Production apparatus

Abstract

A production apparatus (1) comprises: a first liquid supply unit (10) that continuously supplies a first liquid (12) to a first flow path (14); a second liquid supply unit (20) that continuously supplies a second liquid (22) to a second flow path (24); an insoluble fluid supply unit (30) that supplies an insoluble fluid (32) having insoluble properties; an insoluble fluid introduction unit (40) that introduces the insoluble fluid (32) into the first liquid (12); and a mixing unit (50) that mixes the first liquid (12) and the second liquid (22). The insoluble fluid introduction unit (40) is disposed upstream from the mixing unit (50) in which a solid compound precipitates.

Description

manufacturing equipment

[0001] The present disclosure relates to an apparatus for producing a solid compound.

[0002] Methods for forming solid compounds include liquid-phase reaction methods and solid-phase reaction methods. Examples of known liquid-phase reaction methods include coprecipitation, sol-gel, injection pyrolysis, reduction, and reprecipitation. Conventionally, batch-type reactions have been used in liquid-phase reaction methods, but the formation of high-quality solid compounds has been difficult due to inconsistencies in mixing performance and heat transfer. A method using a microreactor utilizing a microspace has been proposed as a method for forming high-quality solid compounds. Reactions using a microreactor are believed to enable accurate flow control, temperature control, and rapid mixing of the reaction solution. Patent Document 1 discloses a method and apparatus for forming high-quality solid compounds using a microreactor. This method involves mixing two types of liquids so that one liquid surrounds the other, followed by solidification. This method and apparatus enable high-yield, simple, and inexpensive production of colorant particles with a small particle size and a narrow particle size distribution.

[0003] Japanese Patent Application Laid-Open No. 2008-7612

[0004] In the method and apparatus described in Patent Document 1, if a solid compound precipitates immediately after one liquid is mixed so as to surround the other liquid, the precipitated solid compound adheres to the wall surface inside the flow path, and the compound adheres, accumulates, and grows from the adhesion point, clogging the flow path and leading to variations in quality and a stoppage of production.

[0005] Therefore, an object of the present disclosure is to provide a production apparatus that can continuously produce a high-quality solid compound more stably, even in a reaction system in which a solid compound precipitates immediately after mixing.

[0006] A manufacturing apparatus according to one aspect of the present disclosure includes a first liquid supply unit that continuously supplies a first liquid to a first flow path, a second liquid supply unit that continuously supplies a second liquid to a second flow path, an insoluble fluid supply unit that supplies an insoluble fluid, an insoluble fluid introduction unit that introduces the insoluble fluid into at least one of the first liquid and the second liquid, and a mixing unit that mixes the first liquid flowing out of the first flow path and the second liquid flowing out of the second flow path, and the insoluble fluid introduction unit is positioned upstream of the mixing unit where a solid compound precipitates.

[0007] According to the production apparatus according to one aspect of the present disclosure, a high-quality solid compound can be produced continuously and more stably, even in a reaction system in which a solid compound precipitates immediately after mixing.

[0008] 1A and 1B are schematic diagrams showing an example of the configuration of a manufacturing apparatus according to an embodiment of the present disclosure; and FIG. 1C is a schematic diagram showing a mixing section of a manufacturing apparatus according to an embodiment of the present disclosure.

[0023] Figure 1A shows a mixing channel of a manufacturing apparatus according to an embodiment of the present disclosure, where (a) is a schematic diagram showing a slug flow formed in the mixing section, in which the distance between the insoluble fluid cells is greater than the channel diameter of the mixing channel, and (b) is a schematic diagram showing a slug flow formed in the mixing section, in which the distance between the insoluble fluid cells is equal to or less than the channel diameter of the mixing channel, and where (b) is a schematic diagram showing a mixing section when an insoluble fluid is introduced into a second liquid, and (b) is a schematic diagram showing a mixing section when an insoluble fluid is introduced into a first liquid.

[0024] Figure 1A is a schematic diagram showing a mixing section formed so that the angle between the first and second channels is greater than 90°, and (b) is a schematic diagram showing a mixing section formed so that the angle between the first and second channels is less than 90°.

[0009] The manufacturing apparatus according to the first aspect includes a first liquid supply unit that continuously supplies a first liquid to a first flow path, a second liquid supply unit that continuously supplies a second liquid to a second flow path, an insoluble fluid supply unit that supplies an insoluble fluid, an insoluble fluid introduction unit that introduces the insoluble fluid into at least one of the first liquid and the second liquid, and a mixing unit that mixes the first liquid flowing out of the first flow path and the second liquid flowing out of the second flow path, and the insoluble fluid introduction unit is positioned upstream of the mixing unit where a solid compound precipitates.

