Crystallization apparatus, crystallization system, and crystallization method

Abstract

The crystallization device (4) includes: a stirring blade (W) having a plurality of holes (h) through in a radial direction and rotatable around a rotation axis (3); a bottomed cylindrical reaction tank (1) capable of housing the stirring blade (W) in a concentric manner inside; a first liquid supply portion (5a) provided to the reaction tank (1) and capable of supplying a first reaction liquid (L1) to the inside of the reaction tank (1); and a second liquid supply portion (5b) provided to the stirring blade (W) and capable of supplying a second reaction liquid (L2).

Description

Technical Field

[0001] This invention relates to crystallization apparatus, crystallization system, and crystallization method.

[0002] This application claims priority to Japanese Patent Application No. 2021-052574, filed on March 26, 2021, the contents of which are incorporated herein by reference. Background Technology

[0003] As a crystallization apparatus for mixing multiple raw material solutions to obtain particles of raw materials from the raw material solutions, crystallization apparatuses described in Patent Documents 1 to 4 are known.

[0004] In the crystallization apparatus described above, stirring is promoted by applying shear force to the mixture by rotating stirring blades disposed in a mixture of multiple feed solutions. To generate particles with more uniform particle size and higher quality, it is important to effectively transmit the shear force generated by the high-speed rotation of the stirring blades to the reaction field, which is the field where multiple feed solutions come into contact and react to generate particles. To achieve effective shear force transmission, efforts are made to minimize the gap between the stirring blades (rotor) and the reaction tank or reaction liquid supply nozzle (stator).

[0005] However, the faster the stirring blades rotate, the more difficult it becomes to minimize the gaps between the stirring blades and the reaction tank, and between the stirring blades and the reaction liquid supply nozzles, from the perspective of manufacturing precision when producing industrial-scale devices.

[0006] Patent Document 1: Japanese Patent Application Publication No. 2010-137183

[0007] Patent Document 2: Japanese Patent Application Publication No. 2010-022894

[0008] Patent Document 3: Japanese Patent No. 3256801

[0009] Patent Document 4: Japanese Patent Application Publication No. 2016-87590

[0010] The present invention is proposed in this context. The purpose of the present invention is to provide a crystallization apparatus, crystallization system and crystallization method that can minimize the gap between the stirring blade and the reaction liquid supply nozzle without requiring high manufacturing precision, and can use the very close distance, for example within 2 mm, of the inner and outer peripheries of the stirring blade with the highest shear force as the reaction start point. Summary of the Invention

[0011] In order to solve the above-mentioned problems and achieve this objective, the present invention proposes the following solution.

[0012] The first aspect of the present invention is a crystallization apparatus, characterized in that it comprises: a stirring blade having a plurality of holes extending radially and capable of rotating about a central axis; a bottomed cylindrical reaction tank capable of concentrically housing the stirring blade inside; a first liquid supply unit disposed in the reaction tank and capable of supplying a first reaction liquid to the interior of the reaction tank; and a second liquid supply unit disposed in the stirring blade and capable of supplying a second reaction liquid to the interior of the reaction tank.

[0013] According to the first aspect of the present invention, since the second reaction liquid is supplied from the second liquid supply section provided on the stirring blade, the high manufacturing precision required when the reaction liquid supply nozzle and the stirring blade are separately provided is not necessary. The second reaction liquid can be supplied to a very close range, for example, within 2 mm, of the inner and outer peripheries of the stirring blade where the shear force is highest. Furthermore, since the stirring blade has multiple holes penetrating radially, the mixture of the first and second reaction liquids reacts while moving radially outward through the holes towards the outer periphery of the stirring blade due to centrifugal force. Therefore, stirring of the mixture within a very close range, for example, within 2 mm, of the inner and outer peripheries of the stirring blade where the shear force is highest can be further promoted.

[0014] The second aspect of the present invention is characterized in that, in the first aspect, the stirring blade comprises: a cylindrical portion; a disc portion, the outer edge of which is fixed to the inner circumferential surface of the cylindrical portion; and a rotating shaft extending upward along the central axis from the center of the disc portion when viewed from above, wherein the second reaction liquid can flow inside the disc portion and the rotating shaft, and a second liquid supply portion is provided at the outer edge of the disc portion.

[0015] According to a second aspect of the present invention, since a second liquid supply section is provided at the outer edge of the disk portion, the second reaction liquid can be supplied to a range within a very close distance, for example, within 2 mm, from the inner and outer peripheries of the stirring blade where the shear force is highest.

[0016] The third aspect of the present invention is characterized in that, in the second aspect, the second liquid supply section opens downwards.

[0017] According to a third aspect of the invention, since the second liquid supply section opens downwards, the second reaction liquid can be supplied to a very close distance, for example, within 2 mm, to the inner and outer peripheries of the stirring blade where the shear force is highest.

[0018] The fourth aspect of the present invention is characterized in that, in the second aspect, the second liquid supply section opens radially outward and penetrates the cylindrical section.

[0019] According to a fourth aspect of the invention, since the second liquid supply section opens radially outward and penetrates the cylindrical section, the second reaction liquid can be supplied to a very close distance, for example, within 2 mm, to the inner and outer peripheries of the stirring blade where the shear force is highest.

[0020] The fifth aspect of the present invention is characterized in that, in the third or fourth aspect, the plurality of radially penetrating holes are blocked at an upper position of the cylindrical portion compared to the disc portion, and a disc-shaped second disc portion is provided at the upper end of the cylindrical portion, the outer edge of the second disc portion being fixed to the inner circumferential surface of the cylindrical portion.

