemical / biochemical reactions is, for example, microreactors. Devices similar to microreactors can be used as devices for extracting an extraction target substance from a liquid raw material.

[0023] Microreactors have lower production capacity than conventional batch reactors. In microreactors designed for production, scaling up is being studied to increase production capacity. This includes branching the flow path and paralleling the devices. In addition to scaling up, another method for increasing production capacity is scaling up (in Japanese: イコーリングアップ), which increases flow rate by increasing the diameter and length of the piping without changing the residence time.

[0024] In extraction using slug flow, increasing the size of the extraction process to increase throughput can lead to problems distinct from those encountered with reactions. Increasing the flow rate can lead to emulsion formation, impairing separation performance. Using thicker tubing can also reduce extraction efficiency and destabilize the slug flow. Therefore, increasing the number of extraction processes is necessary to increase throughput.

[0025] It is generally believed that increasing the number of branched flow paths makes it difficult to evenly distribute the liquid feedstock throughout multiple flow paths. Furthermore, if one flow path becomes clogged, the flow rate in other flow paths will change, necessitating blockage prevention. Furthermore, there is the disadvantage of having to constantly monitor each flow path to ensure it is free of blockage.

[0026] Thus, scaling up by branching the flow path involves numerous technical challenges. Therefore, scaling up by parallelizing the devices is more readily industrializable. However, this scaling up approach incurs significant manufacturing costs, leading to the desire for a microreactor that can more cost-effectively and conveniently scale up the device.

[0027] One of the main factors affecting the manufacturing cost of a microreactor is the price and performance of the pump. Generally, in a microreactor, syringe pumps and / or plunger pumps with low pulsation are used to transport the reactants (liquid raw materials and / or raw material solutions). Using a pulsating pump to transport the solution makes it difficult to generate a fine and stable slug flow within the equipment used to extract the target substance, resulting in reduced extraction efficiency.

[0028] Syringe pumps do not produce pulsation, but continuous operation requires two or more pumps per system. Precise flow control requires an expensive syringe pump system. Furthermore, continuous operation can cause syringe deterioration, leading to the risk of leakage or breakage.

[0029] Plunger pumps are easy to operate continuously, but using a single piston results in significant pulsation, increasing the slug length (the length of a single liquid flowing through a pipe when two liquids flow as a slug), which reduces the efficiency of extracting the target substance. Consequently, expensive duplex or triplex pumps, consisting of two or three connected pistons, are required.

[0030] Furthermore, when extracting contaminants contained in a liquid raw material multiple times, contamination may occur due to removal for each extraction operation.

[0031] The present invention has been made in view of the above-mentioned problems, and its object is to provide a device that can more easily extract the extraction target substance contained in the liquid raw material. In addition, the present invention is to provide a device that can more easily extract the extraction target substance contained in the liquid raw material while suppressing the occurrence of contamination.

[0032] In order to solve the above-mentioned problems, the present invention has the following structure.

[0033] (Structure 1)

[0034] Structure 1 is a device for extracting an extraction target substance dissolved in a liquid raw material, wherein:

[0035] The device comprises:

[0036] at least one raw material tank for storing the liquid raw material;

[0037] a solvent tank for storing a solvent used to extract the extraction target substance from the liquid raw material;

[0038] a pressurized gas supply component for supplying pressurized gas to the solvent tank;

[0039] a small-diameter portion, one end of the small-diameter portion being connected to the solvent tank via a first solvent pipe, the other end of the small-diameter portion being connected to a second solvent pipe, the inner diameter of the small-diameter portion being smaller than the inner diameters of the first solvent pipe and the second solvent pipe;

[0040] at least one extraction unit, comprising a mixer, an extraction section, and a liquid separation section, the mixer comprising a first inlet connected to the raw material tank and a second inlet connected to the small-diameter section via the second solvent pipe, the mixer being configured to mix the liquid flowing in from the first inlet with the liquid flowing in from the second inlet, the extraction section being configured to extract the extraction target substance from the liquid raw material into the solvent, the extraction section being connected to the mixer, the liquid separation section being connected to the extraction section, and comprising a first outflow hole for outflowing a first recovery liquid containing the solvent and the extraction target substance, and a second outflow hole for outflowing a second recovery liquid separated from the first recovery liquid, at least one raw material tank being connected to the first inflow hole of the mixer of at least one extraction unit;

[0041] a first recovery tank connected to the first outflow hole and configured to recover the first recovery liquid; and

[0042] The second recovery tank is connected to the second outflow hole and is used to recover the second recovery liquid.

[0043] (Structure 2)

[0044] Structure 2 is an apparatus according to Structure 1, wherein:

[0045] The extraction target substance is a pollutant, and the device is a washing device for the liquid raw material.

[0046] (Structure 3)

[0047] Structure 3 is an apparatus according to Structure 1, wherein:

[0048] The extraction target substance is a target substance, and the device is a device for extracting the target substance.

[0049] (Structure 4)

[0050] Structure 4 is a device according to any one of Structures 1 to 3, wherein:

[0051] The pressurized gas supply component includes a high-pressure gas supply unit and a pressure adjustment unit.

[0052] The pressure inside the solvent tank and the first solvent pipe is 1.5 MPa or less.

[0053] (Structure 5)

[0054] Structure 5 is a device according to any one of Structures 1 to 4, wherein:

[0055] The small diameter portion further includes a thermostat for adjusting the temperature of the small diameter portion.

[0056] (Structure 6)

[0057] Configuration 6 is a device according to any one of Configurations 1 to 5, wherein:

[0058] The device comprises at least two extraction units connected in series,

[0059] The raw material tank is connected to the first inflow port of the mixer of the extraction unit at the most upstream side.

[0060] In a pair of the extraction units connected in series, the second outflow port of the extraction unit on the upstream side is connected to the first inflow port of the mixer of the extraction unit on the downstream side.

[0061] The solvent tank is connected to the mixers of at least two extraction units via the small diameter portion.

[0062] The small-diameter portion connected to the second inflow hole is a small-diameter portion having different pressure losses between the small-diameter portion on the upstream side and the small-diameter portion on the downstream side.

[0063] A second small-diameter portion is provided in the flow path connected to the first recovery tank and the second recovery tank.

[0064] (Structure 7)

[0065] Structure 7 is a device according to any one of Structures 1 to 5, wherein:

[0066] The device comprises at least two extraction units connected in parallel,

[0067] The raw material tank is connected to the first inflow port of the mixer of at least two extraction units.

[0068] The solvent tank is connected to the second inflow port of the mixer of at least two of the extraction units via the small-diameter portion.

[0069] Structure 8 is a device according to any one of Structures 1 to 5, wherein:

[0070] The device comprises at least two extraction units connected in series,

[0071] The raw material tank is connected to the first inflow port of the mixer of the extraction unit at the most upstream side.

[0072] In at least one pair of the extraction units connected in series, the first outflow hole of the extraction unit on the upstream side is connected to the first inflow hole of the mixer of the extraction unit on the downstream side.

[0073] The solvent tank is connected to the mixer of the extraction unit via the small diameter portion.

[0074] The small-diameter portion connected to the second inflow hole is a small-diameter portion having different pressure losses between the small-diameter portion on the upstream side and the small-diameter portion on the downstream side.

[0075] A second small-diameter portion is provided in the flow path connected to the first recovery tank and the second recovery tank.

[0076] Structure 9 is the apparatus according to Structure 8, wherein:

[0077] In the extraction unit at the most upstream side and the extraction unit connected in series thereto, the first outflow hole of the extraction unit at the most upstream side is connected to the second inflow hole of the mixer of the extraction unit at the downstream side.

[0078] In at least one pair of the extraction units connected in series, the second outflow port of the extraction unit on the upstream side is connected to the first inflow port of the mixer of the extraction unit on the downstream side.

[0079] Structure 10 is an apparatus according to structure 8 or 9, wherein

[0080] The apparatus includes at least two solvent tanks, each of which stores a different solvent.

[0081] (Structure 11)

[0082] Configuration 8 is a device according to any one of Configurations 1 to 10, wherein:

[0083] The solvent tank is a pressure-resistant tank.

[0084] (Structure 12)

[0085] Configuration 9 is a device according to any one of Configurations 1 to 11, wherein:

[0086] The mixer has a micro flow path, and the width of the micro flow path is 0.01 μm to 20 mm.

[0087] (Structure 13)

[0088] Structure 10 is a device according to any one of Structures 1 to 12, wherein:

[0089] The inner diameters of the first solvent pipe and the second solvent pipe are 0.1 mm to 20 mm.

[0090] (Structure 14)

[0091] Structure 11 is a device according to any one of Structures 1 to 13, wherein:

[0092] The apparatus further includes liquid raw material supply means for supplying the liquid raw material to the mixer.

[0093] According to the present invention, it is possible to provide an apparatus capable of more easily extracting an extraction target substance contained in a liquid raw material. In addition, according to the present invention, it is possible to provide an apparatus capable of more easily extracting an extraction target substance contained in a liquid raw material while suppressing the occurrence of contamination. BRIEF DESCRIPTION OF THE DRAWINGS

[0094] Figure 1 This is a schematic diagram of the device according to the first embodiment.

[0095] Figure 2 This is a schematic diagram of another form of the device of the first embodiment.

[0096] Figure 3It is a schematic diagram of the apparatus of the 2nd embodiment and the 3rd embodiment.

[0097] Figure 4 This is a schematic diagram of a device according to a fourth embodiment.

[0098] Figure 5 It is an enlarged cross-sectional schematic diagram of the small diameter portion.

[0099] Figure 6 It is a perspective schematic diagram showing another example of the small-diameter portion.

[0100] Figure 7 It is a schematic cross-sectional view showing another example of the small-diameter portion.

[0101] Figure 8 is a schematic diagram of a reaction apparatus for producing reactants.

[0102] Figure 9 It is a schematic diagram of the device of the sixth embodiment. DETAILED DESCRIPTION

[0103] This embodiment is an apparatus for extracting an extraction target substance dissolved in a liquid raw material.

[0104] <First embodiment>

[0105] Figure 1 A schematic diagram of a first embodiment of the present embodiment is shown. The first embodiment of the present embodiment includes a raw material tank 10, a solvent tank 20, a pressurized gas supply unit 30, a flow path having a small diameter portion 40, an extraction unit 100, a first recovery tank 50, and a second recovery tank 60. The first embodiment of the present embodiment can extract an extraction target substance dissolved in a liquid raw material 12.

[0106] exist Figure 1 , the parts connected by straight lines represent connections in a manner that allows fluid to move. The same is true in other figures. In this specification, "part A is connected to part B" means that part A and part B are connected by piping or the like in a manner that allows fluid to move.

[0107] The piping etc. for connecting each part can use piping such as pipes, but is not limited thereto. For example, the piping can be connected by using a plate-like structure having flow paths formed by grooves etc. on a plate-like surface such as a flat plate.

[0108] In this specification, the terms "upstream" and "downstream" are defined by the direction in which the liquid raw material 12 and solvent 22 flow within the apparatus of this embodiment. Specifically, the direction closer to the raw material tank 10 and solvent tank 20 is the upstream side, and the direction closer to the first recovery tank 50 and second recovery tank 60 is the downstream side.

[0109] In this specification, "extraction target substance" refers to either a pollutant or a target substance. When the extraction target substance is a pollutant, the apparatus of this embodiment is an apparatus for washing liquid raw material 12. Alternatively, when the extraction target substance is a target substance, the apparatus of this embodiment is an apparatus for extracting the target substance.

[0110] When the substance to be extracted is a contaminant, the cleaning apparatus of this embodiment can remove the liquid raw material 12 from the raw material tank 10 and extract the contaminant from the liquid raw material 12. As a result, the contaminant can be removed from the liquid raw material 12 and cleaned. In the apparatus of this embodiment, by bringing the solvent 22 into contact with the liquid raw material 12, the contaminant can be extracted from the liquid raw material 12 into the solvent 22 and removed.

[0111] When the substance to be extracted is the target substance, the extraction apparatus of this embodiment can remove the liquid raw material 12 from the raw material tank 10 and extract the target substance from the liquid raw material 12. As a result, the target substance can be extracted from the liquid raw material 12. In addition, in the apparatus of this embodiment, by bringing the solvent 22 into contact with the liquid raw material 12, the target substance can be extracted from the liquid raw material 12 into the solvent 22.

[0112] The device of this embodiment can also be used as a device for extracting an extraction target substance contained in the slurry-like liquid raw material 12 .

[0113] In the apparatus of this embodiment, when a hydrophilic liquid raw material 12 is used as the liquid raw material 12, it is preferable to use a hydrophobic solvent 22 as the solvent 22 for extracting the extraction target substance from the liquid raw material 12. Furthermore, in the apparatus of this embodiment, when a hydrophobic liquid raw material 12 is used as the liquid raw material 12, it is preferable to use a hydrophilic solvent 22 as the solvent 22 for extracting the extraction target substance from the liquid raw material 12. By using different types of liquids for the liquid raw material 12 and the solvent 22, it is possible to facilitate separation of the liquid raw material 12 from the solvent 22 after the extraction target substance has been extracted.

[0114] <<Raw material tank 10>>

[0115] like Figure 1 As shown, the apparatus of this embodiment includes at least one raw material tank 10 for storing a liquid raw material 12. The raw material tank 10 is a tank for storing the liquid raw material 12.

[0116] The raw material tank 10 is not particularly limited as long as it can store the liquid raw material 12. For example, a metal, resin, or glass tank can be used. In this embodiment, a pressure-resistant tank made of SUS or polyethylene can be used as the raw material tank 10. By using a pressure-resistant tank as the raw material tank 10, the interior of the raw material tank 10 can be maintained at a high pressure. Therefore, by using the pressurized gas supply unit 30 described below, the liquid raw material 12 can be easily and cost-effectively removed from the raw material tank 10.

[0117] The raw material tank 10 is connected to the extraction unit 100 described later. As the pipe connecting the raw material tank 10 and the extraction unit 100, for example, a PTFE (polytetrafluoroethylene) tube having an inner diameter of 1.0 to 10 mm can be used.

[0118] The apparatus of this embodiment preferably further includes a liquid raw material supply unit for supplying the liquid raw material 12 to the mixer 110 of the extraction unit 100 described later. Figure 1 In the example shown, a pump 14 is used as the liquid raw material supply means. As the liquid raw material supply means, the pump 14 may be a syringe pump, a plunger pump, a diaphragm pump, a pulsation-free tube pump, a centrifugal pump, or the like.

[0119] like Figure 2 As shown, the liquid raw material supply unit of the apparatus of this embodiment can be configured similarly to the solvent tank 20 described later. It includes a pressurized gas supply unit 30 for the raw material tank 10. By introducing pressurized gas into the raw material tank 10 via the pressurized gas supply unit 30, the liquid raw material 12 can be removed from the solvent tank 20. When the liquid raw material 12 is supplied to two or more predetermined extraction units 100 using a pump 14, a predetermined number of pumps 14 are required. However, the apparatus of this embodiment, by including the pressurized gas supply unit 30 for the raw material tank 10, eliminates the need for a predetermined number of pumps 14. Consequently, the cost of the apparatus of this embodiment can be reduced, and the apparatus structure can be simplified.

[0120] The liquid raw material 12 may be a target substance (reactant) produced using the apparatus described in Patent Document 5, for example.

[0121] Using the apparatus described in Patent Document 5, liquid raw materials 12 stored in two raw material tanks 10 are mixed by a mixer 110 to obtain a reaction product containing a target substance within a pipe. The reaction product obtained by reacting the substances contained in the two liquid raw materials 12 can be used as the liquid raw material 12 of this embodiment. The details are as follows.