[0010] In the manufacturing apparatus according to the second aspect, in the first aspect described above, in the mixing section, the first liquid flowing out from the first flow path and the second liquid flowing out from the second flow path are mixed and flow into a mixing flow path, and in the mixing flow path, a slug flow is formed in which first cells containing the first liquid and the second liquid and second cells containing the immiscible fluid flow alternately, and the distance between the second cells in the slug flow may be less than the flow path diameter of the mixing flow path.

[0011] In the manufacturing apparatus according to a third aspect, in the first or second aspect, the second flow path may be formed so as to surround an outlet of the first flow path.

[0012] In a manufacturing apparatus according to a fourth aspect, in the third aspect, the insoluble fluid introduction section may introduce the insoluble fluid into the first liquid.

[0013] In the manufacturing apparatus according to a fifth aspect, in the first to fourth aspects, an angle formed between the first flow path and the second flow path may be 90° or less.

[0014] Hereinafter, a manufacturing apparatus according to an embodiment will be described with reference to the accompanying drawings.

[0015] The embodiments described below are all comprehensive or specific examples. The numerical values, shapes, materials, components, component placement and connection configurations, steps, and step order shown in the following embodiments are merely examples and are not intended to limit the present disclosure. Furthermore, among the components in the following embodiments, components that are not recited in independent claims are described as optional components. Furthermore, each drawing is a schematic diagram and is not necessarily an exact illustration. Furthermore, substantially identical components in the drawings are designated by the same reference numerals.

[0016] (Embodiment) Fig. 1 is a schematic diagram showing an example of the configuration of a manufacturing apparatus 1 according to an embodiment of the present disclosure. Fig. 2 is a schematic diagram showing a mixing section 50 of the manufacturing apparatus 1 according to an embodiment of the present disclosure. Fig. 2(a) shows a cross section, and Fig. 2(b) shows a cross section taken along line IIb-IIb in Fig. 2(a).

[0017] As shown in FIG. 1 , the manufacturing apparatus 1 mixes multiple fluids in a mixing channel to stably produce a higher-quality solid compound 90. Specifically, the manufacturing apparatus 1 includes a first liquid supply unit 10 that continuously supplies a first liquid 12 to a first flow channel 14, a second liquid supply unit 20 that continuously supplies a second liquid 22 to a second flow channel 24, an insoluble fluid supply unit 30 that supplies an insoluble fluid 32, an insoluble fluid introduction unit 40 that introduces the insoluble fluid 32 into the first liquid 12, and a mixing unit 50 that mixes the first liquid 12 and the second liquid 22. The manufacturing apparatus 1 also includes a recovery unit 60. As will be described in detail below, the mixing unit 50 is formed so that the second flow channel 24 surrounds the outlet 14a of the first flow channel 14. The insoluble fluid introduction unit 40 is located upstream of the mixing unit 50 where the solid compound 90 precipitates.

[0018] In this embodiment, an example has been shown in which solid compound 90 is produced by bringing two liquids to be mixed, namely, first liquid 12 and second liquid 22, into contact with and mixing immiscible fluid 32 in mixing unit 50, but when a compound is produced using three or more liquids to be mixed, a configuration similar to first liquid supply unit 10 may be provided in parallel, or a configuration similar to second liquid supply unit 20 may be provided in parallel. Furthermore, first liquid supply unit 10 and second liquid supply unit 20 may use a thermostatic bath or the like depending on the synthesis process of the target compound to change the temperatures of first liquid 12 and second liquid 22 supplied to mixing unit 50, but this is omitted in this embodiment and is not shown.

[0019] The flow path diameters of the first flow path 14 and the second flow path 24, which are the subject of the present disclosure, may be set within a range that allows the device to function as a micromixer or microreactor, for example, 0.1 to 1.0 mm. Flow paths fabricated by grooved flat plates and bonding them together, or by laminating and fixing them together, metal tubes, or resin tubes may be used. Examples of materials that can be used for the flat plates include metal materials such as stainless steel alloys, copper, titanium, and Hastelloy; glass materials such as quartz glass and borosilicate glass; and resin materials such as vinyl chloride, PP, PFA, PTFE, ETFE, PEEK, and PPS. Examples of materials that can be used for the metal tubes include stainless steel alloys and copper. Examples of materials that can be used for the resin tubes include PP, PFA, PTFE, ETFE, PEEK, and PPS.

[0020] The main components of the first liquid 12 and the second liquid 22 that are the subject of the present disclosure may be either water-soluble or water-insoluble as long as they are mutually soluble. For example, both liquids (first liquid 12 and second liquid 22) may be water or an aqueous solution, or both liquids (first liquid 12 and second liquid 22) may be organic solvents or oil-based. The mixing ratio and concentration of the first liquid 12 and the second liquid 22 can also be freely set. For example, when used in a crystallization reaction of particles such as iron hydroxide, lithium aluminum fluoride, titanium oxide, or 2-methylimidazole zinc salt (ZIF-8), the ionic solution that constitutes the particles can be used as the first liquid 12 and the second liquid 22.