[0021] According to the fifth aspect of the present invention, the second reaction liquid supplied from the second liquid supply section can be supplied to a very close distance, for example, within 2 mm, from the inner and outer peripheries of the stirring blade where the shear force is highest, and the resistance when the stirring blade rotates can be reduced, thereby reducing the power required to rotate the stirring blade.

[0022] The sixth aspect of the present invention is characterized in that, in the third aspect, the disk portion is disposed at the upper end of the cylindrical portion.

[0023] According to the sixth aspect of the present invention, since the disc portion is provided at the upper end of the cylindrical portion, the second reaction liquid supplied from the second liquid supply portion can be supplied to a range within a very close distance, for example, within 2 mm, from the inner and outer peripheries of the stirring blade with the highest shear force. Furthermore, since the stirring blade is not provided at a position higher than the disc portion, it is possible to construct a lightweight and simple stirring blade.

[0024] The seventh aspect of the present invention is characterized in that, in any of the first to sixth aspects, the circumferential speed of the stirring blade is more than 5 m / s and less than 50 m / s.

[0025] According to the seventh aspect of the present invention, since the circumferential speed of the stirring blade is more than 5 m / s and less than 50 m / s, sufficient shear force can be applied to the mixture of the first reaction liquid and the second reaction liquid.

[0026] The eighth aspect of the present invention is characterized in that, in any of the second to seventh aspects, when the gap between the outer peripheral surface of the cylindrical portion and the inner peripheral surface of the reaction tank is set to L3 and the height of the cylindrical portion is set to H, H / L3 is 10 or more.

[0027] According to the eighth aspect of the present invention, the gap between the outer peripheral surface of the stirring blade and the inner peripheral surface of the reaction tank is set within a range that is not too difficult to manufacture, relative to the size of the stirring blade. Therefore, when manufacturing an industrial-scale device, the reaction start point of the reaction between the first reaction liquid and the second reaction liquid can be set within a very close distance (e.g., within 2 mm) from the inner and outer peripheral surfaces of the stirring blade where the shear force is highest.

[0028] The ninth aspect of the present invention is characterized in that, in any one of the first to eighth aspects, the second liquid supply unit is provided as a plurality of units.

[0029] According to the ninth aspect of the present invention, since multiple second liquid supply units are provided, the mixing of the second reaction liquid and the first reaction liquid can be carried out faster than when a single second liquid supply unit is provided.

[0030] The tenth aspect of the present invention is characterized in that, in the first aspect, the stirring blade comprises: a cylindrical portion; a disk base disposed concentrically with the upper end of the cylindrical portion; a rotating shaft extending upward along the central axis when viewed from above the center of the disk base; and a cylindrical perforated plate disposed concentrically with the cylindrical portion on the radially outer side of the cylindrical portion, the perforated plate extending downward from the outer edge of the disk base, the second reaction liquid being able to flow inside the rotating shaft, the disk base, and the cylindrical portion, and a plurality of second liquid supply portions being disposed at intervals in the vertical direction on the outer circumferential surface of the cylindrical portion.

[0031] According to the tenth aspect of the present invention, the second reaction liquid can be supplied to a very close distance, for example, within 2 mm, to the inner and outer peripheries of the stirring blade where the shear force is highest. Since multiple second liquid supply sections are provided at intervals in the vertical direction, the first and second reaction liquids can be mixed more uniformly, and the effect of the shear force can be applied to more areas, thus producing uniform and fine particles.

[0032] The eleventh aspect of the present invention is characterized in that, in the first aspect, the stirring blade comprises: a cylindrical portion; a rotating shaft extending upward along the central axis when viewed from above the center of the cylindrical portion; and a cylindrical perforated plate arranged concentrically with the cylindrical portion on the radially outer side of the cylindrical portion, the perforated plate being fixed to a connecting rod extending radially outward from the outer circumference of the cylindrical portion, the second reaction liquid being able to flow inside the rotating shaft and the cylindrical portion, and a plurality of second liquid supply portions being provided on the outer circumference of the cylindrical portion at intervals in the vertical direction.

[0033] According to the eleventh aspect of the present invention, the second reaction liquid can be supplied to a very close distance, for example, within 2 mm, to the inner and outer peripheries of the stirring blade where the shear force is highest. Since multiple second liquid supply sections are provided at intervals in the vertical direction, the first and second reaction liquids can be mixed more uniformly, and the effect of the shear force can be applied to more areas, thus producing uniform and fine particles.

[0034] The 12th aspect of the present invention is characterized in that, in the 10th or 11th aspect, an extension tube is provided that extends radially outward from a plurality of second liquid supply sections.

[0035] According to the 12th aspect of the present invention, the second reaction liquid can be supplied to a very close distance, for example, within 2 mm, to the inner and outer peripheries of the stirring blade with the highest shear force, and the gap between the outer peripheral surface of the cylindrical portion and the inner peripheral surface of the perforated plate can be increased, thereby promoting the circulation of the reaction liquid.

[0036] The 13th aspect of the present invention is a crystallization system, characterized in that it comprises: a crystallization apparatus of any one of the first to 12 aspects; a retention tank for retaining the product transferred from the reaction tank; and a circulation pump for circulating the product between the retention tank and the crystallization apparatus.

[0037] According to the 13th aspect of the present invention, a crystallization system can be obtained that achieves the technical effects of the crystallization apparatus of any of the first to 12th aspects.

[0038] The 14th aspect of the present invention is a crystallization method, characterized by the following steps included in a crystallization apparatus: a first liquid supply step, supplying a first reaction liquid from a first liquid supply unit to a reaction tank; and a second liquid supply step, supplying a second reaction liquid from a second liquid supply unit to the reaction tank, wherein the crystallization apparatus includes: a stirring blade having a plurality of radially penetrating holes and rotating about a central axis; a bottomed cylindrical reaction tank, concentrically housing the stirring blade inside; a first liquid supply unit, supplying the first reaction liquid into the interior of the reaction tank; and a second liquid supply unit disposed on the stirring blade and capable of supplying the second reaction liquid, wherein the crystallization apparatus obtains a product by mixing two or more liquids.