[0122] Figure 8An example of a flow chart of a micro-chemical equipment described in Patent Document 5 is shown. In this embodiment, the micro-chemical equipment can be used as the reaction device 210 .

[0123] like Figure 8 As shown, the reaction device 210 for manufacturing the reactant has two reaction device raw material tanks 212a and 212b, a reaction device mixer 214, and a reactant tank 216. The reaction device raw material tanks 212a and 212b are tanks for storing two liquid raw materials. The liquid raw materials transported from the reaction device raw material tanks 212a and 212b are mixed by the reaction device mixer 214. The reactant obtained by mixing the liquid raw materials is stored in the reactant tank 216. The reaction device raw material tank 212a and the reaction device mixer 214 are connected by a pipe 218a. The reaction device raw material tank 212b and the reaction device mixer 214 are connected by a pipe 218b. The reaction device mixer 214 and the reactant tank 216 are connected by a pipe 220.

[0124] The pipes 218a and 218b connecting the reaction device raw material tanks 212a and 212b to the reaction device mixer 214 are respectively provided with small-diameter portions 228a and 228b for the reaction device. The small-diameter portions 228a and 228b for the reaction device can be tubes having an inner diameter smaller than the inner diameter of the pipes on the upstream and / or downstream sides thereof. As the small-diameter portions 228a and 228b for the reaction device, the same small-diameter portion 40 as that of the device of this embodiment described later can be used.

[0125] The reaction device 210 is a device capable of mixing two liquid raw materials. By mixing the two raw materials and reacting them, the target reaction product can be obtained.

[0126] The reaction device 210 is equipped with a nitrogen tank (not shown). Nitrogen (N2 gas) can be supplied from the nitrogen tank to the two reaction device raw material tanks 212a and 212b. The nitrogen tank and the reaction device raw material tanks 212a and 212b are connected by reaction device nitrogen supply pipes 222a and 222b. Reactor pressure regulating valves 224a and 224b (pressure regulators) are provided at the reaction device nitrogen supply pipes 222a and 222b. Utilizing the reaction device pressure regulating valves 224a and 224b, the pressure of the nitrogen in the reaction device raw material tanks 212a and 212b can be maintained constant. In addition, utilizing the reaction device pressure regulating valves 224a and 224b, the flow rate of the liquid raw material transferred from the two reaction device raw material tanks 212a and 212b to the reaction device mixer 214 can be adjusted respectively. The pressure range of the gas supplied to the raw material tanks 212a and 212b for the reaction device is 1 kPa to 200 MPa, preferably 10 kPa to 15 MPa.

[0127] exist Figure 8 In the reaction device 210 shown in FIG. 1 , the reaction product is recovered in the reaction product tank 216. In the device of this embodiment, the piping 220 of the reaction device 210 can be connected to the pipe 220 of the embodiment. Figure 1 As a result, it is possible to use Figure 8 The reaction device 210 shown is replaced Figure 1 In this case, the raw material tank 10 is Figure 8 The reactant produced by the reaction device 210 shown in FIG. 1 becomes the liquid raw material 12 of the device of this embodiment. Figure 8 The reactant tank 216 shown is used as the raw material tank 10 of the apparatus of this embodiment.

[0128] <<Solvent tank 20>>

[0129] like Figure 1 As shown in FIG. 1 , the apparatus of this embodiment includes a solvent tank 20 for storing a solvent 22 . The solvent 22 is a liquid for extracting an extraction target substance from a liquid raw material 12 .

[0130] The solvent tank 20 is not particularly limited as long as it can store the solvent 22 , and for example, a tank made of metal, resin, or glass can be used.

[0131] The solvent tank 20 of the apparatus of this embodiment is preferably a pressure-resistant tank. Pressure-resistant tanks made of SUS or polyethylene can be used as the solvent tank 20. Using a pressure-resistant tank as the solvent tank 20 allows the interior of the solvent tank 20 to be maintained at a high pressure. Consequently, by using the pressurized gas supply unit 30 (described later), the solvent 22 can be easily and cost-effectively removed from the solvent tank 20.

[0132] << Pressurized gas supply unit 30 >>

[0133] like Figure 1 As shown, the apparatus of this embodiment includes a pressurized gas supply unit 30 for supplying pressurized gas to the solvent tank 20. In the apparatus of this embodiment, the pressurized gas supply unit 30 may include a high-pressure gas supply portion 32 and a pressure regulator 34.

[0134] The apparatus of this embodiment can also include a pressurized gas supply unit 30 for supplying pressurized gas to the raw material tank 10, similarly to the solvent tank 20. Therefore, in addition to the pressurized gas supply unit 30 for the solvent tank 20, the apparatus of this embodiment can also include a pressurized gas supply unit 30 for the raw material tank 10. Furthermore, the pressurized gas supply unit 30 can be a single unit, shared by both the solvent tank 20 and the raw material tank 10.

[0135] The liquid extraction method implemented by the pressurized gas supply unit 30 is less expensive and simpler than using a device such as the pump 14. However, compared to devices such as the pump 14, the liquid extraction method implemented by the pressurized gas supply unit 30 is more difficult to strictly control the flow rate. When extracting the target substance using the device of this embodiment, it is not necessary to strictly control the flow rate of the solvent 22. Therefore, the liquid extraction method implemented by the pressurized gas supply unit 30 is preferably used to extract the solvent 22 from the solvent tank 20.

[0136] On the other hand, when extracting the target substance using the apparatus of this embodiment, it may be necessary to strictly control the liquid raw material 12. In such cases, a pump 14 such as a syringe pump 14 or a plunger pump 14 capable of strictly controlling the flow rate is preferably used to remove the liquid raw material 12 from the raw material tank 10. However, if strict flow rate control of the liquid raw material 12 is not necessary, a relatively low-cost and simple liquid removal method using the pressurized gas supply unit 30 can be used to remove the liquid raw material 12 from the raw material tank 10.

[0137] A nitrogen tank, for example, can be used as the high-pressure gas supply unit 32 of the pressurized gas supply component 30. Nitrogen gas (N2 gas) can be supplied from the nitrogen tank to the solvent tank 20 (and, if necessary, the raw material tank 10). The nitrogen tank and the solvent tank 20 (and, if necessary, the raw material tank 10) are connected by a nitrogen supply pipe 36. A pressure regulating valve (pressure regulator) is provided on the nitrogen supply pipe 36 as a pressure regulating unit 34. The pressure regulating valve can be used to adjust the pressure of the nitrogen gas in the solvent tank 20 (and, if necessary, the raw material tank 10).

[0138] Nitrogen corresponds to the "gas" of this embodiment. The nitrogen tank, pressure regulating valve and nitrogen supply piping 36 for supplying nitrogen correspond to the "pressurized gas supply component 30" of this embodiment. The pressure regulating valve that adjusts the pressure of the nitrogen filled in the solvent tank 20 (and the raw material tank 10 as needed) corresponds to the "pressure regulating unit 34" of this embodiment. The pressure regulating valve can be used to adjust the flow rate of the solvent 22 (and the liquid raw material 12 as needed) transferred from the solvent tank 20 (and the raw material tank 10 as needed). As a gas, gases other than nitrogen can be used, such as compressed air, inert gas, etc. Nitrogen is relatively cheap and less dangerous, so it is preferred to use nitrogen as the pressurized gas.

[0139] The pressure inside the solvent tank 20 and the first solvent pipe 42 is preferably 1.5 MPa or less. The pressure range of the gas supplied to the solvent tank 20 (and to the raw material tank 10 as needed) is more preferably 1 kPa to 1 MPa, and preferably 10 kPa to 500 kPa.

[0140] Solvent 22 is stored in solvent tank 20. The space above the stored solvent 22 is filled with nitrogen gas. The pressure of the nitrogen gas above solvent 22 allows solvent 22 to be transferred from solvent tank 20 to small-diameter portion 40, described later, via the pipe. In other words, solvent tank 20 can transfer solvent 22 to the next device using the pressure of the nitrogen gas (gas) filled therein. When a liquid removal method using pressurized gas supply unit 30 is used to remove liquid raw material 12 from raw material tank 10, the pressure of the nitrogen gas (gas) can also be used to transfer liquid raw material 12 within raw material tank 10 to the next device.

[0141] <<Small diameter portion 40>>

[0142] like Figure 1 As shown, the device of this embodiment includes a small-diameter portion 40. One end of the small-diameter portion 40 is connected to the solvent tank 20 via a first solvent pipe 42, and the other end of the small-diameter portion 40 is connected to a second solvent pipe 44. Furthermore, the inner diameter of the small-diameter portion 40 is smaller than the inner diameters of the first solvent pipe 42 and the second solvent pipe 44. By setting the inner diameter and length of the small-diameter portion 40 to an appropriate value, the flow rate of a fluid such as the solvent 22 flowing through the small-diameter portion 40 can be controlled.

[0143] When using the pressurized gas supply unit 30 to remove liquid from the solvent tank 20, the small-diameter portion 40 must be used. The combination of pressurizing the interior of the solvent tank 20 and the small-diameter portion 40 allows the flow rate of the solvent 22 to be controlled. Similarly, when using the pressurized gas supply unit 30 to remove the liquid raw material 12 from the raw material tank 10, the small-diameter portion 40 can be used to control the flow rate of the liquid raw material 12.

[0144] The first solvent piping 42 connecting the solvent tank 20 and the small diameter portion 40 can be, for example, a tube made of PTFE (polytetrafluoroethylene). An on-off valve (not shown) can be provided in the first solvent piping 42. The on-off valve is a valve for controlling the circulation / non-circulation of the solvent 22 flowing inside the first solvent piping 42. The on-off valve can be, for example, an electromagnetic valve. The pressure inside the first solvent piping 42 connecting the raw material tank 10 and the small diameter portion 40 preferably does not exceed the allowable pressure of the on-off valve. In the case where the on-off valve is composed of an electromagnetic valve, the pressure inside the first solvent piping 42 connecting the raw material tank 10 and the small diameter portion 40 is preferably below 1.5 MPa, and more preferably below 0.8 MPa.

[0145] A second solvent pipe 44 is connected to the other end of the small diameter portion 40 (the end opposite to the end connected to the first solvent pipe 42). Like the first solvent pipe 42, the second solvent pipe 44 can be a PTFE (polytetrafluoroethylene) tube.

[0146] The second solvent pipe 44 is connected to the extraction unit 100 described later. A flow rate adjustment valve (not shown) for fine-tuning the flow rate of the solvent 22 can be provided on the second solvent pipe 44 between the small-diameter portion 40 and the extraction unit 100. The flow rate adjustment valve can be provided to more accurately control the flow rate of the solvent 22.

[0147] In the apparatus of this embodiment, the inner diameters of the first solvent pipe 42 and the second solvent pipe 44 are preferably 0.1 mm to 20 mm, more preferably 0.2 mm to 10 mm, and even more preferably 0.5 mm to 2 mm. By having the inner diameters of the first solvent pipe 42 and the second solvent pipe 44 being of the specified size, the solvent 22 can be smoothly transferred. Furthermore, pipes having the aforementioned inner diameters can also be used for pipes other than the first solvent pipe 42 and the second solvent pipe 44.

[0148] A small diameter portion 40 is arranged between the first solvent piping 42 and the second solvent piping 44. The inner diameter of the small diameter portion 40 (the inner diameter of the flow path for the solvent 22 to flow) is smaller than the inner diameters of the first solvent piping 42 and the second solvent piping 44. As the small diameter portion 40, a tube having an inner diameter smaller than the inner diameters of the first solvent piping 42 and the second solvent piping 44 connected to the small diameter portion 40 can be used. The inner diameter of the small diameter portion 40 is preferably, for example, 0.01 mm to 1.0 mm in diameter. The small diameter portion 4 can be, for example, a tube made of PEEK (polyetheretherketone) with an inner diameter of 0.2 mm. As Figure 5 As shown, the first solvent pipe 42 and the small-diameter portion 40 can be connected by a connector 41a. The second solvent pipe 44 and the small-diameter portion 40 can be connected by a connector 41b.

[0149] The length of the small diameter portion 40 can be appropriately selected to control the flow rate of the fluid such as the solvent 22 flowing through the small diameter portion 40. Specifically, the length of the small diameter portion 40 is preferably 10 to 500 mm, more preferably 30 to 400 mm, and even more preferably 50 to 300 mm.

[0150] exist Figure 1 , an example is shown in which one solvent tank 20 and one small diameter portion 40 are connected by one first solvent pipe 42. In other embodiments of this embodiment, two or more first solvent pipes 42 can be connected to two or more small diameter portions 40 from one solvent tank 20 (see Figure 3 and Figure 4 That is, a plurality of first solvent pipes 42 may be branched from the solvent tank 20 or provided in parallel, and the solvent tank 20 and the plurality of small-diameter portions 40 may be connected by the first solvent pipes 42 branched from or provided in parallel.

[0151] Hereinafter, the small-diameter portion 40 will be further described.

[0152] The small-diameter portion 40 can be a valve. For example, a valve equipped with a valve core or a spool that can adjust the size of the flow path can be used as the small-diameter portion 40. For example, a gate valve or a stop valve can be used as the small-diameter portion 40. Specifically, a "needle valve" (manufactured by IDEX, Model P-445) that can adjust the size of the flow path can be used as the small-diameter portion 40.

[0153] The small-diameter portion 40 can be a throttle hole. For example, a throttle hole formed in a resin or metal thin plate with an opening smaller than the inner diameter of the first solvent pipe 42 and the second solvent pipe 44 can be used as the small-diameter portion 40. The throttle hole can be a throttle hole formed in a plate with one opening, or a throttle hole formed in a plate with multiple openings. For example, an online filter for HPLC or ion chromatography can be used as the small-diameter portion 40. Specifically, a PEEK pre-column filter for HPLC (manufactured by Shimadzu GLC Co., Ltd.) can be used as the small-diameter portion 40.

[0154] like Figure 6 As shown, the small-diameter portion 40 can be manufactured by forming a microchannel 404 on one surface of a metal plate 402a and then overlapping another metal plate 402b on the surface of the metal plate 402a on which the microchannel 404 is formed. That is, the small-diameter portion 40 can also be formed by forming the microchannel 404 on the metal plate 402a, similar to the aforementioned micromixer 110. The microchannel 404 has an inner diameter smaller than the inner diameter of the upstream pipe (first solvent pipe 42) and the downstream pipe (second solvent pipe 44) of the small-diameter portion 40.

[0155] like Figure 7 As shown, the small-diameter portion 40 may be formed by physically deforming a metal or resin tube 412 to partially reduce the inner diameter of the tube 412. The inner diameter of the deformed portion 414 of the tube 412 is smaller than the inner diameters of the first solvent pipe 42 and the second solvent pipe 44 on the upstream and / or downstream sides thereof.

[0156] like Figure 1 As shown, in the device of this embodiment, the small-diameter portion 40 is preferably further provided with a thermostat 46 for adjusting the temperature of the small-diameter portion 40. By adjusting the temperature of the small-diameter portion 40, the temperature of the solvent 22 at the small-diameter portion 40 can be controlled. By controlling the temperature of the solvent 22, the physical properties such as the viscosity of the solvent 22 can be changed, and thus the flow rate of the solvent 22 at the small-diameter portion 40 can be controlled.

[0157] When an on-off valve is provided in the first solvent pipe 42, the pressure inside the first solvent pipe 42 connecting the solvent tank 20 and the small-diameter portion 40 preferably does not exceed the permissible pressure of the on-off valve. When the on-off valve is a solenoid valve, the pressure inside the first solvent pipe 42 connecting the solvent tank 20 and the small-diameter portion 40 is preferably 1.5 MPa or less, and more preferably 0.8 MPa or less.