[0021] The main component of the immiscible fluid 32 of the present disclosure may be either a liquid or a gas, as long as it is insoluble in both the first liquid 12 and the second liquid 22. For example, when the first liquid 12 and the second liquid 22 are water or an aqueous solution, a water-insoluble organic solvent or gas can be used, such as benzene, hexane, Ar gas, or N ２ Gases can be used, for example, water, Ar gas, or N when the first liquid 12 and the second liquid 22 are oil-based. ２ When a gas is used as the insoluble fluid 32, it is desirable that the gas does not affect the reaction product. ２ The use of an inert gas such as a gas is preferred.

[0022] The first liquid supply unit 10 is connected to the first flow path 14 and continuously supplies the first liquid 12 to the first flow path 14. The second liquid supply unit 20 is connected to the second flow path 24 and continuously supplies the second liquid 22 to the second flow path 24. The insoluble fluid supply unit 30 continuously or intermittently supplies the insoluble fluid 32. The insoluble fluid 32 supplied by the insoluble fluid supply unit 30 is supplied to the first liquid 12 flowing through the first flow path 14 at the insoluble fluid introduction unit 40. For example, the first liquid supply unit 10, the second liquid supply unit 20, and the insoluble fluid supply unit 30 may each be configured by a pump or the like.

[0023] The insoluble fluid introduction section 40, which is a target of the present disclosure, introduces the insoluble fluid 32 into the first liquid 12 and is disposed upstream of the mixing section 50 in which the solid compound 90 precipitates. For example, the insoluble fluid introduction section 40 has a configuration in which the first flow path 14 and a flow path to which the insoluble fluid 32 is supplied are connected, and the insoluble fluid supply section 30 supplies the insoluble fluid 32 to the flow path, thereby intermittently introducing the insoluble fluid 32 into the first liquid 12 flowing through the first flow path 14. The flow path diameter of the flow path in the insoluble fluid introduction section 40 may be set within a range that allows the insoluble fluid to function as a micromixer or a microreactor, and may be, for example, 0.1 to 1.0 mm. A flow path made by forming grooves in flat plates and bonding them together, or by stacking and fixing them together, a metal tube, a resin tube, or the like may be used. The flat plate may be made of a metal such as stainless steel alloy, copper, titanium, or Hastelloy; a glass such as quartz glass or borosilicate glass; or a resin such as vinyl chloride, PP, PFA, PTFE, ETFE, PEEK, or PPS. The metal tube may be made of a stainless steel alloy or copper. The resin tube may be made of PP, PFA, PTFE, ETFE, PEEK, or PPS.

[0024] In this embodiment, the insoluble fluid introduction section 40 has a configuration in which the flow path to which the insoluble fluid 32 is supplied is connected to the first flow path 14, but it may also have a configuration in which the flow path to which the insoluble fluid 32 is supplied is connected to the second flow path 24. As will be described later, in consideration of the uniformity and stability of the slug flow formed in the mixing section 50, it is desirable that the insoluble fluid introduction section 40 has a configuration in which the flow path to which the insoluble fluid 32 is supplied is connected to the first flow path 14.

[0025] The mixing section 50 of the present disclosure mixes the first liquid 12 and the second liquid 22. As shown in FIG. 2 , in this embodiment, the mixing section 50 has a configuration in which the first flow path 14, the second flow path 24, and the mixing flow path 52 are connected, and is configured so that the first liquid 12 flowing out from the first flow path 14 and the second liquid 22 flowing out from the second flow path 24 are mixed and flow into the mixing flow path 52. In the mixing section 50, the second flow path 24 is formed to surround the outlet 14a of the first flow path 14. The outlet 14a of the first flow path 14 and the outlet 24a of the second flow path 24 are connected. The angle between the first flow path 14 and the second flow path 24 is 90° or less. In other words, the first flow path 14 and the second flow path 24 converge at an angle of 90° or less, and the angle between the outflow direction of the first liquid 12 from the first flow path 14 and the outflow direction of the second liquid 22 from the second flow path 24 is 90° or less. The mixing channel 52 is located on an extension of the first channel 14, is aligned with the first channel 14 in the outflow direction of the first liquid 12 from the first channel 14, and extends axially in the outflow direction. In the mixing channel 52, the first liquid 12 and the second liquid 22 are mixed, forming a slug flow consisting of immiscible fluid cells 70 and target-mixing cells 80 (see FIG. 3 ). The target-mixing cells 80 and the target-mixing cells 70 flow alternately. The target-mixing cells 80 are an example of a first cell containing the mixed first liquid 12 and second liquid 22. The immiscible fluid cells 70 are an example of a second cell containing the immiscible fluid 32. The target-mixing cells 80 are formed by the first liquid 12 and the second liquid 22, and the immiscible fluid cells 70 are formed by the immiscible fluid 32. For example, the slug flow is formed so that the distance between the immiscible fluid cells 70 is equal to or less than the channel diameter of the mixing channel 52. For example, such a slug flow can be formed by adjusting the flow rate per unit time at which the insoluble fluid supply unit 30 supplies the insoluble fluid 32. In this embodiment, solid compounds 90 precipitate in the mixing target cells 80 of the slug flow formed in the mixing unit 50.The flow path diameter of the mixing flow path 52 of the mixing section 50 may be set within a range in which the mixing section 50 functions as a micromixer or a microreactor, and may be, for example, 0.1 to 1.0 mm. The material may be a metal material such as stainless steel alloy, copper, titanium, or Hastelloy, a glass material such as quartz glass or borosilicate glass, or a resin material such as vinyl chloride, PP, PFA, PTFE, ETFE, PEEK, or PPS.