[0039] According to the 14th aspect of the present invention, since the second reaction liquid is supplied from the second liquid supply section provided on the stirring blade, the high manufacturing precision required when the reaction liquid supply nozzle and the stirring blade are separately provided is not needed. The second reaction liquid can be supplied to a range within a very close distance, for example, within 2 mm, from the inner and outer peripheries of the stirring blade where the shear force is highest. Furthermore, since the stirring blade has multiple holes extending radially, the mixture of the first and second reaction liquids reacts while moving radially outward through the holes towards the outer periphery of the stirring blade due to centrifugal force. Therefore, stirring of the mixture within a very close distance, for example, within 2 mm, from the inner and outer peripheries of the stirring blade where the shear force is highest can be further promoted.

[0040] The 15th aspect of the present invention is characterized in that, in the 14th aspect, the stirring blade further comprises: a cylindrical portion; a disc portion, the outer edge of which is fixed to the inner circumferential surface of the cylindrical portion; and a rotating shaft extending upward along the central axis from the center of the disc portion when viewed from above, wherein the second reaction liquid can flow inside the disc portion and the rotating shaft, and in the second liquid supply step, the second reaction liquid is supplied downward from the outer edge of the disc portion.

[0041] According to the 15th aspect of the present invention, since the second reaction liquid is supplied downward from the outer edge of the disk portion, the second reaction liquid can be supplied to a very close distance, for example, within 2 mm, to the inner and outer peripheries of the stirring blade with the highest shear force.

[0042] The 16th aspect of the present invention is characterized in that, in the 14th aspect, the stirring blade further comprises: a cylindrical portion; a disc portion, the outer edge of which is fixed to the inner circumferential surface of the cylindrical portion; and a rotating shaft extending upward along the central axis from the center of the disc portion when viewed from above, wherein the second reaction liquid can flow inside the disc portion and the rotating shaft, and in the second liquid supply step, the second reaction liquid is supplied radially outward from the outer edge of the disc portion through the cylindrical portion.

[0043] According to the 16th aspect of the present invention, since the second reaction liquid is supplied radially outward from the outer edge of the disc portion through the cylindrical portion, the second reaction liquid can be supplied to a range within a very close distance, for example, within 2 mm, from the inner and outer peripheries of the stirring blade with the highest shear force.

[0044] The 17th aspect of the present invention is characterized in that, in the 14th aspect, the stirring blade comprises: a cylindrical portion; a disk base disposed concentrically with the upper end of the cylindrical portion; a rotating shaft extending upward along the central axis from the center of the disk base when viewed from above; and a cylindrical perforated plate disposed concentrically with the cylindrical portion on the radially outer side of the cylindrical portion, the perforated plate extending downward from the outer edge of the disk base, the second reaction liquid being able to flow inside the rotating shaft, the disk base, and the cylindrical portion, and in the second liquid supply step, the second reaction liquid being supplied radially outward from a plurality of second liquid supply portions disposed at intervals in the vertical direction on the outer peripheral surface of the cylindrical portion.

[0045] According to the 17th aspect of the present invention, the second reaction liquid supplied from the second liquid supply section can be supplied to a range within a very close distance, for example, within 2 mm, from the inner and outer peripheries of the stirring blade where the shear force is highest, and the first and second reaction liquids can be mixed more uniformly, and the effect of the shear force can be applied to more areas, thus enabling the production of uniform and fine particles.

[0046] The 18th aspect of the present invention is characterized in that, in the 14th aspect, the stirring blade comprises: a cylindrical portion; a rotating shaft extending upward along the central axis when viewed from above the center of the cylindrical portion; and a cylindrical perforated plate arranged concentrically with the cylindrical portion on the radially outer side of the cylindrical portion, the perforated plate being fixed to a connecting rod extending radially outward from the outer circumferential surface of the cylindrical portion, the second reaction liquid being able to circulate inside the rotating shaft and the cylindrical portion, and in the second liquid supply step, the second reaction liquid being supplied radially outward from a plurality of second liquid supply portions arranged at intervals in the vertical direction on the outer circumferential surface of the cylindrical portion.

[0047] According to the 18th aspect of the present invention, the second reaction liquid supplied from the second liquid supply section can be supplied to a range within a very close distance, for example, within 2 mm, from the inner and outer peripheries of the stirring blade where the shear force is highest, and the first and second reaction liquids can be mixed more uniformly, and the effect of the shear force can be applied to more areas, thus enabling the production of uniform and fine particles.

[0048] According to the present invention, a crystallization apparatus, crystallization system and crystallization method can be obtained that can minimize the gap between the stirring blade and the reaction liquid supply nozzle without requiring high manufacturing precision, and can take the extremely close distance, for example within 2 mm, from the inner and outer peripheries of the stirring blade with the highest shear force as the reaction start point. Attached Figure Description

[0049] Figure 1 This is a longitudinal sectional view of the crystallization apparatus according to the first embodiment of the present invention.

[0050] Figure 2A This is a longitudinal sectional view showing a schematic diagram of the stirring blades of the crystallization apparatus according to the first embodiment of the present invention.

[0051] Figure 2B This is a top view showing a schematic diagram of the stirring blades of the crystallization apparatus according to the first embodiment of the present invention.

[0052] Figure 3 This is a schematic diagram of a crystallization system including the crystallization apparatus of the first embodiment of the present invention.