[0158] When a liquid extraction method using pressurized gas supply unit 30 is used to extract liquid raw material 12 from raw material tank 10, a small-diameter portion 40 can be provided midway along the piping connecting raw material tank 10 to extraction unit 100 (described later), similarly to the case of solvent tank 20 described above. Providing small-diameter portion 40 allows control of the flow rate of liquid raw material 12 transferred from raw material tank 10.

[0159] <<Extraction unit 100>>

[0160] The device of this embodiment includes at least one extraction unit 100 including a mixer 110, an extraction unit 130, and a liquid separation unit 140. The device of this embodiment can include a plurality of extraction units 100. Figure 1 In the illustrated example, the case where there is only one extraction unit 100 is shown.

[0161] (Mixer 110)

[0162] The extraction unit 100 of the apparatus of this embodiment includes a mixer 110. In this specification, the mixer 110 may be referred to as a "mixing section."

[0163] The mixer 110 has a first inflow hole 112 connected to the raw material tank 10 and a second inflow hole 114 connected to the small diameter portion 40 via a second solvent pipe 44. The mixer 110 can mix the liquid flowing in from the first inflow hole 112 and the liquid flowing in from the second inflow hole 114. Figure 1 In the example shown, the liquid flowing in from the first inflow hole 112 is the liquid raw material 12, and the liquid flowing in from the second inflow hole 114 is the solvent 22. Figure 1 In the example shown, the liquid raw material 12 and the solvent 22 are mixed by being brought together in the mixer 110 .

[0164] When there are a plurality of extraction units 100 , at least one raw material tank 10 is connected to the first inflow port 112 of the mixer 110 of the plurality of extraction units 100 .

[0165] As long as mixer 110 can mix two kinds of liquids (liquid raw materials 12 and solvent 22), there is no particular restriction, and any mixer 110 can be used. As mixer 110, for example, commercially available known metal, resin or glass micro mixers can be used. Micro mixer refers to a mixer having a micro flow path for mixing a plurality of liquid raw materials 12. Micro mixer can be manufactured by, for example, forming micro flow path on one face of a metal plate and overlapping another metal plate on the face of the metal plate formed with micro flow path. There is no particular restriction on the shape of micro flow path, for example, a mixer having a T-shaped micro flow path or a mixer having a Y-shaped micro flow path can be used.

[0166] In the apparatus of this embodiment, the mixer 110 has a microchannel, and the width (or diameter) of the microchannel is preferably 0.01 μm to 20 mm, more preferably 0.01 mm to 10 mm, and even more preferably 0.1 mm to 5 mm. By keeping the width (or diameter) of the microchannel of the mixer 110 within a predetermined range, the liquid raw material 12 and the solvent 22 can be efficiently mixed.

[0167] In the mixer 110 , the diameters of the pipes for the liquid raw material 12 and the solvent 22 upstream of the point where the liquid raw material 12 and the solvent 22 merge are preferably 0.01 μm to 20 mm, more preferably 0.01 mm to 10 mm, and even more preferably 0.1 mm to 5 mm.

[0168] In mixer 110, the diameter of the pipe for the mixed liquid of liquid raw material 12 and solvent 22 downstream of the point where liquid raw material 12 and solvent 22 merge is preferably 0.01 μm to 20 mm, more preferably 0.01 mm to 10 mm, and even more preferably 0.1 mm to 5 mm. When the pipe diameter in mixer 110 is within this range, the liquid raw material 12 and solvent 22 can be mixed more efficiently.

[0169] The two liquids (liquid raw material 12 and solvent 22) mixed in the mixer 110 preferably form a slug flow and are transferred to the downstream extraction unit 130. By forming a slug flow of the liquid raw material 12 and the solvent 22, the extraction target substance dissolved in the liquid raw material 12 can be efficiently extracted into the solvent 22.

[0170] A specific example of the mixer 110 is as follows. The shape of the flow path of the mixer 110 can include a flow path consisting of a groove or a slit-shaped through-hole provided on a substrate. The flow path can be any shape that can mix two liquids. The mixer 110 of the device of this embodiment can include two liquid injection ports (a first inflow hole 112 and a second inflow hole 114), two inflow paths connected to the injection ports, a confluence point where the two inflow paths converge, a conveying path connected to the confluence point, and a discharge port connected to the conveying path. The mixing portion can be Y-shaped. The inflow path and the conveying path can be composed of a groove with a bottom provided on a substrate. In addition, the groove can become a flow path by covering and sealing it with a protective member or the like.

[0171] (Extraction Unit 130)

[0172] The extraction unit 100 of the device of this embodiment includes an extraction section 130 .

[0173] The extraction unit 130 is connected to the downstream side of the mixer 110 . In the extraction unit 130 , the extraction target substance can be extracted from the liquid raw material 12 into the solvent 22 .

[0174] The extraction part 130 can be a pipe such as a tube having a predetermined diameter and length connected to the mixer 110. The extraction part 130 can be a tube made of PTFE (polytetrafluoroethylene), for example.

[0175] The extraction portion 130 can be a plate-like structure in which a flow path of a predetermined size (width and depth) is formed by grooves or the like on a surface of a plate such as a flat plate.

[0176] The liquid raw material 12 and solvent 22 mixed in the mixer 110 preferably form a slug flow in the extraction section 130. Since the mixed liquid of the liquid raw material 12 and solvent 22 forms a slug flow in the extraction section 130, the liquid raw material phase and the solvent phase are maintained, and each phase flows through the extraction section 130 while circulating internally. As a result, the liquid raw material 12 and solvent 22 are supplied from the interiors of the liquid raw material phase and the solvent phase to the interface between the liquid raw material phase and the solvent phase. This facilitates the movement (extraction) of the extraction target substance in the liquid raw material 12 into the solvent phase. Therefore, by forming a slug flow of the liquid raw material 12 and solvent 22, the extraction target substance can be efficiently extracted from the liquid raw material 12 into the solvent 22. By controlling the flow rate ratio of the liquid raw material 12 and solvent 22, the inner diameter and length of the extraction section 130, and the flow rate of the mixed liquid of the liquid raw material 12 and solvent 22 in the extraction section 130, the mixed liquid of the liquid raw material 12 and solvent 22 can be made to form a slug flow in the extraction section 130.

[0177] The inner diameter or size of the extraction section 130 is preferably 0.1 to 20 mm, more preferably 0.2 to 10 mm, and even more preferably 0.5 to 5 mm. By setting the inner diameter or size of the extraction section 130 to a specified range, the two liquids (liquid raw material 12 and solvent 22) mixed in the mixer 110 can form a slug flow. As a result, the extraction target substance dissolved in the liquid raw material 12 can be efficiently extracted into the solvent 22 in the extraction section 130. When the inner diameter or size of the extraction section 130 is large, the extraction efficiency tends to decrease. In addition, when the inner diameter or size of the extraction section 130 is small, productivity decreases, and the pressure loss is too large, so the flow of the liquid requires high pressure, which is uneconomical. In order to efficiently extract the extraction target substance, the inner diameter or size of the extraction section 130 is preferably constant in the longitudinal direction.

[0178] The length of extraction section 130 is preferably 0.5 to 10 m, more preferably 1 to 5 m, and even more preferably 2 to 4 m. If the length of extraction section 130 is shorter than the specified range, the transfer (extraction) of the target substance into the solvent phase will be insufficient. Furthermore, if the length of extraction section 130 is longer than the specified range, the pressure loss in extraction section 130 will be excessive. Consequently, high pressure will be required to maintain the liquid flow, which is uneconomical.

[0179] (Liquid Separation Unit 140)

[0180] The extraction unit 100 of the device of this embodiment includes a liquid separation unit 140 .

[0181] The liquid separation section 140 is connected to the extraction section 130. In the liquid separation section 140, the first recovery liquid 52 containing the solvent 22 and the extraction target substance and the second recovery liquid 62 other than the first recovery liquid 52 are separated. The liquid separation section 140 has a first outflow hole 142 and a second outflow hole 144. The first recovery liquid 52 containing the solvent 22 and the extraction target substance flows out from the first outflow hole 142. The second recovery liquid 62 separated from the first recovery liquid 52 flows out from the second outflow hole 144. By separating the first recovery liquid 52 containing the solvent 22 and the extraction target substance in the liquid separation section 140, the extraction target substance can be recovered.

[0182] In this specification, the solvent 22 containing the extraction target substance extracted in the extraction unit 130 (i.e., the liquid containing the solvent 22 and the extraction target substance) is referred to as the "first recovered liquid 52." Furthermore, in this specification, the liquid separated from the first recovered liquid 52 (e.g., the liquid containing the liquid raw material 12 as a main component) is referred to as the "second recovered liquid 62."

[0183] A clarifier can be used as the liquid separator 140. The clarifier is a device for separating a light liquid phase into a heavy liquid phase. Because the specific gravity of the solvent 22 differs from that of the liquid raw material 12, the clarifier can separate the solvent 22 containing the extraction target substance extracted in the extraction section 130 (first recovered liquid 52) and the remaining liquid (second recovered liquid 62).

[0184] Hereinafter, a case where a clarifier is used as the liquid separation unit 140 will be described as an example.

[0185] The clarifier can include a separation tank. The shape of the separation tank can be any shape that can accumulate multiple mixed liquids and separate them into phases using specific gravity. In the device of this embodiment, as the clarifier, for example, a clarifier with a separation tank described in Patent Document 6 can be used.

[0186] In the apparatus of the present embodiment, when a hydrophilic liquid raw material 12 is used as the liquid raw material 12, it is preferred to use a hydrophobic solvent 22 as the solvent 22 for extracting the extraction target substance from the liquid raw material 12. In addition, in the apparatus of the present embodiment, when a hydrophobic liquid raw material 12 is used as the liquid raw material 12, it is preferred to use a hydrophilic solvent 22 as the solvent 22 for extracting the extraction target substance from the liquid raw material 12. As a result, in the liquid separation section 140, it is possible to separate into a liquid caused by the liquid raw material 12 (the second recovered liquid 62) and a liquid caused by the solvent 22 (the first recovered liquid 52). In addition, the specific gravity of the liquid raw material 12 is preferably different from the specific gravity of the solvent 22. The liquid with a smaller specific gravity goes to the lower part of the separation tank, and the liquid with a larger specific gravity goes to the upper part of the separation tank. In Figure 1 In the illustrated example, the first recovered liquid 52 containing the solvent 22 and the extraction target substance is directed to the upper portion of the separation tank, while the second recovered liquid 62 containing a relatively large amount of the liquid raw material 12 is directed to the upper portion of the separation tank. However, depending on the relative specific gravity of the liquid raw material 12 and the solvent 22, the first recovered liquid 52 may be directed to the lower portion of the separation tank, while the second recovered liquid 62 may be directed to the upper portion of the separation tank. In this embodiment, the description is based on the example of a case where the specific gravity of the liquid raw material 12 is greater than that of the solvent 22.

[0187] like Figure 1As shown, the mixed liquid flowing out of the extraction part 130 is supplied from the injection port to the separation tank and accumulated in the separation tank. In the separation tank, the mixed liquid is accumulated and separated. A discharge port connected to the first outflow hole 142 is provided at the upper portion of the separation tank. The first recovered liquid 52 with a smaller specific gravity located at the upper portion of the liquid separated in the separation tank is discharged from the upper discharge port to the outside of the clarifier (liquid separation part 140). A discharge port connected to the second outflow hole 144 is provided at the lower portion of the separation tank. The second recovered liquid 62 with a larger specific gravity located at the lower portion of the liquid separated in the separation tank is discharged from the lower discharge port to the outside of the clarifier (liquid separation part 140).

[0188] The first recovered liquid 52 and the second recovered liquid 62 discharged from the clarifier (liquid separator 140 ) are discharged to the outside of the extraction unit 100 from the first outflow hole 142 and the second outflow hole 144 of the extraction unit 100 , respectively.

[0189] <<First recovery tank 50>>

[0190] The apparatus of this embodiment includes a first recovery tank 50 connected to the first outflow port 142 of the extraction unit 100 and configured to recover the first recovery liquid 52 .

[0191] The first recovery tank 50 is not particularly limited as long as it can store the first recovery liquid 52 mainly composed of the solvent 22. The first recovery tank 50 can be formed of, for example, a tank made of metal, resin, or glass.

[0192] A flow rate-adjustable valve 150 can be provided between the first outflow hole 142 and the first recovery tank 50. The valve 150 can be used to fine-tune the flow rate of the first recovery liquid 52 flowing out of the liquid separation section 140 of the extraction unit 100, making it easier to adjust the liquid level in the separation tank.

[0193] <<Second recovery tank 60>>

[0194] The apparatus of this embodiment includes a second recovery tank 60 connected to the second outflow port 144 of the extraction unit 100 and configured to recover the second recovery liquid 62 .

[0195] The second recovery tank 60 is not particularly limited as long as it can store the second recovery liquid 62. Like the first recovery tank 50, the second recovery tank 60 can be formed of a tank made of metal, resin, or glass, for example.

[0196] A flow-regulating valve 150 can be provided between the second outflow hole 144 and the second recovery tank 60. The valve 150 can be used to fine-tune the flow rate of the second recovery liquid 62 flowing out of the liquid separation section 140 of the extraction unit 100, making it easier to adjust the liquid level in the separation tank.

[0197] The operation and effects of the device of the first embodiment configured as described above will be described.

[0198] Conventional devices require expensive syringe pumps and / or plunger pumps to transfer the liquid raw material 12 and solvent 22 used to extract the target substance. This results in high manufacturing costs for the entire device and a complex structure.

[0199] The apparatus of this embodiment utilizes the pressure of a gas, such as nitrogen, filling the solvent tank 20 to transfer the solvent 22, eliminating the need for a syringe pump and / or plunger pump. This significantly reduces the overall manufacturing cost of the apparatus and simplifies the apparatus structure. Furthermore, utilizing the pressure of a gas, such as nitrogen, to transfer the liquid raw material 12 within the raw material tank 10 further reduces the overall manufacturing cost and simplifies the apparatus structure.

[0200] According to the apparatus of this embodiment, the pressure of the nitrogen gas in the raw material tank 10 can be maintained constant by the pressure regulating valve or the like, thereby preventing fluctuations in the flow rate of the solvent 22 (and the liquid raw material 12 ) flowing through the pipe.

[0201] Furthermore, a small-diameter portion 40 is provided in the piping connecting the solvent tank 20 (and the raw material tank 10) to the mixer 110 of the extraction section 130. This small-diameter portion 40 can be used to adjust the pressure loss of the flowing liquid. By adjusting the pressure loss, the flow rate of the solvent 22 (and the liquid raw material 12) flowing in the piping can be adjusted. As a result, the flow rate of the solvent 22 (and the liquid raw material 12) flowing in the piping can be maintained constant. Furthermore, in the extraction section 130 of the extraction unit 100, the contact between the liquid raw material 12 and the solvent 22 can be appropriately controlled, enabling stable extraction of the extraction target substance dissolved in the liquid raw material 12.

[0202] <Second embodiment>

[0203] A second embodiment of the present invention is a washing apparatus. Figure 3 A schematic diagram of a washing device according to the second embodiment is shown. Figure 3 Although details of the interior of the three extraction units 100a, 100b, and 100c are omitted, they are the same as the extraction unit 100 of the first embodiment described above. As described in the first embodiment, the three extraction units 100a, 100b, and 100c each include a mixer 110, an extraction unit 130, and a liquid separation unit 140.