[0026] As shown in FIG. 1 , the recovery unit 60 is connected to the end of the mixing channel 52 and recovers the mixing target cell 80 and the solid compound 90. In the recovery unit 60, it may be necessary to remove the remaining raw materials and the insoluble fluid 32 contained in the mixing target cell 80, but this is omitted in the present embodiment and is therefore not shown. Methods such as filtration or centrifugation can be used to recover the solid compound 90 from the mixing target cell 80. Methods such as gravity separation can also be used to separate the insoluble fluid cell 70 and the mixing target cell 80.

[0027] 3A and 3B show the mixing flow channel 52 of the manufacturing apparatus 1 according to the embodiment of the present disclosure, and FIG. 3A shows the distance L between the insoluble fluid cells 70 in the slug flow formed in the mixing section 50 and the cells to be mixed 80. ｓｌｕｇ is the flow path diameter L of the mixing flow path 52 ｔｕｂｅ 1(b) is a schematic diagram showing the case where the distance L between the immiscible fluid cells 70 is larger than the distance L between the immiscible fluid cells 70 in the slug flow formed in the mixing section 50 and the cells to be mixed 80. ｓｌｕｇ is the flow path diameter L of the mixing flow path 52 ｔｕｂｅ 1 is a schematic diagram of the following case.

[0028] 3A and 3B, in the mixing section 50, a slug flow consisting of the immiscible fluid cells 70 and the target mixing cells 80 flows downstream, and the target mixing cells 80 contain solid compounds 90 formed by the reaction of the first liquid 12 and the second liquid 22. The solid compounds 90 contained in the target mixing cells 80 are separated by a distance L between the immiscible fluid cells 70. ｓｌｕｇ Therefore, as shown in FIG. 3A, the distance L between the immiscible fluid cells 70 is ｓｌｕｇis the flow path diameter L of the mixing flow path 52 ｔｕｂｅ If the distance L between the immiscible fluid cells 70 is larger than the distance L 1 , the grown solid compound 90 is likely to clog the mixing channel 52 or destabilize the liquid supply, making it impossible to stably and continuously produce a high-quality solid compound 90. On the other hand, as shown in FIG. ｓｌｕｇ is the flow path diameter L of the mixing flow path 52 ｔｕｂｅ When the distance L is equal to or less than 1 / 2 mm, clogging of the mixing flow channel 52 by the grown solid compound 90 and destabilization of the liquid supply are unlikely to occur, and the solid compound 90 of higher quality can be produced more stably and continuously. ｓｌｕｇ is the distance between the upstream surface of the downstream immiscible fluid cell 70 and the downstream surface of the upstream immiscible fluid cell 70. Here, the longest distance in a predetermined direction inclined with respect to the direction of the slug flow is defined as the distance L ｓｌｕｇ The distance between the insoluble fluid cells 70 may be the distance between the upstream surface of the downstream insoluble fluid cell 70 and the downstream surface of the upstream insoluble fluid cell 70, which may be the longest distance in the direction of the slug flow. As described above, for example, by adjusting the flow rate per unit time at which the insoluble fluid supply unit 30 supplies the insoluble fluid 32, the distance L between the insoluble fluid cells 70 can be adjusted as shown in FIG. 3(b). ｓｌｕｇ is the flow path diameter L of the mixing flow path 52 ｔｕｂｅ The slug flow can be formed so that the flow rate is smaller than

[0029] Distance L between the immiscible fluid cells 70 ｓｌｕｇ For example, a method of calculating the distance L between the immiscible fluid cells 70 can be considered, by taking a video or photograph of the mixing channel 52 and measuring the distance between the immiscible fluid cells 70 as shown in (a) and (b) of Figure 3. Alternatively, the difference in the physical properties of the immiscible fluid cells 70 and the mixing target cells 80 can be utilized to calculate the distance L between the immiscible fluid cells 70 from the change over time. ｓｌｕｇ For example, the light transmittance of the immiscible fluid cell 70 can be calculated as T １ , the light transmittance of the mixing target cell 80 is T ２ When T is set, the optical transmittance of the slug flow observed at a certain point in the mixing channel 52 changes periodically. ２The time during which the flow is continuously observed is t [s], the flow speed is f [mm / s], and the flow path diameter is L ｔｕｂｅ [mm], the distance L between the insoluble fluid cells 70 ｓｌｕｇ　 [mm] can be calculated as follows:

[0030] The above is an example, and may be changed according to the device configuration, the materials used for the piping, and the liquid to be delivered.