[0053] Figure 4 This is a schematic diagram showing a first modified example of the crystallization apparatus according to the first embodiment of the present invention.

[0054] Figure 5A This is a front cross-sectional view showing a schematic diagram of the main parts of a second modified example of the crystallization apparatus according to the first embodiment of the present invention.

[0055] Figure 5B This is a top view showing a schematic diagram of the main parts of a second modified example of the crystallization apparatus according to the first embodiment of the present invention.

[0056] Figure 6A This is a front cross-sectional view showing a schematic diagram of the main parts of a third modified example of the crystallization apparatus according to the first embodiment of the present invention.

[0057] Figure 6B This is a top view showing a schematic diagram of the main parts of a third modified example of the crystallization apparatus according to the first embodiment of the present invention.

[0058] Figure 7A This is a front cross-sectional view showing a schematic diagram of the main parts of a fourth modified example of the crystallization apparatus according to the first embodiment of the present invention.

[0059] Figure 7B This is a top view showing a schematic diagram of the main parts of a fourth modified example of the crystallization apparatus according to the first embodiment of the present invention.

[0060] Figure 8A This is a front cross-sectional view showing a schematic diagram of the main parts of a fifth modified example of the crystallization apparatus according to the first embodiment of the present invention.

[0061] Figure 8B This is a top view showing a schematic diagram of the main parts of a fifth modified example of the crystallization apparatus according to the first embodiment of the present invention.

[0062] Figure 9 This is a schematic diagram of the main parts of a sixth modified example of the crystallization apparatus according to the first embodiment of the present invention.

[0063] Figure 10 This is a schematic diagram of the main parts of a seventh modified example of the crystallization apparatus according to the first embodiment of the present invention.

[0064] Figure 11 This is a schematic diagram of the main parts of an eighth modified example of the crystallization apparatus according to the first embodiment of the present invention.

[0065] Figure 12 This is a schematic diagram of the main parts of a ninth modified example of the crystallization apparatus according to the first embodiment of the present invention. Detailed Implementation

[0066] Below, refer to Figure 1 The crystallization apparatus 4 according to the first embodiment is described below. The crystallization apparatus 4 includes: a bottomed cylindrical reaction tank 1 with a central shaft O1 facing vertically; and cylindrical stirring blades W. The stirring blades W are rotatable about a hollow rotating shaft 3 extending upward from the center when viewed from above, and the central shaft O1 is housed inside the reaction tank 1 as the same central shaft. The rotating shaft 3 is rotated by a rotational force supplied by a prime mover M provided outside the crystallization apparatus 4 via a belt B. Furthermore, the prime mover M is not particularly limited to any device that generates rotational power, such as an electric motor or an engine. In addition, the belt B that transmits the rotational force to the rotating shaft 3 is not particularly limited to any device capable of transmitting rotational force, such as a chain or gear. Furthermore, the bottom surface of the reaction tank 1 can be either a flat surface as shown in the figure or a conical shape that protrudes downwards. A discharge port 6 is provided at the upper part of the reaction tank 1, which can discharge the slurry containing particles (crystallization) generated in the reaction tank 1 to the next process. In reaction tank 1, a buffer plate (baffle) 7 is provided on the upper side of the stirring blades W to suppress the generation of eddies and promote the stirring of the mixture. The buffer plate 7 is constructed by installing flat plates or cylindrical tubes at equal intervals. In addition, since the buffer plate 7 is provided as needed, it may not be provided.

[0067] A first supply section 5a is provided at the lower part of the reaction tank 1 to supply the first reaction liquid L1. The first reaction liquid L1 is supplied to the reaction tank 1 in the desired amount from the first supply section 5a.

[0068] Below, refer to Figure 1 , Figure 2A and Figure 2B The stirring blade W of the crystallization apparatus 4 involved in the first embodiment is explained.

[0069] The stirring blade W comprises: a cylindrical portion 2; and a disc-shaped portion 8, the outer edge of which is fixed to the inner circumferential surface 2i of the cylindrical portion 2. The disc portion 8 is positioned approximately half the height of the cylindrical portion 2, but is not limited to this example; it may also be positioned approximately half the height of the cylindrical portion 2, either below or above. A rotating shaft 3 is fixed at the center of the disc portion 8 when viewed from above. The hollow interior of the rotating shaft 3 is a pipe P1. Inside the disc portion 8, multiple pipes P2 extend radially from the center to the outer edge. The pipes P1 of the rotating shaft 3 communicate with the pipes P2 of the disc portion 8. A second reaction liquid L2 is supplied from a tank T located outside the crystallization apparatus 4 to the rotating shaft 3 of the stirring blade W. The second reaction liquid L2 is supplied to the hollow pipe P1 of the rotating shaft 3 via a rotary joint R, and then to the pipes P2 of the disc portion 8. The radially outer front end of the reaction tank 1 of pipeline P2 opens downwards, becoming a second liquid supply section 5b for discharging the second reaction liquid L2. Therefore, multiple second liquid supply sections 5b are provided at intervals along the circumference of the disc portion 8. Figure 2A and Figure 2B In the example shown, such as Figure 2B As shown, eight second liquid supply sections 5b are provided. The number of second liquid supply sections 5b is not limited, but they are preferably arranged symmetrically with respect to the central axis O1.