[0204] The washing device of this embodiment has at least two extraction units 100 connected in series. By connecting at least two extraction units 100 in series, more pollutants contained in the liquid raw material 12 can be extracted. As a result, the washing of the liquid raw material 12 can be performed more effectively. In addition, since the washing is continuous, contamination can be suppressed. In addition, the number N of extraction units 100 connected in series is preferably 2 to 10, and more preferably 3 to 7. When the number of stages N is large, the number of pumps required can be reduced by using a pressurized gas supply component 30 to transfer the solvent 22 (and the liquid raw material 12).

[0205] exist Figure 3 In the example shown, the washing apparatus includes three extraction units 100a, 100b, and 100c. In the washing apparatus of the second embodiment, the raw material tank 10 is connected to the first inflow hole 112 of the mixer 110 of the extraction unit 100a at the most upstream. In the washing apparatus of the second embodiment, in a pair of extraction units 100 connected in series (for example, adjacent extraction units 100a and 100b), the second outflow hole 144 of the extraction unit 100a on the upstream side is connected to the first inflow hole 112 of the mixer 110 of the extraction unit 100b on the downstream side. The same applies to the extraction units 100b and 100c connected in series. In the washing apparatus of the second embodiment, the solvent tank 20 is connected via the small diameter portion 40 (at Figure 3 In the case of three small diameter parts 40a, 40b, 40c) connected to at least two extraction units 100 (in Figure 3 In the case of the mixer 110, there are three extraction units 100a, 100b, 100c).

[0206] The pressure of the liquid at the first inflow hole 112 of the mixer 110 of the extraction unit 100 on the upstream side is preferably higher than the pressure of the liquid at the first inflow hole 112 of the mixer 110 of the extraction unit 100 on the downstream side. Figure 3 In the example shown, when the pressures of the liquid at the first inlet 112 of the mixer 110 of the extraction units 100a, 100b, and 100c are set to P1, P2, and P3, respectively, it is preferable that P1>P2>P3. By setting the liquid pressures in this manner, the flow of the liquid in the device of this embodiment can be optimized.

[0207] In the washing apparatus of the second embodiment, the small-diameter portion 40 connected to the second inflow hole 114 can be a small-diameter portion 40 having different pressure losses at the upstream small-diameter portion 40a and the downstream small-diameter portion 40b (or at the upstream small-diameter portion 40b and the downstream small-diameter portion 40c). By having different pressure losses at the multiple small-diameter portions 40a, 40b, and 40c, the flow rates of the liquid raw material 12, the solvent 22, and the mixed liquid of the liquid raw material 12 and the solvent 22 within the apparatus can be controlled to appropriate flow rates. As a result, the contaminants (extraction target substances) contained in the liquid raw material 12 can be efficiently extracted. Specifically, it is preferred that the small-diameter portions 40a, 40b, and 40c have the same inner diameter, and when the lengths of the small-diameter portions 40a, 40b, and 40c are set to L1, L2, and L3, respectively, L1 < L2 < L3. That is, the pressure loss of the solvent 22 in the small-diameter portion 40 for supplying the solvent 22 to the downstream extraction unit 100 is preferably greater than that in the small-diameter portion 40 for supplying the solvent 22 to the upstream extraction unit 100 .

[0208] In the device of this embodiment, as in the first embodiment, the small-diameter portions 40a, 40b, and 40c preferably further include a thermostat 46 for regulating the temperature of the small-diameter portions 40. By regulating the temperature of the small-diameter portions 40a, 40b, and 40c, the temperature of the solvent 22 in the small-diameter portions 40a, 40b, and 40c can be controlled. By controlling the temperature of the solvent 22, the physical properties of the solvent 22, such as its viscosity, can be changed. Therefore, the flow rate of the solvent 22 in each of the small-diameter portions 40a, 40b, and 40c can be controlled. Furthermore, the second small-diameter portions 70a, 70b, 70c, and 70d, described later, can also include a thermostat 46, similar to the small-diameter portions 40a, 40b, and 40c.

[0209] exist Figure 3 In the example shown, three pipes are connected to the solvent tank 20 and are respectively connected to the mixers 110 of different extraction units 100. Since a single pressurized gas supply unit 30 is required for transferring the solvent 22 from the solvent tank 20, the cost of the apparatus of this embodiment can be reduced and the apparatus structure can be simplified.

[0210] In the washing apparatus of the second embodiment, the flow path connected to the first recovery tank 50 and the second recovery tank 60 can be provided with second small-diameter portions 70a, 70b, 70c, and 70d. There is a situation where the flow rate flowing to the first recovery tank 50 and the second recovery tank 60 is unstable due to the height position of the pipes connected to the first recovery tank 50 and the second recovery tank 60. By providing the second small-diameter portions 70a, 70b, 70c, and 70d in the flow path connected to the first recovery tank 50 and the second recovery tank 60, the flow rate flowing to the first recovery tank 50 and the second recovery tank 60 is not easily changed, thereby stabilizing the flow rate. In addition, in the above-mentioned first embodiment, a second small-diameter portion can also be provided.

[0211] exist Figure 3 , an example is shown in which the pump 14 is used to transfer the liquid raw material 12. As described in the first embodiment, the liquid raw material 12 can also be transferred using the pressurized gas supply means 30 in the cleaning apparatus of the second embodiment.

[0212] In addition, as described in the description of the first embodiment, using Figure 8 In the illustrated reaction apparatus 210, liquid raw materials stored in two reaction apparatus raw material tanks 212a and 212b are mixed in a reaction apparatus mixer to obtain a reactant, the target substance, within the piping. The reactant obtained by reacting the substances contained in the two liquid raw materials can be used as the liquid raw material 12 of this embodiment. In the cleaning apparatus of the second embodiment, the reactant can be cleaned by extracting contaminants from the reactant.

[0213] <Third embodiment>

[0214] The third embodiment of this embodiment is an extraction device. The third embodiment of this embodiment is similar to the washing device of the second embodiment and can be used Figure 3 The extraction device of the third embodiment is the same as the cleaning device of the second embodiment except that the extraction target substance contained in the liquid raw material 12 is the target substance.

[0215] The extraction apparatus of this embodiment includes at least two extraction units 100 connected in series. By connecting at least two extraction units 100 in series, a larger amount of the target substance contained in the liquid raw material 12 can be extracted. As a result, a larger amount of the target substance can be extracted from the liquid raw material 12. Furthermore, the number N of extraction units 100 connected in series is preferably 2 to 10, more preferably 3 to 7. When the number N of stages is large, the number of pumps 14 required can be reduced by using a pressurized gas supply unit 30 to transfer the solvent 22 (and the liquid raw material 12).

[0216] exist Figure 3 , an example is shown in which the pump 14 is used to transfer the liquid raw material 12. As described in the first embodiment, in the extraction apparatus of the third embodiment, the liquid raw material 12 can also be transferred using the pressurized gas supply means 30.

[0217] In the device of this embodiment, as in the first embodiment, the small-diameter portions 40a, 40b, and 40c preferably further include a thermostat 46 for regulating the temperature of the small-diameter portions 40. By regulating the temperature of the small-diameter portions 40a, 40b, and 40c, the temperature of the solvent 22 in the small-diameter portions 40a, 40b, and 40c can be controlled. By controlling the temperature of the solvent 22, the physical properties of the solvent 22, such as its viscosity, can be changed. Therefore, the flow rate of the solvent 22 in each of the small-diameter portions 40a, 40b, and 40c can be controlled. Furthermore, similar to the small-diameter portions 40a, 40b, and 40c, the second small-diameter portions 70a, 70b, 70c, and 70d can also include a thermostat 46.

[0218] In addition, as described in the description of the first embodiment, using Figure 8 In the illustrated reaction apparatus 210, liquid raw materials stored in two reaction apparatus raw material tanks 212a and 212b are mixed in a reaction apparatus mixer to obtain a reactant, which is a target substance, within the piping. The reactant obtained by reacting the substances contained in the two liquid raw materials can be used as the liquid raw material 12 of this embodiment. In the extraction apparatus of the third embodiment, the reactant, which is a target substance, can be extracted from the liquid raw material 12.

[0219] <Fourth embodiment>

[0220] Figure 4 A schematic diagram of a fourth embodiment of this embodiment is shown. Figure 4 Although details of the interior of the extraction units 100a, 100b, and 100c are omitted, they are similar to the extraction unit 100 of the first embodiment described above. As described above, each of the three extraction units 100a, 100b, and 100c includes a mixer 110, an extraction unit 130, and a liquid separator 140. The apparatus of the fourth embodiment can be used as a washing apparatus or an extraction apparatus.

[0221] The apparatus of this embodiment comprises at least two extraction units 100 connected in parallel. This apparatus is a so-called mass-amplification device. By connecting at least two extraction units 100 in parallel, the amount of the target substance extracted per unit time can be increased. Consequently, the cost of extracting the target substance can be reduced.

[0222] exist Figure 4In the illustrated example, the apparatus includes three extraction units 100a, 100b, and 100c. In the apparatus of the fourth embodiment, the raw material tank 10 is connected to the first inlet 112 of the mixer 110 of at least two extraction units 100. In the apparatus of the fourth embodiment, the solvent tank 20 is connected to the second inlet 114 of the mixer 110 of at least two extraction units 100 via the small-diameter portion 40. With this structure, the apparatus of the fourth embodiment can connect the extraction units 100 in parallel, thereby increasing the amount of the extraction target substance extracted per unit time.

[0223] exist Figure 4 , an example is shown in which the pressurized gas supply means 30 is used to transfer the liquid raw material 12. As described in the first embodiment, in the apparatus of the fourth embodiment, the liquid raw material 12 can be transferred using the pump 14.

[0224] In the device of this embodiment, as in the first embodiment, it is preferable that the small diameter parts 40a, 40b, 40c further include a thermostat 46 for adjusting the temperature. By adjusting the temperature of the small diameter parts 40a, 40b, 40c, the temperature of the solvent 22 in the small diameter parts 40a, 40b, 40c can be controlled. By controlling the temperature of the solvent 22, the physical properties such as the viscosity of the solvent 22 can be changed, so the flow rate of the solvent 22 in the small diameter parts 40a, 40b, 40c can be controlled. In addition, the device of the fourth embodiment can have the following features as in the devices of the second and third embodiments: Figure 3 When the device of the fourth embodiment includes the second small diameter portions 70a, 70b, 70c, 70d, the second small diameter portions 70a, 70b, 70c, 70d can also be provided with the thermostat 46 similarly to the small diameter portions 40a, 40b, 40c.

[0225] In addition, as described in the description of the first embodiment, using Figure 8 The reaction device 210 shown in the figure can obtain a reactant as a target substance in the piping after the liquid raw materials accumulated in the two reaction device raw material tanks 212a and 212b are mixed by the reaction device mixer. The reactant obtained by reacting the substances contained in the two liquid raw materials can be used as the liquid raw material 12 of this embodiment. The device of the fourth embodiment can be a washing device for washing the reactant by extracting contaminants from the reactant. In addition, the device of the fourth embodiment can be an extraction device for extracting the reactant as the target substance from the liquid raw material 12.

[0226] <Fifth embodiment>

[0227] The apparatus of the fifth embodiment of the present embodiment is an apparatus that replaces the at least two extraction units 100 connected in parallel in the fourth embodiment with a set of extraction units 100 (a set of at least two extraction units 100 connected in series) of the apparatuses of the second and third embodiments as the extraction units 100. In other words, the apparatus of the fifth embodiment is a combination of the apparatuses of the second and third embodiments, which connect at least two extraction units 100 in series, and the apparatus of the fourth embodiment, which connects at least two extraction units 100 in parallel.

[0228] The apparatus of the fifth embodiment, by connecting at least two extraction units 100 in series, can extract a greater amount of the target substance contained in the liquid raw material 12. As a result, washing the liquid raw material 12 and extracting the target substance from the liquid raw material 12 can be performed more reliably. Furthermore, the apparatus of the fifth embodiment of this embodiment, by connecting at least two extraction units 100 in parallel, can increase the amount of target substance extracted per unit time. Consequently, the cost of extracting the target substance can be reduced.

[0229] As described in the first embodiment, in the apparatus of the fifth embodiment, the pressurized gas supply unit 30 can be used to transfer the liquid raw material 12. Also, as described in the first embodiment, in the apparatus of the fifth embodiment, the pump 14 can be used to transfer the liquid raw material 12.

[0230] In the device of this embodiment, as in the first embodiment, it is preferable that the plurality of small diameter portions 40 further include a thermostat 46 for temperature control. Furthermore, the second small diameter portions 70a, 70b, 70c, and 70d can also include a thermostat 46 similar to the small diameter portions 40a, 40b, and 40c.

[0231] In addition, as described in the description of the first embodiment, using Figure 8 The reactor 210 shown is capable of obtaining a target reactant within a pipe after the liquid raw materials stored in two reactor raw material tanks 212a and 212b are mixed by a reactor mixer. The reactant obtained by reacting the substances contained in the two liquid raw materials can be used as the liquid raw material 12 of the fifth embodiment. The apparatus of the fifth embodiment can be a washing apparatus for washing the reactants by extracting contaminants from the reactants. Alternatively, the apparatus of the fifth embodiment can be an extraction apparatus for extracting the target reactant from the liquid raw material 12.

[0232] In the apparatus of the fifth embodiment, the number N of extraction units 100 connected in series and in parallel is preferably 2 to 10, more preferably 3 to 7. When the number N is large, the number of pumps 14 required can be reduced by using the pressurized gas supply unit 30 to transfer the solvent 22 (and the liquid raw material 12).

[0233] <Sixth embodiment>

[0234] The sixth embodiment of this embodiment is an extraction and washing device that has the functions of both an extraction device and a washing device. The device of the sixth embodiment of this embodiment can be used Figure 9 In addition, the Figure 9 Although details of the interior of the three extraction units 100a, 100b, and 100c are omitted, they are the same as the extraction unit 100 of the first embodiment described above. As described in the first embodiment, the three extraction units 100a, 100b, and 100c each include a mixer 110, an extraction unit 130, and a liquid separation unit 140.

[0235] The apparatus of the sixth embodiment of the present embodiment includes at least two extraction units 100 connected in series. The raw material tank 10 of the apparatus of the sixth embodiment is connected to the first inflow port 112 of the pre-mixer 110 of the extraction unit 100a at the most upstream end. The apparatus of the sixth embodiment of the present embodiment preferably includes at least three extraction units 100 connected in series. The upper limit of the number of extraction units 100 is preferably 10 or less, and more preferably 5 or less.

[0236] In the device of the sixth embodiment, in at least one pair of extraction units 100 connected in series, the first outflow hole 142 of the extraction unit 100 on the upstream side is connected to the first inflow hole 112 of the mixer 110 of the extraction unit 100 on the downstream side. Figure 9 In the example shown, the first outflow hole 142 of the extraction unit 100a at the most upstream is connected to the first inflow hole 112 of the mixer 110 of the extraction unit 100b at the downstream side. The extraction unit 100a in this case can function as an extraction device. Therefore, in the extraction unit 100a, the extraction object substance contained in the liquid raw material 12 is the target substance. The target substance extracted by the solvent 22a flows out from the first outflow hole 142 of the extraction unit 100a. In addition, the second outflow hole 144 of the extraction unit 100a is connected to the second recovery tank 60. The liquid (second recovered liquid 62) after the target substance is extracted from the liquid raw material 12 is recovered in the second recovery tank 60.

[0237] like Figure 9As shown, in the device of the sixth embodiment, it is preferred that, in the most upstream extraction unit 100a and the extraction unit 100b connected in series with the most upstream extraction unit 100a, the first outflow hole 142 of the most upstream extraction unit 100a is connected to the first inflow hole 110 of the extraction unit 100b on the downstream side.