[0031] Figure 4(a) is a schematic diagram of the mixing section 50 when an immiscible fluid 32 is introduced into the second liquid 22, and Figure 4(b) is a schematic diagram of the mixing section 50 when an immiscible fluid 32 is introduced into the first liquid 12.

[0032] As shown in (a) and (b) of Figures 4, in an immiscible fluid inlet section 40 or the like, an immiscible fluid 32 is introduced into at least one of the first liquid 12 and the second liquid 22, and in a mixing section 50, a slug flow consisting of an immiscible fluid cell 70 and a mixing target cell 80 is formed from the immiscible fluid 32, the first liquid 12, and the second liquid 22.

[0033] In this embodiment, the second flow path 24 is formed in the mixing section 50 so as to surround the outlet 14a of the first flow path 14. Therefore, when the immiscible fluid 32 is introduced into the second liquid 22, as shown in Fig. 4A, the slug flow becomes slightly unstable due to a change in the flow direction of the immiscible fluid 32 and shear forces caused by the flow of the first liquid 12. However, this does not pose a problem depending on the solid compound being produced. On the other hand, when the immiscible fluid 32 is introduced into the first liquid 12, as shown in Fig. 4B, the flow direction of the immiscible fluid 32 does not change in the mixing section 50. Furthermore, the second liquid 22 joins the immiscible fluid 32 flowing through the first flow path 14 so as to surround it. Therefore, a slug flow consisting of the immiscible fluid cells 70 and the mixing target cells 80 is stably formed, enabling the continuous production of a high-quality solid compound 90 with greater stability.

[0034] FIG. 5(a) is a schematic diagram of a case where the mixing section 150 is formed so that the angle θ between the first flow path 14 and the second flow path 124 is greater than 90°, and FIG. 5(b) is a schematic diagram of a case where the mixing section 50 is formed so that the angle θ between the first flow path 14 and the second flow path 24 is 90° or less.

[0035] As shown in Figures 5(a) and (b), in the immiscible fluid inlet section 40, the immiscible fluid 32 is introduced into the first liquid 12, and in the mixing sections 50, 150, a slug flow consisting of an immiscible fluid cell 70 and a mixing target cell 80 is formed from the immiscible fluid 32, the first liquid 12, and the second liquid 22.

[0036] In this embodiment, the mixing section 150 is formed with the second flow path 124 surrounding the outlet 14a of the first flow path 14. Therefore, if the mixing section 150 is formed so that the angle θ between the first flow path 14 and the second flow path 124 is greater than 90°, as shown in FIG. 5A , shear forces due to the flow of the second liquid 22 cause the immiscible fluid 32 to split, resulting in size variations. This makes the slug flow consisting of the immiscible fluid cells 70 and the target cells 80 in the mixing section 150 somewhat unstable, but this does not pose a problem depending on the solid compound being produced. On the other hand, if the mixing section 50 is formed so that the angle θ between the first flow path 14 and the second flow path 24 is less than 90°, the immiscible fluid cells 70 are not split due to shear forces due to the flow of the second liquid 12. Therefore, the slug flow consisting of the immiscible fluid cells 70 and the target cells 80 is stably formed, enabling more stable and continuous production of a high-quality solid compound 90.

[0037] According to the manufacturing apparatus 1 of this embodiment as described above, even in a reaction system in which the solid compound 90 precipitates immediately after mixing, it is possible to continuously manufacture a high-quality solid compound 90 more stably.

[0038] The manufacturing apparatus 1 according to this embodiment comprises a first liquid supply section 10 that continuously supplies a first liquid 12 to a first flow path 14, a second liquid supply section 20 that continuously supplies a second liquid 22 to a second flow path 24, an insoluble fluid supply section 30 that supplies an insoluble fluid 32, an insoluble fluid introduction section 40 that introduces the insoluble fluid 32 into the first liquid 12, and a mixing section 50 that mixes the first liquid 12 flowing out from the first flow path 14 and the second liquid 22 flowing out from the second flow path 24, and the insoluble fluid introduction section 40 is arranged upstream of the mixing section 50 in which the solid compound 90 precipitates.