[0070] In this embodiment, the distance between the inner circumferential surface 2i of the cylindrical portion 2 of the stirring blade W and the center of the second liquid supply portion 5b is 2 mm or less. Furthermore, if the distance (gap) between the outer circumferential surface 2o of the cylindrical portion 2 of the stirring blade W and the inner circumferential surface 1i of the reaction tank 1 is set as L3, and the height of the stirring blade W (cylindrical portion 2) along the central axis O1 is set as H, then the ratio of H to L3, H / L3, is preferably 10 or more. Moreover, H / L3 is more preferably 25 or more. Therefore, even when using a device with a different size than that of this embodiment, the same device can be manufactured based on this ratio. The stirring blade W rotates at a circumferential speed of 5 m / s or more and 50 m / s or less.

[0071] Furthermore, the H / L3 ratio may differ from the ratios described above, depending on the intended purpose. For example, in cases where it is desirable to suppress crystal breakage, the ratio may be reduced from the values ​​mentioned above.

[0072] A plurality of holes h extending radially through the cylindrical portion 2 of the stirring blade W are provided. A first reaction liquid L1, a second reaction liquid L2, or a mixture thereof can flow through these holes h. Therefore, the first reaction liquid L1, the second reaction liquid L2, or a mixture thereof can move from the inside to the outside of the stirring blade W or from the outside to the inside of the stirring blade W through the plurality of holes h. In addition to the holes h, a plurality of holes 9 extending in the direction of the central axis O1 may also be provided on the disc portion 8 (see description below). Figure 5A and Figure 5B In this case, in addition to the multiple holes h, the first reaction liquid L1, the second reaction liquid L2, or a mixture thereof can also move through the holes 9 from the inside to the outside of the stirring blade W or from the outside to the inside of the stirring blade W.

[0073] In this crystallization apparatus 4, a required amount of first reaction liquid L1 is supplied to the reaction tank 1 from the first liquid supply section 5a. The amount of first reaction liquid L1 supplied can be such that the reaction tank 1 is completely filled (full liquid state), or it can be supplied to such a degree that, when the stirring blade W rotates, the first reaction liquid L1 moves in a circular motion around the central axis O1 of the reaction tank 1, thereby generating centrifugal force in the first reaction liquid L1. Through this centrifugal force, the first reaction liquid L1 is pushed onto the inner circumferential surface 1i of the reaction tank 1, and a liquid film of the first reaction liquid L1 is formed on the inner circumferential surface 1i of the reaction tank 1. The supply amount of the first reaction liquid L1 can be adjusted by adjusting the opening of the opening adjustment valve V (described later) to select the desired supply amount. Hereinafter, the case where the first reaction liquid L1 is supplied to a full liquid state will be described. Alternatively, the supply of the first reaction liquid L1 can be stopped after it has been supplied to the extent that it has reached the state of full liquid or liquid film formation, and then the reaction can be carried out in the reaction tank 1. Or, the reaction in the reaction tank 1 can be continued while the flow rate of the first reaction liquid L1 is maintained at the level that has reached the state of full liquid or liquid film formation.

[0074] With the reaction tank 1 filled with the first reaction liquid L1, the stirring blade W is rotated, and the second reaction liquid L2 is discharged from the second supply section 5b along the inner circumferential surface 2i of the cylindrical portion 2 of the stirring blade W, thereby supplying the second reaction liquid L2 into the reaction tank 1. Thus, the second reaction liquid L2 discharged from the second supply section 5b along the inner circumferential surface 2i of the cylindrical portion 2 of the stirring blade W comes into contact with the first reaction liquid L1, which rotates near the inner circumferential surface 2i of the cylindrical portion 2 of the stirring blade W as the stirring blade W rotates. In this way, a reaction occurs through the contact of the first reaction liquid L1 and the second reaction liquid L2, thereby generating particles.

[0075] At this time, by supplying the second reaction liquid L2 to the first reaction liquid L1 from the second liquid supply section 5b of the stirring blade W rotating at a circumferential speed of 5 m / s or more and 50 m / s or less, the second reaction liquid L2 and the first reaction liquid L1 can be uniformly mixed.

[0076] Here, the centrifugal force generated by the first reaction liquid L1 rotating along with the stirring blade W, the second reaction liquid L2 discharged from the second liquid supply section 5b of the stirring blade W rotating at a circumferential speed of 5 m / s or more and 50 m / s or less, and their mixture causes the first reaction liquid L1, the second reaction liquid L2, and the mixture (hereinafter sometimes collectively referred to as the mixture) to move radially outward toward the cylindrical portion 2 of the stirring blade W. After passing through multiple holes h provided on the cylindrical portion 2 of the stirring blade W, they collide with the inner circumferential surface 1i of the reaction tank 1, and then move vertically along the inner circumferential surface 1i of the reaction tank 1. The mixture, which mainly moves downward, is attracted by the radially outward flow caused by the centrifugal force generated by the rotation of the stirring blade W, and again collides with the inner circumferential surface 1i of the reaction tank 1 after passing through multiple holes h provided on the cylindrical portion 2 of the stirring blade W. After that, it moves vertically along the inner circumferential surface 1i of the reaction tank 1, thereby generating convection. Here, as the mixture passes through multiple orifices h, it accelerates radially outward due to the effect of the throttling flow path, resulting in the highest radial outward flow velocity near the orifices h. Furthermore, the mixture between the outer circumferential surface 2o and inner circumferential surface 2i of the cylindrical portion 2 of the stirring blade W rotating at a circumferential speed of 5 m / s to 50 m / s and the inner circumferential surface 1i of the fixed reaction tank 1 is subjected to shear force in the circumferential direction. The closer the shear force applied to the mixture is to the inner circumferential surface 2i and outer circumferential surface 2o of the cylindrical portion 2 of the stirring blade W, the greater the shear force. The shear force applied to the mixture is a major factor determining the particle size and uniformity of the obtained particles. In particular, the greater the applied shear force, the finer the particles can be obtained.