[0238] In the device of the sixth embodiment, it is preferred that, in at least one pair of extraction units 100 connected in series, the second outflow hole 144 of the extraction unit 100 on the upstream side is connected to the first inflow hole 112 of the mixer 110 of the extraction unit 100 on the downstream side. Figure 9 In the example shown, the second outflow hole 144 of the second extraction unit 100b is connected to the first inflow hole 112 of the mixer 110 of the downstream extraction unit 100c. The extraction unit 100b functions as a washing device. Therefore, in the extraction unit 100b, the contaminants contained in the liquid are the target substances. The liquid washed with the solvent 22b flows out from the second outflow hole 144 of the extraction unit 100b. In addition, the first recovery tank 50 is connected to the first outflow hole 142 of the extraction unit 100b. The liquid (first recovered liquid 52) containing the solvent 22b and the contaminants is recovered in the first recovery tank 50.

[0239] In the device of the sixth embodiment, the extraction unit 100c on the downstream side of the second extraction unit 100b can function as a washing device in the same manner as the second extraction unit 100b. Therefore, in the extraction unit 100c, the pollutants contained in the liquid can be the target substance. The liquid washed by the solvent 22b flows out from the second outflow hole 144 of the extraction unit 100c. Therefore, the second recovery liquid containing the washed substance is recovered in the second recovery tank 60 connected to the second outflow hole 144. In addition, the first recovery tank 50 is connected to the first outflow hole 142 of the extraction unit 100b. The liquid (first recovery liquid 52) containing the solvent 22b and the pollutants is recovered in the first recovery tank 50.

[0240] The device of the sixth embodiment preferably includes at least two solvent tanks 20. In addition, it is preferred that each of the solvent tanks 20 stores a different solvent 22. Figure 9 As shown, in the extraction and washing apparatus of the sixth embodiment, at least two solvent tanks 20a and 20b store different solvents 22 (a first solvent 22a and a second solvent 22b). For example, when there are two solvent tanks 20, a solvent 22 for extracting the target substance can be stored in one solvent tank 20. In addition, a solvent 22 for washing can be stored in the other solvent tank 20. Figure 9In the example shown, solvent tank 20a connected to extraction unit 100a can store solvent 22a for extracting the target substance. Furthermore, solvent tank 20b connected to extraction units 100b and 100c can store solvent 22b for washing. As a result, extraction unit 100a can function as an extraction device, while extraction units 100b and 100c can function as washing devices.

[0241] Furthermore, when two different solvents 22 are present, it is preferred that one be a hydrophobic solvent and the other be a hydrophilic solvent. If the liquid raw material 12 is hydrophobic, the solvent 22a stored in the first solvent tank 20a connected to the most upstream extraction unit 100a is preferably hydrophilic. Furthermore, if the liquid raw material 12 is hydrophilic, the solvent 22a stored in the first solvent tank 20a connected to the most upstream extraction unit 100a is preferably hydrophobic. By ensuring that the liquid raw material 12 and the specified solvent 22a have a specified hydrophilicity or hydrophobicity, efficient extraction and washing of the target substance from the liquid raw material 12 can be achieved. Furthermore, the solvent 22a stored in the first solvent tank 20a connected to the most upstream extraction unit 100a and the solvent 22b stored in the second solvent tank 20b connected to the extraction units 100b and 100c other than the most upstream extraction unit 100a are preferably different types of solvents (hydrophilic or hydrophobic). By using different types of solvents for both, extraction and washing by the apparatus of the sixth embodiment can be facilitated.

[0242] In the apparatus of the sixth embodiment, the solvent tank 20 is connected to the mixer 110 of the extraction unit via the small-diameter portion 40. Similar to the apparatus of the second embodiment, in the apparatus of the sixth embodiment, the small-diameter portion 40 connected to the second inlet port 114 can be a small-diameter portion 40 having different pressure losses at the upstream small-diameter portion 40a and the downstream small-diameter portion 40b (or at the upstream small-diameter portion 40b and the downstream small-diameter portion 40c). Furthermore, similar to the apparatus of the second embodiment, in the apparatus of the sixth embodiment, second small-diameter portions 70a, 70b, 70c, and 70d can be provided in the flow paths connected to the first recovery tank 50 and the second recovery tank 60.

[0243] As mentioned above, in Figure 9 In the extraction and cleaning apparatus of the sixth embodiment shown, extraction unit 100a functions as an extraction apparatus, while extraction units 100b and 100c function as cleaning apparatuses. Alternatively, extraction unit 100a, located at the most upstream end, can function as a cleaning apparatus. In this case, extraction units 100b and / or 100c, located at the most upstream end, can function as extraction apparatuses.

[0244] In addition, Figure 9, one extraction unit 100a having a function as an extraction device and two extraction units 100b and 100c having a function as a washing device are illustrated, but the present invention is not limited thereto. The extraction and washing device of the sixth embodiment can have at least one extraction unit 100 having a function as an extraction device and at least one extraction unit 100 having a function as a washing device. The number N1 of extraction units 100 having a function as an extraction device is preferably 1 to 5, more preferably 1 to 3. In addition, the number N2 of extraction units 100 having a function as a washing device is preferably 1 to 5, more preferably 1 to 3. When the total number of stages N1+N2 is large, the number of pumps required can be reduced by using a pressurized gas supply component 30 to transfer the solvent 22 (and the liquid raw material 12).

[0245] <Other Implementation Methods>

[0246] (1) In the above embodiment, an example is shown in which the number of the raw material tank 10 and the number of the solvent tank 20 is one, but the number of the raw material tank 10 and the solvent tank 20 is not limited to this.

[0247] (2) In the above embodiment, an example is shown in which the material of the pipe is resin, but the material of the pipe is not limited to this. The pipe may be formed of metal, for example.

[0248] (3) In the above embodiment, the small-diameter portion 40 is an example of a resin tube, but the small-diameter portion 40 is not limited to this. The small-diameter portion 40 may also be formed of a metal tube, for example. In addition, a known needle valve, back pressure tube, or back pressure regulator used to adjust the back pressure of HPLC or ion chromatography may also be used as the small-diameter portion 40.

[0249] (4) In the above embodiment, the gas used to transfer the liquid raw material 12 is nitrogen gas, but the type of gas is not limited to this. The gas used to transfer the liquid raw material 12 may be air or argon gas, for example.

[0250] [Example]

[0251] Hereinafter, embodiments of the present invention will be described using examples.

[0252] (Example 1)

[0253] In Example 1, the device shown in the first embodiment (see Figure 1 ) is applied to the cleaning of propionic acid. Specifically, the cleaning of Example 1 is performed by extracting the metal ions (contaminants as the extraction target substance) contained in the propionic acid as the liquid raw material 12 into the solvent 22 as ultrapure water. The metal ions can be easily extracted using ultrapure water.

[0254] In addition, in Example 1, the Figure 1 The same device as shown in FIG. As the piping for connecting each part, piping with an outer diameter of 1 / 8 inch and an inner diameter of 1.58 mm was used.

[0255] 30 g of propionic acid and 170 g of toluene (Kanto Chemical, Primepure standard) were mixed to obtain 200 g of a liquid raw material 12. The obtained liquid raw material 12 was stored in a raw material tank 10.

[0256] Ultrapure water was stored as the washing solvent 22 in a polypropylene solvent tank 20. A PEEK tube with an inner diameter of 0.25 mm and a length of 150 mm was placed midway in the piping connecting the solvent tank 20 to the mixer 110 of the extraction unit 100 as a small-diameter portion 40. Furthermore, the inner diameters of the piping connected upstream (first solvent piping 42) and downstream (second solvent piping 44) of the small-diameter portion 40 were 1.58 mm.

[0257] The liquid raw material 12 in the raw material tank 10 was fed to the mixer 110 by a plunger pump (pump 14). The flow rate of the liquid raw material 12 at this time was set to 2.0 ml / min.

[0258] The cleaning solvent 22 stored in the solvent tank 20 is fed to the mixer 110 by the pressure of nitrogen gas (pressurized gas supply means 30). At this time, the pressure in the solvent tank 20 is adjusted to 50 kPa.

[0259] A mixer-settler (manufactured by MAK Engineering, model number MS-L-IT-02-00-00) was used as the mixer 110 and liquid separator 140 of the extraction unit 100 of Example 1. The liquid raw material 12 and the washing solvent 22 were mixed using the mixer 110, which had a Y-shaped microchannel with a width of 0.8 mm, formed therein.

[0260] The mixer 110 and the clarifier (liquid separator 140) built into the mixer-settler are connected by a PTFE pipe having an outer diameter of 1 / 16 inch, an inner diameter of 1 mm, and a length of 5 m, serving as the extraction section 130. The liquid raw material 12 and the solvent 22 mixed in the mixer 110 are allowed to flow through the pipe (extraction section 130), whereby the liquid raw material 12 and the solvent 22 form a slug flow in the pipe (extraction section 130), and the metal component, the extraction target substance, in the liquid raw material 12 is extracted into the ultrapure water serving as the washing solvent 22.

[0261] The mixed liquid of liquid raw material 12 and solvent 22 sent from extraction unit 100 to the clarifier (liquid separator 140) is separated in the clarifier into solvent 22 containing the metal component (first recovered liquid 52) and the remaining liquid (second recovered liquid 62). First recovered liquid 52 and second recovered liquid 62 are sent to first recovery tank 50 and second recovery tank 60, respectively.

[0262] Table 1 shows the results (weight ratios) of metal content measurement in the toluene solution of propionic acid before washing and in the toluene solution of propionic acid after washing recovered in the second recovery tank 60. The measurement was performed using ICP-MS (inductively coupled plasma mass spectrometry). As can be seen from Table 1, according to Example 1, the metal components in propionic acid were effectively extracted and removed into ultrapure water as the solvent 22, thereby enabling washing of the propionic acid.

[0263] In the apparatus of Example 1, the solvent 22 stored in the solvent tank 20 is fed to the mixer 110 by the pressurized gas supply unit 30. Therefore, the apparatus of Example 1 is an apparatus capable of more easily extracting the extraction target substance contained in the liquid raw material.

[0264]

Table 1

[0265] Na(ppb) Mg(ppb) Ca(ppb) Ti(ppb) Before washing 75.2 36.7 517.7 15.5 After washing 17.5 1.9 125.9 1.8

[0266] (Example 2)

[0267] In Example 2, the device shown in the second embodiment (see Figure 3 ) removes the water-soluble monomers (pollutants as the extraction target substances) in the phenolic resin, thereby washing the phenolic resin. In Example 2, as Figure 3 As shown, three sets of extraction units 100a, 100b, and 100c were connected in series and used, and three consecutive washings were performed using the three sets of extraction units 100a, 100b, and 100c.

[0268] In addition, in Example 2, the Figure 3 The same device as shown is used except that the second small diameter portions 70a, 70b, 70c, 70d and the valve 150 are not provided. As pipes for connecting the various parts, pipes having an outer diameter of 1 / 8 inch and an inner diameter of 1.58 mm are used.

[0269] 2.0 g of phenol resin was dissolved in 198 g of ethyl acetate to obtain 200 g of liquid raw material 12. The obtained liquid raw material 12 was stored in the raw material tank 10.

[0270] Ion-exchanged water, serving as a washing solvent 22, is stored in a solvent tank 20. Three flow paths are connected to the solvent tank 20, each connected to the mixer 110 of the extraction units 100a, 100b, and 100c. PEEK tubes with an inner diameter of 0.25 mm and a length of 150 mm are disposed midway along the piping connecting the solvent tank 20 to the mixer 110, serving as small-diameter sections 40a, 40b, and 40c. Furthermore, the piping (first solvent piping 42 and second solvent piping 44) connected to the small-diameter sections 40a, 40b, and 40c) has an inner diameter of 1.58 mm.

[0271] The liquid raw material 12 in the raw material tank 10 was fed to the mixer 110 by a plunger pump (pump 14). The flow rate of the liquid raw material 12 at this time was set to 2.0 ml / min.

[0272] The ion-exchanged water stored in the solvent tank 20 is fed to the mixers 110 of the extraction units 100a, 100b, and 100c using the pressure of nitrogen gas (pressurized gas supply means 30). At this time, the pressure in the tank is adjusted to 50 kPa.

[0273] A mixer-settler (manufactured by MAK Engineering, model number MS-L-IT-02-00-00) was used as the mixer 110 and liquid separator 140 of the extraction units 100a, 100b, and 100c of Example 2. The liquid raw material 12 and the washing solvent 22 were mixed using the mixer 110, which had a Y-shaped microchannel with a width of 0.8 mm, formed therein.

[0274] The mixer 110 and the clarifier (liquid separator 140) built into the mixer-settler are connected by a PTFE pipe having an outer diameter of 1 / 8 inch, an inner diameter of 1.58 mm, and a length of 3 m, serving as the extraction section 130. The liquid raw material 12 and the solvent 22 mixed in the mixer 110 are allowed to flow through the pipe (extraction section 130), whereby the liquid raw material 12 and the solvent 22 form a slug flow in the pipe, and the monomer of the extraction target substance in the liquid raw material 12 is extracted into the ion-exchanged water serving as the washing solvent 22.

[0275] The mixed liquid of liquid raw material 12 and solvent 22 sent from extraction section 130 to clarifier (liquid separator 140) is separated in the clarifier into solvent 22 containing monomer (first recovered liquid 52) and liquid other than the solvent (second recovered liquid 62). First recovered liquid 52 is sent to first recovery tank 50.

[0276] The second recovered liquid 62 (liquid obtained by removing monomers from the liquid raw material 12) flowing out of the clarifier of the first extraction unit 100a is transported to the mixer 110 of the second extraction unit 100b, and the second recovered liquid 62 is mixed with the washing solvent 22 transported from the solvent tank 20 by the mixer 110.

[0277] The liquid mixed in mixer 110 forms a slug flow in the piping of extraction section 130. The monomers in liquid raw material 12 contained in second recovered liquid 62 are extracted into washing solvent 22, thereby being washed and transported to a clarifier (liquid separator 140). In the clarifier, the liquid is separated into solvent 22 containing the monomers (first recovered liquid 52) and the remaining liquid (second recovered liquid 62). First recovered liquid 52 is transported to first recovery tank 50.

[0278] The second recovered liquid 62 (the liquid after the monomers have been removed from the liquid raw material 12) flowing out of the clarifier of the second extraction unit 100b is similarly conveyed to the mixer 110 of the third extraction unit 100c. The second recovered liquid 62 is mixed with the washing solvent 22 in the mixer 110. The monomers are extracted into the solvent 22 by the extraction unit 130, thereby washing the solvent. The second recovered liquid 62 is then conveyed to the clarifier (liquid separation unit 140). In the clarifier, the liquid is separated into the solvent 22 containing the monomers (the first recovered liquid 52) and the remaining liquid (the second recovered liquid 62). The first recovered liquid 52 and the second recovered liquid 62 are conveyed to the first recovery tank 50 and the second recovery tank 60, respectively.

[0279] Table 2 shows the results of GPC (Gel Permeation Chromatography) measurements (peak area ratio of UV absorption at 254 nm) of the monomer component ratio (%) in the phenolic resin before washing and after washing in each washing step. As can be seen from Table 2, according to Example 2, the phenolic resin can be effectively washed by extracting and removing the monomers serving as the extraction target substance in the phenolic resin with ultrapure water as the solvent 22.

[0280] In the apparatus of Example 2, the solvent 22 stored in the solvent tank 20 is fed to the mixer 110 by the pressurized gas supply unit 30. Therefore, the apparatus of Example 2 is an apparatus capable of more easily extracting a target substance contained in a liquid raw material.