[0039] According to this, the insoluble fluid 32 is introduced into the first liquid 12 before the first liquid 12 and the second liquid 22 are mixed, so that even if the solid compound 90 precipitates immediately after the first liquid 12 and the second liquid 22 are mixed, the solid compound 90 can be swept downstream by the insoluble fluid 32. Therefore, the solid compound 90 can be prevented from adhering to the inside of the flow channel, and a high-quality solid compound 90 can be produced continuously and more stably.

[0040] Furthermore, in the manufacturing apparatus 1 according to this embodiment, in the mixing section 50, the first liquid 12 flowing out from the first flow path 14 and the second liquid 22 flowing out from the second flow path 24 are mixed and flow into the mixing flow path 52, and in the mixing flow path 52, a slug flow is formed in which mixing target cells 80 containing the first liquid 12 and the second liquid 22 and insoluble fluid cells 70 containing the insoluble fluid 32 flow alternately, and the distance between the insoluble fluid cells 70 in the slug flow is less than the flow path diameter of the mixing flow path 52.

[0041] This makes it easier to make the size of the solid compound 90 precipitated in the mixing cell 80 equal to or smaller than the flow path diameter of the mixing flow path 52. Therefore, it is possible to prevent the solid compound 90 from adhering to the inside of the mixing flow path 52, and therefore it is possible to continuously produce a high-quality solid compound 90 in a more stable manner.

[0042] In addition, in the manufacturing apparatus 1 according to this embodiment, the second flow path 24 is formed so as to surround the outlet 14 a of the first flow path 14 .

[0043] According to this, the second liquid 22 can be mixed from the periphery of the first liquid 12, and therefore the solid compound 90 of high quality can be produced continuously and more stably.

[0044] In the manufacturing apparatus 1 according to this embodiment, the insoluble fluid introduction section 40 introduces the insoluble fluid 32 into the first liquid 12 .

[0045] This makes it possible to prevent the insoluble fluid 32 from splitting when the second liquid 22 is mixed in from around the first liquid 12, and therefore the solid compound 90 can be more reliably pushed downstream by the insoluble fluid 32. Therefore, it is possible to further prevent the solid compound 90 from adhering to the inside of the flow channel, and therefore it is possible to continuously produce a high-quality solid compound 90 more stably.

[0046] In addition, in the manufacturing apparatus 1 according to this embodiment, the angle formed between the first flow path 14 and the second flow path 24 is 90° or less.

[0047] This makes it possible to prevent the immiscible fluid 32 from splitting when the first liquid 12 and the second liquid 22 are mixed, and therefore the solid compound 90 can be more reliably pushed downstream by the immiscible fluid 32. Therefore, it is possible to further prevent the solid compound 90 from adhering to the inside of the flow channel, and therefore it is possible to continuously produce the solid compound 90 with even more stability and high quality.

[0048] Hereinafter, the results of producing lithium aluminum fluoride microparticles using the production apparatus 1 shown in FIG. 1 will be described in detail, but the present disclosure is not limited to these examples.

[0049] 1 , SUS tubes with an inner diameter of 1 mm and an outer diameter of 1.59 mm were used for the first flow path 14 and the second flow path 24. The mixing section 50 was designed so that the cylindrical second flow path 24 with an inner diameter of 2 mm and an outer diameter of 3 mm was formed to surround the outlet of the cylindrical first flow path 14 with an inner diameter of 1 mm and an outer diameter of 1.59 mm, and the first flow path 14 and the second flow path 24 merged at an angle of 45°.

[0050] An aqueous solution of ammonium fluoride dissolved in pure water to a concentration of 750 mM was prepared as the first liquid 12, an aqueous solution of lithium nitrate and aluminum nitrate dissolved in pure water and mixed to give lithium nitrate and aluminum nitrate concentrations of 375 mM and 125 mM, respectively, was prepared as the second liquid 22, and Ar gas was prepared as the insoluble fluid 32.

[0051] In the first liquid supply unit 10, a plunger pump (UI-22) manufactured by Flom Corporation was used to deliver the first liquid 12 to the first flow path 14 at a flow rate of 10 mL / min. In the second liquid supply unit 20, a plunger pump (UI-22) manufactured by Flom Corporation was used to deliver the second liquid 22 to the second flow path 24 at a flow rate of 10 mL / min. In the insoluble fluid supply unit 30, a syringe pump (YSP-101) manufactured by YMC Corporation was used to deliver the insoluble fluid 32 at a flow rate of 20 mL / min. In the insoluble fluid introduction unit 40, a T-shaped SUS micromixer with an inner diameter of 1 mm was used, and the insoluble fluid 32 was introduced into the first liquid 12.

[0052] The production was carried out for 1 hour, and the lithium aluminum fluoride microparticle-containing solution produced was collected in a PFA collection section 60 by connecting a PFA tube having an inner diameter of 2.18 mm, an outer diameter of 3.18 mm, and a length of 2 m downstream of the mixing section 50.