[0077] In the crystallization apparatus 4 of this embodiment, the second liquid supply section 5b is provided at the outer edge of the disc section 8. Specifically, as described above, the distance between the inner circumferential surface 2i of the cylindrical section 2 of the stirring blade W and the center of the second liquid supply section 5b is 2 mm or less. Therefore, at the reaction start point where the second reaction liquid L2 discharged from the second liquid supply section 5b along the inner circumferential surface 2i of the cylindrical section 2 of the stirring blade W first comes into contact with the first reaction liquid L1 that rotates near the inner circumferential surface 2i of the cylindrical section 2 of the stirring blade W along with the rotation of the stirring blade W, a shear force is applied to the maximum extent, in addition to the flow toward the radially outward due to the influence of centrifugal force and the throttling flow path. Therefore, the area with the greatest applied shear force can be used as the reaction start point. Specifically, the reaction start point can be formed in a region within a very close distance, for example, 2 mm or less, from the inner circumferential surface 2i and the outer circumferential surface 2o of the cylindrical section 2 of the stirring blade W. Here, the mixture can move from the inner circumferential side to the outer circumferential side of the cylindrical section 2 through the aforementioned plurality of holes h. Therefore, shear force promotes the stirring of the first reaction liquid L1 and the second reaction liquid L2 at the reaction initiation point. Thus, more uniform mixing of the first reaction liquid L1 and the second reaction liquid L2 begins from the reaction initiation point, and mixing and reaction occur in a reaction field, which is the field where the reaction occurs along the flow of the mixture, thereby generating particles with fine and uniform diameters. Furthermore, when the reaction tank 1 is full, the buffer plate 7 has the effect of suppressing the generation of eddies and promoting the stirring of the mixture. On the other hand, when the reaction tank 1 is not full but forms a liquid film of the mixture, the buffer plate 7 is not needed. Here, the reaction initiation point refers to the region where the reaction begins, and the reaction field refers to the entire field where the reaction occurs. Therefore, the reaction initiation point is included in the reaction field.

[0078] Furthermore, the buffer plate 7 is not a necessary structure and can be omitted. For example, if a mechanical seal (not shown) is installed at the location where the rotating shaft 3 is inserted in the reaction tank 1, resulting in a completely saturated state without a gas phase, the buffer plate 7 can be omitted because it suppresses the generation of eddies. Without the buffer plate 7, the flow resistance is reduced, which can reduce the power of the prime mover M.

[0079] Furthermore, even when the liquid film is formed instead of the liquid being fully saturated, the same effect as in the case of full liquid can be obtained.

[0080] Figure 3 This is a schematic diagram of a crystallization system S equipped with the crystallization apparatus 4 of the first embodiment.

[0081] The crystallization system S of the crystallization apparatus 4 has a retention tank 10 downstream of the crystallization apparatus 4, into which slurry D1, including particles generated by the crystallization apparatus 4, is transferred. A discharge outlet for slurry D1 is provided at the upper part of the retention tank 10, and a first stock solution S3 of the first reaction liquid L1 is supplied to the retention tank 10 from a tank (not shown). A pipeline is provided on the retention tank 10 to discharge the mixture of the first stock solution S3 and slurry D1 to the outside. This pipeline is connected to the crystallization apparatus 4 via a circulation pump P. This pipeline, from the retention tank 10 to the crystallization apparatus 4, can supply a second stock solution S2 of the first reaction liquid L1 upstream of the circulation pump P as needed, and can also further discharge residual slurry D2 downstream of the circulation pump P.

[0082] Here, the circulation rate of the mixture of the first raw solution S3 and slurry D1 is adjusted by changing the rotational speed of the circulation pump P or by adjusting the opening of the circulation rate regulating valve (not shown) located downstream of the circulation pump P. The residence time of the mixture in the retention tank 10 is adjusted by changing the level of the slurry held in the retention tank 10. The level of the slurry in the retention tank 10 is adjusted by: selecting any one of the multiple slurry D1 discharge outlets (only one shown in the figure) located at different heights on the side of the retention tank 10; or by automatically adjusting the opening of the automatic valve V2 installed on the discharge outlet to automatically regulate the flow rate of the residual slurry D2 discharged from downstream of the circulation pump P to the outside of the crystallization system S, so that the value of the level gauge Lv1, which detects the level of the retention tank 10, becomes a predetermined value.

[0083] According to the crystallization system S including this crystallization device 4, the shear force, the circulation volume of the first reaction liquid L1, and the residence time of the slurry that affect the particle quality such as particle size, particle size distribution, and sphericity of the reaction products in the crystallization device 4 can be adjusted respectively, thereby further improving the particle quality control performance.

[0084] Figure 4 This is a schematic diagram showing a first modified example of the crystallization apparatus 4 according to the first embodiment.

[0085] In this crystallization apparatus 4a, an opening adjustment valve V is provided on the outlet 6. By adjusting the opening of this opening adjustment valve V, the reaction tank 1 can be selected as either a full liquid state or a liquid film state in which a liquid film is formed.

[0086] Figure 5A and Figure 5B This is a schematic diagram showing the main parts of a second variation of the crystallization apparatus 4 according to the first embodiment. The difference in the second variation is that the stirring blade W of the crystallization apparatus 4 in the first embodiment is a stirring blade Wa. In the following description, only the differences from the stirring blade W will be explained, and repeated descriptions will be omitted.