[0281]

Table 2

[0282]

[0283] (Example 3)

[0284] In Example 3, the apparatus shown in the third embodiment was applied to the extraction of propionic acid (target substance). Figure 3 As shown, three sets of extraction units 100a, 100b, and 100c were connected in series and used, and three extractions were performed continuously using the three sets of extraction units 100a, 100b, and 100c.

[0285] In addition, in Example 3, the Figure 3 The same device as shown is used except that the second small diameter portions 70a, 70b, 70c, 70d and the valve 150 are not provided. As pipes for connecting the various parts, pipes having an outer diameter of 1 / 8 inch and an inner diameter of 1.58 mm are used.

[0286] 40 g of propionic acid and 160 g of ion-exchanged water were mixed to obtain 200 g of a liquid raw material 12. The obtained liquid raw material 12 was stored in a raw material tank 10.

[0287] Toluene, serving as the extraction solvent 22, was stored in a solvent tank 20. Three flow paths were connected to the solvent tank 20, each connected to the mixer 110 of the extraction units 100a, 100b, and 100c. PEEK tubes with an inner diameter of 0.25 mm and a length of 150 mm were positioned midway along the piping connecting the solvent tank 20 to the mixer 110, serving as small-diameter sections 40a, 40b, and 40c. Furthermore, the piping (first solvent piping 42 and second solvent piping 44) connected to the small-diameter sections 40a, 40b, and 40c had an inner diameter of 1.58 mm.

[0288] The liquid raw material 12 in the raw material tank 10 was fed to the mixer 110 by a plunger pump (pump 14). The flow rate of the liquid raw material 12 at this time was set to 2.0 ml / min.

[0289] The toluene stored in the solvent tank 20 is fed to the mixers 110 of the extraction units 100a, 100b, and 100c using the pressure of nitrogen (pressurized gas supply means 30). At this time, the pressure in the tank is adjusted to 75 kPa.

[0290] A mixer-settler (manufactured by MAK Engineering, model number MS-L-IT-02-00-00) was used as the mixer 110 and liquid separator 140 of the extraction units 100a, 100b, and 100c of Example 3. The liquid raw material 12 and the extraction solvent 22 were mixed using the mixer 110, which had a Y-shaped microchannel with a width of 0.8 mm, formed therein.

[0291] The mixer 110 and the clarifier (liquid separator 140) built into the mixer-settler are connected by a PTFE pipe having an outer diameter of 1 / 16 inch, an inner diameter of 1 mm, and a length of 5 m, serving as the extraction section 130. The liquid raw material 12 and the solvent 22 mixed in the mixer 110 are allowed to flow through the pipe (extraction section 130), whereby the liquid raw material 12 and the solvent 22 form a slug flow in the pipe, and the propionic acid in the liquid raw material 12 is extracted into the toluene serving as the extraction solvent 22.

[0292] The mixed liquid of liquid raw material 12 and solvent 22, which is fed from extraction section 130 to clarifier (liquid separator 140), is separated in the clarifier into solvent 22 containing propionic acid (first recovered liquid 52) and liquid other than the solvent 22 (second recovered liquid 62). First recovered liquid 52 is fed to second recovery tank 60. Second recovered liquid 62 (the liquid after propionic acid has been recovered from liquid raw material 12) contains incompletely recovered propionic acid.

[0293] The second recovered liquid 62 (liquid after propionic acid is recovered from the liquid raw material 12) flowing out of the clarifier of the first extraction unit 100a is transported to the mixer 110 of the second extraction unit 100b, and the second recovered liquid 62 is mixed with the extraction solvent 22 transported from the extraction solvent tank 20 by the mixer 110.

[0294] The liquids mixed in mixer 110 form a slug flow in the piping of extraction section 130. Propionic acid in liquid feedstock 12, contained in second recovered liquid 62, is extracted into extraction solvent 22. This liquid is then transported to a clarifier (liquid separator 140). In the clarifier, this liquid is separated into solvent 22 containing the monomer (first recovered liquid 52) and the remaining liquid (second recovered liquid 62). First recovered liquid 52 is then transported to first recovery tank 50.

[0295] The liquid feedstock 12 flowing out of the clarifier of the second extraction unit 100b is similarly conveyed to the mixer 110 of the third extraction unit 100c. The liquid feedstock 12 is mixed with the extraction solvent 22 in the mixer 110, and propionic acid is extracted in the extraction section 130. The liquid feedstock 12 is then conveyed to the clarifier (liquid separation section 140). The clarifier separates the liquid feedstock 12 into the solvent 22 containing propionic acid (first recovered liquid 52) and the remaining liquid (second recovered liquid 62). The first recovered liquid 52 and the second recovered liquid 62 are conveyed to the first recovery tank 50 and the second recovery tank 60, respectively.

[0296] The recovery rate of propionic acid extracted into toluene was calculated based on the concentration measurement results using GC (Gas Chromatograph). Table 3 shows the recovery rate of propionic acid in Example 3. As shown in Table 3, in Example 3, propionic acid, the target substance, can be efficiently extracted by extracting propionic acid from ion-exchanged water into toluene, the solvent 22.

[0297] In the apparatus of Example 3, the solvent 22 stored in the solvent tank 20 is fed to the mixer 110 by the pressurized gas supply unit 30. Therefore, the apparatus of Example 3 is an apparatus capable of more easily extracting a target substance contained in a liquid raw material.

[0298]

Table 3

[0299]

[0300] (Experimental Examples 1 and 2)

[0301] In Experimental Examples 1 and 2, Figure 3 In the apparatus shown, as Experimental Example 1, a liquid raw material 12 and a solvent 22 were removed from a raw material tank 10 and a solvent tank 20 using a plunger pump 14. Furthermore, as Experimental Example 2, a liquid raw material 12 was removed from the raw material tank 10 using a plunger pump 14, and a solvent 22 was removed from the solvent tank 20 using a pressurized gas supply unit 30.

[0302] (Experimental Example 1)

[0303] In Experimental Example 1, Figure 3 In the illustrated apparatus, a single plunger pump (pump 14) is used to deliver liquid raw material 12 from a raw material tank 10 to the first extraction unit 100a. Furthermore, three plunger pumps 14 are used to deliver solvent 22 from a solvent tank 20 to the three extraction units 100a, 100b, and 100c. Water is stored in the raw material tank 10 as the liquid raw material 12. Toluene is stored in the solvent tank 20 as the solvent 22. The flow rate of the liquid raw material 12 to the extraction unit 100a is set to 5.0 ml / min, and the flow rate of the solvent 22 to the extraction units 100a, 100b, and 100c is set to 3.5 ml / min, respectively.

[0304] exist Figure 3 In the device shown in FIG. , small-diameter portions 40a, 40b, and 40c are disposed between the solvent tank 20 and the extraction unit 100. However, in Experimental Example 1, the plunger pump 14 is used to transfer the solvent 22 from the solvent tank 20. Therefore, the small-diameter portions 40a, 40b, and 40c are not required to control the flow rate of the solvent 22. Therefore, in Experimental Example 1, the small-diameter portions 40a, 40b, and 40c are not disposed.

[0305] In Experimental Example 1, in order to stabilize the flow rate of the solvent 22 flowing out of the first outflow hole 142 into the first recovery tank 50, second small-diameter portions 70a, 70b, and 70c were disposed between the first outflow hole 142 and the first recovery tank 50. Furthermore, a second small-diameter portion 70d was disposed between the second outflow hole 144 and the second recovery tank 60. The second small-diameter portions 70a, 70b, 70c, and 70d of Experimental Example 1 were PEEK tubes. From the upstream side, the dimensions of the second small-diameter portion 70a were 0.125 mm in inner diameter and 50 mm in length; the dimensions of the second small-diameter portion 70b were 0.25 mm in inner diameter and 375 mm in length; and the dimensions of the second small-diameter portion 70c were 0.25 mm in inner diameter and 100 mm in length. A PEEK tube with an inner diameter of 0.5 mm and a length of 100 mm is installed as a second small diameter portion 70d before the second recovery tank 60. The inner diameter of the pipes on the upstream and downstream sides of the second small diameter portions 70a, 70b, 70c, and 70d is 1.58 mm.

[0306] As in Example 1 above, a mixer-settler (manufactured by MAK Engineering, Model MS-L-IT-02-00-00) was used as the mixer 110 and liquid separator 140 of the extraction unit 100 of Experimental Example 1. The liquid raw material 12 and the washing solvent 22 were mixed using the mixer 110, which had a Y-shaped microchannel with a width of 0.8 mm, formed therein. The extraction unit 130 and clarifier (liquid separator 140) of the extraction unit 100 were the same as those of Example 1.

[0307] The apparatus of Experimental Example 1 was operated, and as a result, the liquid levels in the clarifiers of the three extraction units 100a, 100b, and 100c were stable. Therefore, it was found that the apparatus of Experimental Example 1 could be used to perform three consecutive washing or extractions.

[0308] (Experimental Example 2)

[0309] In Experimental Example 2, the same method as in Experimental Example 1 was used except that a pressurized gas supply unit 30 was used to supply the solvent 22 from the solvent tank 20 to the three extraction units 100a, 100b, and 100c, small-diameter portions 40a, 40b, and 40c were provided, and the sizes of the second small-diameter portions 70a, 70b, 70c, and 70d were changed. Figure 3 The flow rate of solvent 22 was measured using the same apparatus as shown.

[0310] As in Experimental Example 1, water was stored in the raw material tank 10 as the liquid raw material 12, and toluene was stored in the solvent tank 20 as the solvent 22. As in Experimental Example 1, the flow rate of the liquid raw material 12 to the extraction unit 100a was set to 5.0 ml / min.

[0311] In Experimental Example 2, toluene (solvent 22) stored in the solvent tank 20 was fed to the mixer 110 using nitrogen pressure. At this time, the pressure in the tank was adjusted to 422 kPa by the pressure regulator 34 of the pressurized gas supply unit 30 .

[0312] In Experimental Example 2, small-diameter sections 40a, 40b, and 40c were positioned between the solvent tank 20 and the extraction unit 100. These sections 40a, 40b, and 40c in Experimental Example 2 were made of PEEK tubes. From the upstream side, the dimensions of small-diameter section 40a were 0.5 mm inner diameter and 100 mm long; small-diameter section 40b was 0.25 mm inner diameter and 150 mm long; and small-diameter section 40c was 0.25 mm inner diameter and 300 mm long. Furthermore, the inner diameters of the pipes upstream and downstream of small-diameter sections 40a, 40b, and 40c (first solvent pipe 42 and second solvent pipe 44) were 1.58 mm.

[0313] In addition, a valve (not shown) for finely adjusting the flow rate is provided between the small-diameter portion 40 and the extraction unit 100 .

[0314] In Experimental Example 2, similar to Experimental Example 1, second small-diameter portions 70a, 70b, and 70c were positioned between the first outflow hole 142 and the first recovery tank 50 to stabilize the flow rate of the solvent 22 flowing out of the first outflow hole 142 into the first recovery tank 50. Furthermore, a second small-diameter portion 70d was positioned between the second outflow hole 144 and the second recovery tank 60. The materials and dimensions of the second small-diameter portions 70a, 70b, 70c, and 70d were the same as those in Experimental Example 1. Specifically, the second small-diameter portions 70a, 70b, 70c, and 70d in Experimental Example 2 were PEEK tubes. From the upstream side, the dimensions of the second small-diameter portion 70a were 0.125 mm in inner diameter and 50 mm in length; the dimensions of the second small-diameter portion 70b were 0.25 mm in inner diameter and 375 mm in length; and the dimensions of the second small-diameter portion 70c were 0.25 mm in inner diameter and 100 mm in length. In addition, similarly to Experimental Example 1, a PEEK tube with an inner diameter of 0.5 mm and a length of 100 mm was installed as the second small-diameter portion 70d before the second recovery tank 60. Also, similarly to Experimental Example 1, the inner diameter of the pipes on the upstream and downstream sides of the second small-diameter portions 70a, 70b, 70c, and 70d was 1.58 mm.

[0315] Similar to Example 1 and Experimental Example 1 described above, a mixer-settler (manufactured by MAK Engineering, model number MS-L-IT-02-00-00) was used as the mixer 110 and liquid separator 140 of the extraction unit 100 of Experimental Example 2. The mixer 110, which had a Y-shaped microchannel with a width of 0.8 mm, was built into the mixer-settler to mix the liquid raw material 12 with the washing solvent 22.

[0316] The mixer 110 and the clarifier, built into the mixer-settler, are connected by a PTFE pipe with an outer diameter of 1 / 16 inch, an inner diameter of 1 mm, and a length of 5 m, serving as the extraction section 130. The liquid raw material 12 and solvent 22 mixed in the mixer 110 flow through this pipe (extraction section 130), forming a slug flow within the pipe. The mixed liquid of the liquid raw material 12 and solvent 22, transported from the extraction section 130 to the clarifier (liquid separator 140), is separated in the clarifier into the solvent 22 (first recovered liquid 52) and the remaining liquid, namely the liquid raw material 12 (second recovered liquid 62). The first recovered liquid 52 is transported to the first recovery tank 50.

[0317] like Figure 3 As shown, in the apparatus of Experimental Example 2, three extraction units 100a, 100b, and 100c are arranged in series. The apparatus of Experimental Example 2 was operated under the above-described conditions, and as a result, the flow rate of the solvent 22 flowing into the first extraction unit 100a on the most upstream side was 3.6 ml / min. Furthermore, the pressure of the extraction section 130 at this time was 402 kPa, and the difference between the pressure of the extraction section 130 and the pressure of the solvent tank 20 (pressure of the solvent tank 20 minus the pressure of the extraction section 130) was 19 kPa. As a result, the first recovery liquid 52 could be recovered at a flow rate of 3.6 ml / min in the first recovery tank 50 connected to the extraction unit 100a.

[0318] Furthermore, the flow rate of solvent 22 flowing into the second extraction unit 100b downstream of the first extraction unit 100a can be set to 3.5 ml / min. Furthermore, the pressure in the extraction section 130 at this time is 156 kPa, and the difference between the pressure in the extraction section 130 and the pressure in the solvent tank 20 (pressure in the solvent tank 20 minus the pressure in the extraction section 130) is 265 kPa. As a result, the first recovered liquid 52 can be recovered in the first recovery tank 50 connected to the extraction unit 100b at a flow rate of 3.6 ml / min.

[0319] Furthermore, the flow rate of the solvent 22 flowing into the third extraction unit 100c downstream of the second extraction unit 100b can be set to 3.4 ml / min. Furthermore, the pressure of the extraction section 130 at this time is 63 kPa, and the difference between the pressure of the extraction section 130 and the pressure of the solvent tank 20 (pressure of the solvent tank 20 minus the pressure of the extraction section 130) is 360 kPa. As a result, the first recovered liquid 52 can be recovered at a flow rate of 3.6 ml / min in the first recovery tank 50 connected to the extraction unit 100c. Furthermore, the second recovered liquid 62 can be recovered at a flow rate of 5 ml / min in the second recovery tank 60 connected to the extraction unit 100c.

[0320] As described above, it can be seen that in Experimental Example 2, by using the pressurized gas supply component 30 to pressurize the solvent tank 20 to an appropriate pressure and appropriately selecting the dimensions (inner diameter and length) of the small-diameter portions 40a, 40b, and 40c, as in the case of Experimental Example 1, even when the three extraction units 100a, 100b, and 100c are arranged in series, an appropriate flow of fluid can be generated within the device. Therefore, it can be seen that, as with the device of Experimental Example 1, the device of Experimental Example 2 can be used to perform three consecutive washing or extractions. In addition, compared to Experimental Example 1, in Experimental Example 2, the number of expensive plunger pumps used can be reduced. Therefore, it can be seen that according to the device of this embodiment, a device can be obtained that can more easily extract the extraction target substance contained in the liquid raw material.