[0053] Example 2 Example 2 is the same as Example 1 except that the insoluble fluid supply unit 30 uses a syringe pump (YSP-101) manufactured by YMC Corporation to supply the insoluble fluid 32 at a flow rate of 5 mL / min.

[0054] Example 3 Example 3 is the same as Example 1 except that the insoluble fluid inlet part 40 is replaced with a SUS T-shaped micromixer with an inner diameter of 1 mm, and the insoluble fluid 32 is introduced into the second liquid 22 instead of the first liquid 12.

[0055] Example 4 Example 4 is similar to Example 1 except that mixing section 150, which replaces mixing section 50, is designed such that cylindrical second flow path 124 having an inner diameter of 2 mm and an outer diameter of 3 mm is formed to surround the outlet of cylindrical first flow path 14 having an inner diameter of 1 mm and an outer diameter of 1.59 mm, and first flow path 14 and second flow path 124 join at an angle of 135°.

[0056] Comparative Example 1 Comparative Example 1 is the same as Example 1 except that the insoluble fluid supply unit 30, the insoluble fluid 32, and the insoluble fluid introduction unit 40 are not provided in the manufacturing apparatus 1 of FIG.

[0057] (Evaluation of Continuous Production Stability and Evaluation of Product Quality in Examples and Comparative Examples) In the microparticle production processes of Examples 1-4 and Comparative Example 1, continuous production stability was evaluated by investigating the pressure profile within the flow path. A pressure gauge (FC-PSU-1000: manufactured by DFC) was installed in the second flow path 24, 124 to measure the pressure profile within the flow path. In order to determine the effect on continuous production stability, if the maximum pressure increase value from the start of synthesis was 0.2 MPa or more, it was determined that the effect on continuous production stability was low, if it was 0.1 MPa or more but less than 0.2 MPa, it was determined that there was an effect on continuous production stability, and if it was less than 0.1 MPa, it was determined that there was a better effect on continuous production stability.

[0058] In Table 1, if the maximum pressure rise value is 0.2 MPa or more, the continuous production stability is indicated as "low," if it is 0.1 MPa or more but less than 0.2 MPa, the continuous production stability is indicated as "medium," and if it is less than 0.1 MPa, the continuous production stability is indicated as "high."

[0059] In addition, to evaluate the quality of the product, the particle size variation of the produced lithium aluminum fluoride microparticles was measured using a particle size measurement system (ELSZ-2000) manufactured by Otsuka Electronics Co., Ltd. Here, the particle size variation was evaluated by the cv value, that is, the value obtained by dividing the standard deviation of the particle size distribution by the average value. In this synthesis reaction of lithium aluminum fluoride microparticles, the smaller the cv value of the product, the higher the quality, and when the cv value is 0.1 or more, it is judged to be low quality, when it is 0.05 or more but less than 0.1, it is judged to be high quality, and when it is less than 0.05, it is judged to be even higher quality.

[0060] In Table 1, if the cv value is 0.1 or more, the quality is indicated as "low," if it is 0.05 or more and less than 0.1, the quality is indicated as "high," and if it is less than 0.05, the quality is indicated as "very high."

[0061] As shown in the results in Table 1, Example 1 was evaluated as being extremely excellent in both continuous production stability and quality. Although Examples 2-4 were inferior to Example 1, they were superior in both continuous production stability and quality compared to Comparative Example 1. On the other hand, in Comparative Example 1, adhesion of the product was observed in the mixing section 50 where the first liquid 12 and the second liquid 22 come into contact, and this adhesion caused the flow path to become blocked, and the upper limit of the pump's liquid delivery pressure value was reached, so production was interrupted after 0.1 h.

[0062] As described above, the accompanying drawings and detailed description have been provided to explain exemplary embodiments of the technology disclosed herein. Therefore, the components described in the accompanying drawings and detailed description may include not only components essential for solving the problem, but also components that are not essential for solving the problem in order to illustrate the technology. Therefore, the fact that these non-essential components are described in the accompanying drawings or detailed description should not be interpreted as immediately identifying these non-essential components as essential.

[0063] Although the present disclosure has been fully described in connection with the preferred embodiments with reference to the accompanying drawings, various modifications are possible within the scope of the claims, and such modifications and embodiments obtained by appropriately combining the technical means disclosed in the different embodiments are also included in the technical scope of the present disclosure.

[0064] Other Embodiments, etc. In the above-described embodiment, the case where the insoluble fluid introduction part 40 introduces the insoluble fluid 32 into the first liquid 12 has been described, but the present invention is not limited to this. For example, the insoluble fluid introduction part may introduce the insoluble fluid into the second liquid, or may introduce the insoluble fluid into both the first liquid and the second liquid.