[0087] like Figure 5A As shown, the difference between stirring blade Wa and stirring blade W is that the second liquid supply section 5b, located at the outer edge of the disc portion 8, penetrates the cylindrical portion 2 and opens radially outward. In this stirring blade Wa, since the second reaction liquid L2 is discharged from the radially outward-opening second liquid supply section 5b, the dispersion of the second reaction liquid L2 and the mixture of the first reaction liquid L1 and the second reaction liquid L2 in the radial (horizontal direction) is higher. By using a crystallization apparatus 4 equipped with this stirring blade Wa, the same effect as that of a crystallization apparatus 4 equipped with stirring blade W can be achieved. Furthermore, in Figure 5A and Figure 5B In the example, such as Figure 5B As shown, the disk portion 8 has a plurality of holes 9 extending in the direction of the central axis O1, but it is also possible not to have a plurality of holes 9. When a plurality of holes 9 are provided, it is preferable that they are arranged symmetrically with respect to the center of the disk portion 8. The number of the plurality of holes 9 is not limited to this. Figure 5B The eight shown.

[0088] Here, the multiple holes 9 allow a portion of the mixture to flow through the holes 9 on the underside and top side of the stirring blade W, thereby reducing the dynamic load applied to the stirring blade W. However, since the mixture passing through the multiple holes 9 passes through the reaction field (short path) instead of the reaction field around the stirring blade W, the effect of producing uniform and fine particles is reduced compared to the case without the multiple holes 9. Therefore, the application of the holes 9 can be selected considering the target particle mass and the required power.

[0089] Figure 6A and Figure 6B This is a schematic diagram showing the main parts of a third modification of the crystallization apparatus 4 according to the first embodiment. The difference in this third modification is that the stirring blade Wa in the second modification of the crystallization apparatus 4 of the first embodiment is replaced by a stirring blade Wb. In the following description, only the differences from the stirring blade Wa will be explained, and repeated descriptions will be omitted.

[0090] like Figure 6A As shown, in the cylindrical portion 2 of the stirring blade Wb, which is located higher than the disc portion 8, the multiple radially penetrating holes h are blocked, and a second disc portion 15 is provided at the upper end of the cylindrical portion 2, with its outer edge fixed to the inner circumferential surface 2i of the cylindrical portion 2. The second disc portion 15 is a disc-shaped component with a hole in its center through which the rotating shaft 3 passes. Apart from the hole through which the rotating shaft 3 passes, there are no holes penetrating the second disc portion 15 in the direction of the central axis O1. Therefore, the first reaction liquid L1, the second reaction liquid L2, and their mixture will not enter the inner side of the second disc portion 15.

[0091] In this stirring blade Wb, multiple radially penetrating holes h are not provided on the upper side of the cylindrical portion 2 compared to the disc portion 8. Furthermore, a second disc portion 15, with its outer edge fixed to the inner circumferential surface 2i of the cylindrical portion 2, is provided at the upper end of the cylindrical portion 2. Therefore, the resistance of the stirring blade Wb during rotation is reduced, allowing it to operate with less power than the stirring blade Wa.

[0092] Figure 7A and Figure 7B This is a schematic diagram showing the main parts of a fourth modification of the crystallization apparatus 4 according to the first embodiment. The difference in this fourth modification is that the stirring blade W of the crystallization apparatus 4 in the first embodiment is a stirring blade Wc. In the following description, only the differences from the stirring blade W will be explained, and repeated descriptions will be omitted.

[0093] like Figure 7A As shown, in the cylindrical portion 2 of the stirring blade Wc, which is located higher than the disc portion 8, the multiple radially penetrating holes h are blocked, and a second disc portion 15 is provided at the upper end of the cylindrical portion 2, with its outer edge fixed to the inner circumferential surface 2i of the cylindrical portion 2. The second disc portion 15 is a disc-shaped component with a hole in its center through which the rotating shaft 3 passes. Apart from the hole through which the rotating shaft 3 passes, there are no holes penetrating the second disc portion 15 in the direction of the central axis O1. Therefore, the first reaction liquid L1, the second reaction liquid L2, and their mixture will not enter the inner side of the second disc portion 15.

[0094] In this stirring blade Wc, since multiple radially penetrating holes h are not provided in the upper part of the cylindrical portion 2 compared to the disc portion 8, and a second disc portion 15 with its outer edge fixed to the inner circumferential surface 2i of the cylindrical portion 2 is provided at the upper end of the cylindrical portion 2, the resistance of the stirring blade Wc when rotating is reduced. Therefore, the stirring blade Wc can be operated with less power than the stirring blade W.

[0095] Figure 8A and Figure 8B This is a schematic diagram of the main parts of a fifth modification of the crystallization apparatus 4 according to the first embodiment. The difference in this fifth modification is that the stirring blade W of the crystallization apparatus 4 in the first embodiment is a stirring blade Wd. In the following description, only the differences from the stirring blade W will be explained, and repeated descriptions will be omitted.

[0096] like Figure 8AAs shown, the stirring blade Wd differs from the stirring blade W in that the disc portion 8 is located at the upper end of the cylindrical portion 2. Furthermore, the height of the cylindrical portion 2 is approximately half the height of the cylindrical portion 2 of the stirring blade W. By using a crystallization apparatus 4 equipped with this stirring blade Wd, the same effect as that achieved with a crystallization apparatus 4 equipped with the stirring blade W can be achieved. Additionally, since the cylindrical portion 2 is not located above the disc portion 8, the stirring blade Wd can be made lighter than the stirring blade W, and its structure can be simplified. Therefore, the stirring blade Wd can be operated with less power than the stirring blade W, leading to energy savings in the crystallization apparatus 4 and ease of manufacturing of the stirring blade Wd. Furthermore, since the height of the cylindrical portion 2 is kept shorter, the crystallization apparatus 4 can be miniaturized. Moreover, in Figure 8A and Figure 8B In the example, such as Figure 8B As shown, the disk portion 8 does not have multiple holes 9 extending through the central axis O1, but multiple holes 9 can also be provided. In this case, the same effect can be expected as when multiple holes 9 extending through the central axis O1 are provided on the disk portion 8 of the stirring blade Wa.