[0321] (Example 4)

[0322] As described above, it can be seen that the device of Experimental Example 2 can be used to extract the specified extraction target substance dissolved in the liquid raw material. Therefore, the device of Experimental Example 2 can be used as the extraction device of this embodiment. To confirm this, as Example 4, the extraction target substance (target substance) was extracted from the liquid raw material using the same device as used in Experimental Example 2.

[0323] In Example 4, the same apparatus as that used in Experimental Example 2 was used (with Figure 3 Using the same apparatus as shown in the figure, propionic acid was extracted and recovered from a 20% aqueous solution of propionic acid (liquid feedstock) using toluene as the solvent, as in Example 3 above. The aqueous solution of propionic acid was pumped at a rate of 5 ml / min by a plunger pump, while toluene was delivered to the three extraction units by pressure feeding. As described below, the propionic acid recovery rate in the apparatus of Example 4 was 88%. Example 4 is described in detail below.

[0324] In Example 4, similar to Experimental Example 2, Figure 3 That is, a pressurized gas supply unit 30 is used to supply the solvent 22 from the solvent tank 20 to the three extraction units 100a, 100b, and 100c. In addition, small-diameter portions 40a, 40b, and 40c and second small-diameter portions 70a, 70b, 70c, and 70d are provided.

[0325] As in Example 3, 40 g of propionic acid and 160 g of ion-exchanged water were mixed to obtain 200 g of liquid raw material 12. The obtained liquid raw material 12 was stored in the raw material tank 10. Toluene was stored in the solvent tank 20 as the solvent 22. As in Experimental Example 2, the flow rate of the liquid raw material 12 to the extraction unit 100a was set to 5.0 ml / min.

[0326] The toluene (solvent 22) stored in the solvent tank 20 is fed to the mixer 110 by the pressure of the pressurized gas (nitrogen). At this time, the pressure in the tank is adjusted to 405 kPa by the pressure regulating unit 34 of the pressurized gas supply unit 30.

[0327] Small-diameter sections 40a, 40b, and 40c are positioned between the solvent tank 20 and the extraction unit 100. These sections are made of PEEK tubes. From the upstream side, the dimensions of small-diameter section 40a are 0.5 mm inner diameter and 100 mm long; small-diameter section 40b is 0.25 mm inner diameter and 150 mm long; and small-diameter section 40c is 0.25 mm inner diameter and 300 mm long. Furthermore, the inner diameters of the pipes upstream and downstream of small-diameter sections 40a, 40b, and 40c (first solvent pipe 42 and second solvent pipe 44) are 1.58 mm.

[0328] In addition, a valve (not shown) for finely adjusting the flow rate is provided between the small-diameter portion 40 and the extraction unit 100 .

[0329] Similar to Experimental Example 2, to stabilize the flow rate of solvent 22 flowing out of first outflow hole 142 into first recovery tank 50, second small-diameter portions 70a, 70b, and 70c were disposed between first outflow hole 142 and first recovery tank 50. Furthermore, a second small-diameter portion 70d was disposed between second outflow hole 144 and second recovery tank 60. The materials and dimensions of second small-diameter portions 70a, 70b, 70c, and 70d were the same as those of Experimental Example 2. Specifically, second small-diameter portions 70a, 70b, 70c, and 70d in Example 4 were PEEK tubes. From the upstream side, the dimensions of second small-diameter portion 70a were 0.125 mm inner diameter and 50 mm length, second small-diameter portion 70b were 0.25 mm inner diameter and 375 mm length, and second small-diameter portion 70c were 0.25 mm inner diameter and 100 mm length. In addition, similarly to Experimental Examples 1 and 2, a PEEK tube with an inner diameter of 0.5 mm and a length of 100 mm was installed as the second small-diameter portion 70d before the second recovery tank 60. Also, similarly to Experimental Example 2, the inner diameter of the pipes on the upstream and downstream sides of the second small-diameter portions 70a, 70b, 70c, and 70d was 1.58 mm.

[0330] As in Example 3 and Experimental Example 2 described above, a mixer-settler (manufactured by MAK Engineering, model number MS-L-IT-02-00-00) was used as the mixer 110 and liquid separator 140 of the extraction unit 100 of Example 4. The liquid raw material 12 and the washing solvent 22 were mixed using the mixer 110, which had a Y-shaped microchannel with a width of 0.8 mm, formed therein.

[0331] The mixer 110 and the clarifier, built into the mixer-settler, are connected by a PTFE pipe with an outer diameter of 1 / 16 inch, an inner diameter of 1 mm, and a length of 5 m, serving as the extraction section 130. The liquid raw material 12 and solvent 22 mixed in the mixer 110 flow through this pipe (extraction section 130), forming a slug flow within the pipe, thereby extracting propionic acid from water into toluene. The mixed liquid of the liquid raw material 12 and solvent 22 transported from the extraction section 130 to the clarifier (liquid separator 140) is separated in the clarifier into the solvent 22 (first recovered liquid 52) and the remaining liquid, namely the liquid raw material 12 (second recovered liquid 62). The first recovered liquid 52 is transported to the first recovery tank 50.

[0332] like Figure 3 As shown, in the apparatus of Example 4, three extraction units 100a, 100b, and 100c are arranged in series. The apparatus of Example 4 was operated under the above conditions, resulting in a flow rate of 3.8 ml / min for the solvent 22 flowing into the first extraction unit 100a, located farthest upstream. Furthermore, the pressure in the extraction section 130 at this time was 369 kPa, and the difference between the pressure in the extraction section 130 and the pressure in the solvent tank 20 (pressure in the solvent tank 20 minus the pressure in the extraction section 130) was 36 kPa. The recovery rate of propionic acid extracted into toluene was calculated based on concentration measurements using GC (gas chromatography). The calculated recovery rate of propionic acid in the first recovered liquid 52 was 38%. Therefore, the first recovered liquid 52 could be recovered at a flow rate of 3.8 ml / min in the first recovery tank 50 connected to the extraction unit 100a, resulting in a recovery rate of 38% for propionic acid.

[0333] Furthermore, the flow rate of solvent 22 flowing into the second extraction unit 100b downstream of the first extraction unit 100a can be set to 3.6 ml / min. Furthermore, the pressure in the extraction section 130 at this time is 132 kPa, and the difference between the pressure in the extraction section 130 and the pressure in the solvent tank 20 (pressure in the solvent tank 20 minus pressure in the extraction section 130) is 273 kPa. The recovery rate of propionic acid extracted into toluene was calculated based on the GC concentration measurement results. The calculation results showed that the recovery rate of propionic acid in the second recovered liquid 52 was 29%. Therefore, the first recovered liquid 52 can be recovered at a flow rate of 3.6 ml / min in the first recovery tank 50 connected to the extraction unit 100b, and propionic acid can be recovered at a recovery rate of 29%.

[0334] Furthermore, the flow rate of solvent 22 flowing into the third extraction unit 100c downstream of the second extraction unit 100b can be set to 3.8 ml / min. Furthermore, the pressure in the extraction section 130 at this time is 88 kPa, and the difference between the pressure in the extraction section 130 and the pressure in the solvent tank 20 (pressure in the solvent tank 20 minus pressure in the extraction section 130) is 317 kPa. The recovery rate of propionic acid extracted into toluene was calculated based on the GC concentration measurement results. The calculation results show that the recovery rate of propionic acid in the first recovered liquid 52 is 21%. Therefore, the first recovered liquid 52 can be recovered at a flow rate of 3.8 ml / min in the first recovery tank 50 connected to the extraction unit 100c, and propionic acid can be recovered at a recovery rate of 21%. Furthermore, using the three extraction units 100a, 100b, and 100c, propionic acid can be obtained at a recovery rate of 88%.

[0335] Table 4 shows the recovery rate of propionic acid extracted into toluene in Example 4. The recovery rate of propionic acid was calculated based on the concentration measurement results by GC (Gas Chromatograph). As shown in Table 4, according to Example 4, propionic acid, the target substance, can be efficiently extracted by extracting propionic acid from ion-exchanged water into toluene as solvent 22.

[0336] In the apparatus of Example 4, the solvent 22 stored in the solvent tank 20 is fed to the mixer 110 by the pressurized gas supply unit 30. Therefore, the apparatus of Example 4 is an apparatus capable of more easily extracting a target substance contained in a liquid raw material.

[0337]

Table 4

[0338]

[0339] (Example 5)

[0340] As described above, it is clear that the apparatus of Experimental Example 2 can be used to extract the specified contaminant (extraction target substance) dissolved in the liquid raw material. Therefore, the apparatus of Experimental Example 2 can be used as the cleaning apparatus of this embodiment. In Example 5, to confirm this, the same apparatus as in Example 4 was used to extract the contaminant as the extraction target substance (target substance) from the liquid raw material, thereby cleaning the liquid raw material.

[0341] In Example 5, the same apparatus as that used in Example 4 above was used (with Figure 3Using ultrapure water as solvent 22, metal ions (contaminants serving as the extraction target substance) were extracted and recovered from a liquid raw material 12 consisting of a 2-MeTHF solution of a phenolic resin, thereby removing the metal ions. Specifically, metal ions were continuously removed from the liquid raw material 12 three times using three extraction units 100a, 100b, and 100c connected in series. Example 5 is described in detail below.

[0342] In Example 5, similar to Example 4, Figure 3 That is, a pressurized gas supply unit 30 is used to supply the solvent 22 from the solvent tank 20 to the three extraction units 100a, 100b, and 100c. In addition, small-diameter portions 40a, 40b, and 40c and second small-diameter portions 70a, 70b, 70c, and 70d are provided.

[0343] A 2-MeTHF solution of a phenol resin (concentration: 20% by weight) was stored in a raw material tank 10 as a liquid raw material 12 . Ultrapure water was stored in a solvent tank 20 as a solvent 22 .

[0344] The liquid raw material 12 stored in the solvent tank 10 is fed to the mixer 110 by the pressure of the pressurized gas (nitrogen). At this time, the pressure in the tank is adjusted to 200 kPa by the pressure regulating unit 34 of the pressurized gas supply means 30.

[0345] A small-diameter portion 40 is disposed between the solvent tank 10 and the extraction unit 100. The small-diameter portion 40 is a PEEK tube having an inner diameter of 0.25 mm and a length of 55 mm. Furthermore, the inner diameters of the pipes upstream and downstream of the small-diameter portion 40 (the first solvent pipe 42 and the second solvent pipe 44) are 1.58 mm.

[0346] The ultrapure water (solvent 22) stored in the solvent tank 20 is fed to the mixer 110 by the pressure of nitrogen gas. At this time, the pressure in the tank is adjusted to 200 kPa by the pressure regulating unit 34 of the pressurized gas supply means 30.

[0347] Small-diameter sections 40a, 40b, and 40c are positioned between the solvent tank 20 and the extraction unit 100. Furthermore, in Example 5, the lengths of the small-diameter sections 40a, 40b, and 40c are different from those in Example 4. Specifically, the small-diameter sections 40a, 40b, and 40c are PEEK tubes. From the upstream side, the dimensions of the small-diameter section 40a are 0.5 mm inner diameter and 90 mm long; the dimensions of the small-diameter section 40b are 0.25 mm inner diameter and 110 mm long; and the dimensions of the small-diameter section 40c are 0.25 mm inner diameter and 200 mm long. Furthermore, the inner diameters of the pipes (first solvent pipe 42 and second solvent pipe 44) upstream and downstream of the small-diameter sections 40a, 40b, and 40c are 1.58 mm.

[0348] In addition, a valve (not shown) for finely adjusting the flow rate is provided between the small-diameter portion 40 and the extraction unit 100 .

[0349] Similar to Example 4, to stabilize the flow rate of solvent 22 flowing out of first outflow hole 142 into first recovery tank 50, second small-diameter portions 70a, 70b, and 70c are disposed between first outflow hole 142 and first recovery tank 50. Furthermore, a second small-diameter portion 70d is disposed between second outflow hole 144 and second recovery tank 60. Furthermore, in Example 5, the dimensions of second small-diameter portions 70a and 70b are different from those in Example 4. Specifically, second small-diameter portions 70a, 70b, 70c, and 70d are made of PEEK tubes. From the upstream side, the dimensions of second small-diameter portion 70a are 0.25 mm in inner diameter and 215 mm in length; second small-diameter portion 70b are 0.25 mm in inner diameter and 160 mm in length; and second small-diameter portion 70c are 0.25 mm in inner diameter and 100 mm in length. In addition, similarly to Example 4, a PEEK tube with an inner diameter of 0.5 mm and a length of 100 mm was installed as a second small-diameter portion 70d before the second recovery tank 60. Also, similarly to Example 4, the inner diameter of the pipes on the upstream and downstream sides of the second small-diameter portions 70a, 70b, 70c, and 70d was 1.58 mm.

[0350] As in Example 4 above, a mixer-settler (manufactured by MAK Engineering, model number MS-L-IT-02-00-00) was used as the mixer 110 and liquid separator 140 of the extraction unit 100 of the example. The liquid raw material 12 and the washing solvent 22 were mixed using the mixer 110, which had a Y-shaped microchannel with a width of 0.8 mm, formed therein.

[0351] The mixer 110 and the clarifier, built into the mixer-settler, are connected by a PTFE pipe with an outer diameter of 1 / 16 inch, an inner diameter of 1 mm, and a length of 10 m, serving as the extraction section 130. The liquid raw material 12 and solvent 22 mixed in the mixer 110 flow through this pipe (extraction section 130), forming a slug flow within the pipe, extracting the metal components in the phenolic resin into water. The mixed liquid of the liquid raw material 12 and solvent 22 transported from the extraction section 130 to the clarifier (liquid separation section 140) is separated in the clarifier into the solvent 22 (first recovered liquid 52) and the remaining liquid, namely the liquid raw material 12 (second recovered liquid 62). The first recovered liquid 52 is transported to the first recovery tank 50.

[0352] like Figure 3 As shown, in the apparatus of Example 5, three extraction units 100a, 100b, and 100c are arranged in series. The apparatus of Example 5 was operated under the above conditions, resulting in a flow rate of 3.2 ml / min of solvent 22 flowing into the first extraction unit 100a, located farthest upstream. Furthermore, the pressure in the extraction section 130 at this time was 188 kPa, and the difference between the pressure in the extraction section 130 and the pressure in the solvent tank 20 (pressure in the solvent tank 20 minus the pressure in the extraction section 130) was 12 kPa.

[0353] Furthermore, the flow rate of solvent 22 flowing into second extraction unit 100b downstream of first extraction unit 100a can be set to 1.2 ml / min. Furthermore, the pressure in extraction section 130 at this time is 132 kPa, and the difference between the pressure in extraction section 160 and the pressure in solvent tank 20 (pressure in solvent tank 20 minus pressure in extraction section 130) is 40 kPa.

[0354] Furthermore, the flow rate of the solvent 22 flowing into the third extraction unit 100c downstream of the second extraction unit 100b can be set to 2.2 ml / min, and the flow rate of the liquid raw material 12 can be set to 3.2 ml / min. At this time, the pressure of the extraction section 130 is 125 kPa, and the difference between the pressure of the extraction section 130 and the pressure of the solvent tank 20 (pressure of the solvent tank 20 minus the pressure of the extraction section 130) is 75 kPa.