[0065] Furthermore, in the above-described embodiment, the mixing unit 50 mixes the first liquid 12 and the second liquid 22, but this is not limiting. The mixing unit may mix three or more liquids. For example, when mixing three liquids, namely, the first liquid, the second liquid, and the third liquid, a third liquid supply unit that continuously supplies the third liquid to the third flow path may be provided, and the first liquid flowing out of the first flow path, the second liquid flowing out of the second flow path, and the third liquid flowing out of the third flow path may be mixed in the mixing unit.

[0066] In the above-described embodiment, the second flow path 24 is formed to surround the outlet 14a of the first flow path 14, but this is not limiting. The second flow path does not have to be formed to surround the outlet of the first flow path. For example, the second flow path may be formed in the same shape as the first flow path, and the first and second flow paths may be merged. Alternatively, the second flow path may be branched into two flow paths, one of which may merge with the outlet of the first flow path from one side, and the other of which may merge with the outlet of the first flow path from the other side.

[0067] (Additional Note) The above description of the embodiments and the like discloses the following techniques.

[0068] (Technology 1) A manufacturing apparatus comprising: a first liquid supply unit that continuously supplies a first liquid to a first flow path; a second liquid supply unit that continuously supplies a second liquid to a second flow path; an insoluble fluid supply unit that supplies an insoluble fluid; an insoluble fluid introduction unit that introduces the insoluble fluid into at least one of the first liquid and the second liquid; and a mixing unit that mixes the first liquid flowing out of the first flow path and the second liquid flowing out of the second flow path, wherein the insoluble fluid introduction unit is positioned upstream of the mixing unit where a solid compound precipitates.

[0069] (Technology 2) The manufacturing apparatus according to Technology 1, wherein in the mixing section, the first liquid flowing out from the first flow path and the second liquid flowing out from the second flow path are mixed and flow into a mixing flow path, and in the mixing flow path, a slug flow is formed in which first cells containing the first liquid and the second liquid and second cells containing the immiscible fluid flow alternately, and a distance between the second cells in the slug flow is equal to or less than a flow path diameter of the mixing flow path.

[0070] (Technology 3) The manufacturing apparatus according to Technology 1 or 2, wherein the second flow path is formed so as to surround an outlet of the first flow path.

[0071] (Technology 4) The manufacturing apparatus according to Technology 3, wherein the insoluble fluid introduction section introduces the insoluble fluid into the first liquid.

[0072] (Technology 5) The manufacturing apparatus according to any one of Technologies 1 to 4, wherein an angle formed between the first flow path and the second flow path is 90° or less.

[0073] According to the production apparatus of the present disclosure, even in a reaction system in which a solid compound precipitates immediately after mixing, it is possible to continuously produce a solid compound of higher quality more stably, and the production apparatus can be applied to, for example, production utilizing a crystallization reaction of an inorganic ceramic or a metal-organic framework, or a reprecipitation reaction of a polymer compound.

[0074] REFERENCE SIGNS LIST 1 Manufacturing apparatus 10 First liquid supply section 12 First liquid 14 First flow path 14a, 24a Outlet 20 Second liquid supply section 22 Second liquid 24, 124 Second flow path 30 Insoluble fluid supply section 32 Insoluble fluid 40 Insoluble fluid introduction section 50, 150 Mixing section 52 Mixing flow path 60 Recovery section 70 Insoluble fluid cell 80 Mixing target cell 90 Solid compound

Claims

1. A manufacturing apparatus comprising: a first liquid supply section that continuously supplies a first liquid to a first flow path; a second liquid supply section that continuously supplies a second liquid to a second flow path; an insoluble fluid supply section that supplies an insoluble fluid; an insoluble fluid introduction section that introduces the insoluble fluid into at least one of the first liquid and the second liquid; and a mixing section that mixes the first liquid flowing out of the first flow path and the second liquid flowing out of the second flow path, wherein the insoluble fluid introduction section is located upstream of the mixing section where a solid compound precipitates.

2. The manufacturing apparatus according to claim 1, wherein in the mixing section, the first liquid flowing out from the first flow path and the second liquid flowing out from the second flow path are mixed and flow into a mixing flow path, and in the mixing flow path, a slug flow is formed in which first cells containing the first liquid and the second liquid and second cells containing the immiscible fluid flow alternately, and the distance between the second cells in the slug flow is equal to or less than the flow path diameter of the mixing flow path.

3. The manufacturing apparatus according to claim 1 or 2, wherein the second flow path is formed so as to surround the outlet of the first flow path.

4. The manufacturing apparatus according to claim 3, wherein the insoluble fluid introduction section introduces the insoluble fluid into the first liquid.

5. The manufacturing apparatus according to claim 1 or 2, wherein the angle between the first flow path and the second flow path is 90° or less.

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