[0355] Table 5 shows the measurement results (weight ratio) of the metal components of the 2-MeTHF solution of the phenolic resin before washing (liquid raw material 12) and the 2-MeTHF solution of the phenolic resin after washing (second recovered liquid) recovered in the second recovery tank 60. In addition, in Table 5, the measurement results (weight ratio) of the metal components of the 2-MeTHF solution of the phenolic resin flowing out from the second outflow hole 144 of the first extraction unit 100a are shown in the row "After extraction unit 100a". In addition, the measurement results (weight ratio) of the metal components of the 2-MeTHF solution of the phenolic resin flowing out from the second outflow hole 144 of the second extraction unit 100b are shown in the row "After extraction unit 100b". The solutions used for these measurements were taken out from the second outflow hole 144 of the extraction units 100a and 100b. In addition, the concentration of the metal components in the solution was measured using ICP-MS (inductively coupled plasma mass spectrometry). As can be seen from Table 5, according to Example 5, the metal components in the phenolic resin were efficiently extracted and removed into ultrapure water as the solvent 22, thereby enabling the phenolic resin to be washed.

[0356]

Table 5

[0357]

[0358] (Example 6)

[0359] Example 6 is the extraction and washing device of the sixth embodiment described above. Figure 9 The same apparatus as shown extracts the polyethylene glycol compound from its aqueous solution (liquid raw material), and washes and recovers the extracted polyethylene glycol compound.

[0360] like Figure 9 As shown, the apparatus used in Example 6 includes two solvent tanks 20a and 20b. Solvent tank 20a stores solvent 22a (dichloromethane) for extracting the polyethylene glycol compound. Separately, solvent tank 20b stores solvent 22b (saline solution) for washing the aqueous solution of the polyethylene glycol compound. Solvent tank 20a is connected to the first extraction unit 100a. In the first extraction unit 100a, the polyethylene glycol compound, the target substance, is extracted from the liquid raw material 12 using dichloromethane (solvent 22a). Solvent tank 20b is connected to the second and third extraction units 100b and 100c. In the second and third extraction units 100b and 100c, contaminants are extracted from the polyethylene glycol compound extracted with dichloromethane (solvent 22a) and washed. Example 6 is described in detail below.

[0361] In Example 6, application Figure 9The apparatus shown in the figure extracts the polyethylene glycol compound (useful substance) from the reaction solution of the polyethylene glycol compound and then extracts the water-soluble monomer (pollutant), thereby extracting and washing the polyethylene glycol compound. Figure 9 As shown, three sets of extraction units 100a, 100b, and 100c are connected in series and used. After one extraction is performed using the extraction unit 100a, two washings are performed continuously using the two extraction units 100b and 100c.

[0362] The reaction solution of the polyethylene glycol compound was stored as liquid raw material 12 in raw material tank 10. Dichloromethane for extracting the polyethylene glycol compound was stored as solvent 22a in solvent tank 20a. Furthermore, saline solution for extracting the water-soluble monomer was stored as solvent 22b in solvent tank 20b. The concentration of saline solution in solvent 22b was 10% by weight. The flow rate of liquid raw material 12 to extraction unit 100a was set at 10.0 ml / min.

[0363] Methylene chloride (solvent 22a) stored in solvent tank 20a and saline (solvent 22b) stored in solvent tank 20b are fed to mixer 110 using nitrogen pressure. At this time, the pressure in solvent tanks 20a and 20b is adjusted to 450 kPa by pressure regulator 34 of pressurized gas supply unit 30.

[0364] A small-diameter portion 40a is located between solvent tank 20a and extraction unit 100a. Small-diameter portions 40b and 40c are located between solvent tank 20b and extraction units 100b and 100c, respectively. Small-diameter portions 40a, 40b, and 40c are PEEK tubes. From the upstream side, the dimensions of small-diameter portion 40a are 0.5 mm inner diameter and 50 mm long; small-diameter portion 40b is 0.25 mm inner diameter and 100 mm long; and small-diameter portion 40c is 0.25 mm inner diameter and 150 mm long. Furthermore, the inner diameters of the pipes (first solvent pipe 42 and second solvent pipe 44) upstream and downstream of small-diameter portions 40a, 40b, and 40c are 1.58 mm.

[0365] In addition, a valve (not shown) for finely adjusting the flow rate is provided between the small-diameter portion 40 and the extraction unit 100 .

[0366] In order to stabilize the flow rate of liquid flowing from the first outflow hole 144 of the extraction unit 100a to the second recovery tank 60, a second small-diameter portion 70a is disposed between the second outflow hole 144 and the second recovery tank 60. Similarly, second small-diameter portions 70b and 70c are disposed between the first outflow hole 142 of the extraction units 100b and 100c and the first recovery tank 50. Furthermore, a second small-diameter portion 70d is disposed between the second outflow hole 144 of the extraction unit 100c and the second recovery tank 60. The second small-diameter portions 70a, 70b, 70c, and 70d are made of PEEK tubes. From the upstream side, the dimensions of the second small-diameter portion 70a are 0.25 mm inner diameter and 150 mm long; the dimensions of the second small-diameter portion 70b are 0.25 mm inner diameter and 75 mm long; and the dimensions of the second small-diameter portion 70c are 0.5 mm inner diameter and 100 mm long. A PEEK tube with an inner diameter of 0.5 mm and a length of 50 mm is installed upstream of the second recovery tank 60 as the second small-diameter portion 70d. Furthermore, the inner diameter of the pipes on the upstream and downstream sides of the second small-diameter portions 70a, 70b, 70c, and 70d is 1.58 mm.

[0367] As in Example 1 above, a mixer-settler (manufactured by MAK Engineering, Model MS-L-IT-02-00-00) was used as the mixer 110 and liquid separator 140 of the extraction unit 100 of Example 6. In extraction unit 100a, the liquid raw material 12 was mixed with the extraction solvent 22a using the mixer 110, which had a Y-shaped microchannel with a width of 0.8 mm, formed therein. Separately, in extraction units 100b and 100c, the mixer 110 was used to mix the liquid to be washed with the washing solvent 22b.

[0368] The mixer 110 and the clarifier, which are built into the mixer-settler, are connected by a PTFE pipe with an outer diameter of 1 / 8 inch, an inner diameter of 1.58 mm, and a length of 3 m, serving as the extraction section 130. By allowing the liquid raw material 12 and the solvent 22 mixed by the mixer 110 to flow through this pipe (extraction section 130), the liquid raw material 12 and the solvent 22 form a slug flow in the pipe, and the target substance is extracted into the solvent. In the extraction unit 100a, the mixed liquid of the liquid raw material 12 and the solvent 22, which is transported from the extraction section 130 to the clarifier (liquid separator 140), is separated in the clarifier into the solvent 22a containing the target substance and the remaining liquid, i.e., the liquid derived from the liquid raw material 12 (second recovered liquid 62). The second recovered liquid 62 is transported to the second recovery tank 60. Furthermore, in extraction units 100b and 100c, the solvent 22b containing the extracted contaminants (first recovered liquid 62) is separated by the clarifier (liquid separator 140) into the remaining liquid (liquid containing the polyethylene glycol compound). The liquid containing the polyethylene glycol compound flows out of the second outflow holes 144 of extraction units 100b and 100c and is ultimately recovered in the second recovery tank 60 connected to the second outflow hole 144 of extraction unit 100c.

[0369] like Figure 9 As shown, in the apparatus of Example 6, three extraction units 100a, 100b, and 100c are arranged in series. The apparatus of Example 6 was operated under the above conditions, resulting in a flow rate of 9.8 ml / min of solvent 22a, i.e., dichloromethane, flowing into the first extraction unit 100a, located farthest upstream. Furthermore, at this time, the pressure in the extraction section 130 of extraction unit 100a was 425 kPa, and the difference between the pressure in the extraction section 130 and the pressure in the solvent tank 20 (pressure in the solvent tank 20 minus the pressure in the extraction section 130) was 25 kPa.

[0370] Furthermore, the flow rate of the saline solution (solvent 22) flowing into the second extraction unit 100b downstream of the first extraction unit 100a can be set to 9.6 ml / min. Furthermore, at this time, the pressure in the extraction section 130 of the extraction unit 100b is 288 kPa, and the difference between the pressure in the extraction section 130 and the pressure in the solvent tank 20 (pressure in the solvent tank 20 minus the pressure in the extraction section 130) is 162 kPa.

[0371] Furthermore, the flow rate of the saline solution (solvent 22) flowing into the third extraction unit 100c downstream of the second extraction unit 100b can be set to 9.5 ml / min. Furthermore, the pressure in the extraction section 130 at this time is 176 kPa, and the difference between the pressure in the extraction section 130 of the extraction unit 100c and the pressure in the solvent tank 20 (pressure in the solvent tank 20 minus the pressure in the extraction section 130) is 274 kPa.

[0372] Table 6 shows the purity (weight %) calculated from the integrated ratio of 1H-NMR (proton nuclear magnetic resonance analysis) of the liquid raw material 12 before extraction and washing, and the polyethylene glycol compound and water-soluble monomers (contaminants 1 and 2) recovered in the second recovery tank 60 after extraction and washing. As shown in Table 6, according to Example 6, the polyethylene glycol compound can be extracted from the liquid raw material 12 using dichloromethane as the solvent 22a. In addition, according to Example 6, the water-soluble monomers (contaminants 1 and 2) in the polyethylene glycol compound can be efficiently extracted and removed by saline solution as the solvent 22b, thereby washing the polyethylene glycol compound.

[0373]

Table 6

[0374]

[0375] Description of Reference Numerals

[0376] 10. Raw material tank, 12. Liquid raw material, 14. Pump (liquid raw material supply component), 20. Solvent tank, 20a. First solvent tank, 20b. Second solvent tank, 22. Solvent, 22a. First solvent, 22b. Second solvent, 30. Pressurized gas supply component, 32. High-pressure gas supply unit (nitrogen tank), 34. Pressure regulating unit (pressure regulating valve), 36. Nitrogen supply piping, 40. 40a. 40b. 40c. Small-diameter portion, 41a. 41b. Connector, 42. First solvent piping, 44. Second solvent piping, 46. Thermostat, 50. First recovery tank, 52. First recovered liquid, 60. Second recovery tank, 62. Second recovered liquid, 70a. 70b. 70c. 70d. Second small-diameter portion, 100. 0a, 100b, 100c, extraction unit, 110, mixer, 112, first inflow hole, 114, second inflow hole, 130, extraction part, 140, liquid separation part, 142, first outflow hole, 144, second outflow hole, 150, valve, 210, reaction device, 212a, 212b, raw material tank for reaction device, 214, mixer for reaction device, 216, reactant tank, 218a, 218b, 220, piping, 222a, 222b, nitrogen gas supply piping for reaction device, 224a, 224b, pressure regulating valve for reaction device, 228a, 228b, small-diameter portion for reaction device, 402a, 402b, metal plate, 404, micro-flow path, 412, tube, 414, deformed portion of tube.

Claims

1. A device for extracting an extraction target substance dissolved in a liquid raw material, wherein: The device comprises: at least one raw material tank for storing the liquid raw material; a solvent tank for storing a solvent used to extract the extraction target substance from the liquid raw material; a pressurized gas supply component for supplying pressurized gas to the solvent tank; a small-diameter portion, one end of the small-diameter portion being connected to the solvent tank via a first solvent pipe, the other end of the small-diameter portion being connected to a second solvent pipe, the inner diameter of the small-diameter portion being smaller than the inner diameters of the first solvent pipe and the second solvent pipe; at least one extraction unit, comprising a mixer, an extraction section, and a liquid separation section, the mixer comprising a first inlet connected to the raw material tank and a second inlet connected to the small-diameter section via the second solvent pipe, the mixer being configured to mix the liquid flowing in from the first inlet with the liquid flowing in from the second inlet, the extraction section being configured to extract the extraction target substance from the liquid raw material into the solvent, the extraction section being connected to the mixer, the liquid separation section being connected to the extraction section, and comprising a first outflow hole for outflowing a first recovery liquid containing the solvent and the extraction target substance, and a second outflow hole for outflowing a second recovery liquid separated from the first recovery liquid, at least one raw material tank being connected to the first inflow hole of the mixer of at least one extraction unit; a first recovery tank connected to the first outflow hole and configured to recover the first recovery liquid; and The second recovery tank is connected to the second outflow hole and is used to recover the second recovery liquid.

2. The device according to claim 1, wherein The extraction target substance is a pollutant, and the device is a washing device for the liquid raw material.

3. The device according to claim 1, wherein The extraction target substance is a target substance, and the device is a device for extracting the target substance.

4. The device according to any one of claims 1 to 3, wherein The pressurized gas supply component includes a high-pressure gas supply unit and a pressure adjustment unit. The pressure inside the solvent tank and the first solvent pipe is 1.5 MPa or less.

5. The device according to any one of claims 1 to 4, wherein: The small diameter portion further includes a thermostat for adjusting the temperature of the small diameter portion.

6. The device according to any one of claims 1 to 5, wherein: The device comprises at least two extraction units connected in series, The raw material tank is connected to the first inflow port of the mixer of the extraction unit at the most upstream position. In a pair of the extraction units connected in series, the second outflow port of the extraction unit on the upstream side is connected to the first inflow port of the mixer of the extraction unit on the downstream side. The solvent tank is connected to the mixers of at least two extraction units via the small diameter portion. The small-diameter portion connected to the second inflow hole is a small-diameter portion having different pressure losses between the small-diameter portion on the upstream side and the small-diameter portion on the downstream side. A second small-diameter portion is provided in the flow path connected to the first recovery tank and the second recovery tank.

7. The device according to any one of claims 1 to 5, wherein: The device comprises at least two extraction units connected in parallel, The raw material tank is connected to the first inflow port of the mixer of at least two extraction units. The solvent tank is connected to the second inflow port of the mixer of at least two of the extraction units via the small-diameter portion.

8. The device according to any one of claims 1 to 5, wherein: The device comprises at least two extraction units connected in series, The raw material tank is connected to the first inflow port of the mixer of the extraction unit at the most upstream position. In at least one pair of the extraction units connected in series, the first outflow hole of the extraction unit on the upstream side is connected to the first inflow hole of the mixer of the extraction unit on the downstream side. The solvent tank is connected to the mixer of the extraction unit via the small diameter portion. The small-diameter portion connected to the second inflow hole is a small-diameter portion having different pressure losses between the small-diameter portion on the upstream side and the small-diameter portion on the downstream side. A second small-diameter portion is provided in the flow path connected to the first recovery tank and the second recovery tank.

9. The device according to claim 8, wherein In the extraction unit at the most upstream side and the extraction unit connected in series thereto, the first outflow hole of the extraction unit at the most upstream side is connected to the first inflow hole of the mixer of the extraction unit at the downstream side. In at least one pair of the extraction units connected in series, the second outflow port of the extraction unit on the upstream side is connected to the first inflow port of the mixer of the extraction unit on the downstream side.

10. The device according to claim 8 or 9, wherein The apparatus includes at least two solvent tanks, each of which stores a different solvent.

11. The device according to any one of claims 1 to 10, wherein: The solvent tank is a pressure-resistant tank.

12. The device according to any one of claims 1 to 11, wherein: The mixer has a micro flow path, and the width of the micro flow path is 0.01 μm to 20 mm.

13. The device according to any one of claims 1 to 12, wherein: The inner diameters of the first solvent pipe and the second solvent pipe are 0.1 mm to 20 mm.

14. The device according to any one of claims 1 to 13, wherein: The apparatus further includes liquid raw material supply means for supplying the liquid raw material to the mixer.

Citation Information

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