[0097] Figure 9 This is a schematic diagram of the main parts of a sixth modification of the crystallization apparatus 4 according to the first embodiment. The difference in the sixth modification is that the stirring blade W of the crystallization apparatus 4 in the first embodiment is replaced by a stirring blade We. In the following description, only the differences from the stirring blade W will be explained, and repeated descriptions will be omitted.

[0098] like Figure 9As shown, the stirring blade We comprises: a cylindrical portion 20; a disk base 18, concentrically positioned at the upper end of the cylindrical portion 20; a rotating shaft 3, extending upward along a central axis O1 from the center of the disk base 18 when viewed from above; and a cylindrical perforated plate 18P, concentrically positioned on the radially outer side of the cylindrical portion 20. Multiple holes 18h are provided on the perforated plate 18P, penetrating radially, allowing the first reaction liquid L1, the second reaction liquid L2, and their mixture to flow through the holes 18h. The perforated plate 18P extends downward from the outer edge of the disk base 18. The second reaction liquid can flow through pipes P1, P2, and P3 located inside the rotating shaft 3, the disk base 18, and the cylindrical portion 20, respectively. Pipes P1, P2, and P3 are interconnected. Pipe P2 extends radially outward from the lower end of pipe P1, centered on the central axis O1. Pipe P3 extends downward along the central axis O1 from the radially outer end of pipe P2. Pipes P2 and P3 are formed inside the cylindrical portion 20. Multiple second liquid supply sections 50b are provided on the outer circumferential surface 20o of the cylindrical portion 20 at intervals in the vertical direction. When the stirring blades We rotate, the rotating shaft 3, the disk base 18, the cylindrical portion 20, and the perforated plate 18P rotate as a unit.

[0099] In this stirring blade We, a second reaction liquid L2 is supplied to the reaction tank 1 from a plurality of second liquid supply sections 50b arranged at intervals in the vertical direction on the outer peripheral surface 20o of the cylindrical portion 20. The second reaction liquid L2 flows through a plurality of holes 18h in the porous plate 18P while mixing and reacting with the first reaction liquid L1 in the reaction tank 1. Therefore, the first reaction liquid L1 and the second reaction liquid L2 can be mixed more uniformly.

[0100] The mixture passing through the multiple holes 18h of the perforated plate 18P collides with the inner circumferential surface 1i of the reaction tank 1, and then moves vertically along the inner circumferential surface 1i of the reaction tank 1. The downward-moving mixture is attracted by the radially outward flow caused by the centrifugal force generated by the rotation of the stirring blades We, and after passing through the multiple holes 18h of the perforated plate 18P of the stirring blades We again, it collides with the inner circumferential surface 1i of the reaction tank 1, and then moves vertically along the inner circumferential surface 1i of the reaction tank 1, thereby generating convection. Here, when the mixture passes through the multiple holes 18h, due to the effect of the throttling flow path, the mixture is accelerated radially outward, so the radially outward flow velocity of the mixture is the highest near the multiple holes 18h. Furthermore, the mixture between the outer circumferential surface 20o of the cylindrical portion 20 of the stirring blades We rotating at a circumferential speed of 5 m / s or more and 50 m / s or less, the inner and outer circumferential surfaces of the perforated plate 18P, and the fixed inner circumferential surface 1i of the reaction tank 1 is subjected to shear force in the circumferential direction. The closer the shear force applied to the mixture is to the outer circumferential surface 2o of the cylindrical portion 20 of the stirring blade We and the inner and outer circumferential surfaces of the porous plate 18P, the greater the shear force. The shear force applied to the mixture is a major factor determining the particle size and uniformity of the resulting particles. In particular, the greater the applied shear force, the finer the particles can be obtained. When using the stirring blade We, compared to using the stirring blade W, the shear force can be applied to a wider area, thus enabling the production of uniform and fine particles.

[0101] The second reaction liquid L2 supplied from the second liquid supply section 50b can be supplied to the inner and outer peripheries of the stirring blade We with the highest shear force, that is, within a very close distance, for example, within 2 mm, from the outer peripheral surface 20o of the cylindrical part 20 and the inner and outer peripheral surfaces of the perforated plate 18P.

[0102] exist Figure 9 In the example, four second liquid supply sections 50b are provided in the vertical direction of the cylindrical section 20, but the number of second liquid supply sections 50b is not limited to this. Figure 9 For example, the size of reaction tank 1 can be increased or decreased.

[0103] Figure 10 This is a schematic diagram of the main parts of a seventh modification of the crystallization apparatus 4 according to the first embodiment. The difference in the seventh modification is that the stirring blade W of the crystallization apparatus 4 in the first embodiment is a stirring blade Wf. In the following description, only the differences from the stirring blade W will be explained, and repeated descriptions will be omitted.

[0104] like Figure 10As shown, the stirring blade Wf ​​includes: a cylindrical portion 20; a rotating shaft 3 extending upward along a central axis O1 from the center of the cylindrical portion 20 when viewed from above; and a cylindrical perforated plate 18P arranged concentrically with the cylindrical portion 20 on its radially outer side. Multiple holes 18h are provided on the perforated plate 18P, penetrating it radially, allowing the first reaction liquid L1, the second reaction liquid L2, and their mixture to flow through the holes 18h. The perforated plate 18P is fixed to a connecting rod 11 extending radially outward from the outer peripheral surface 2o of the cylindrical portion 20. The second reaction liquid can flow through pipes P1, P2, and P3 located inside the rotating shaft 3 and the cylindrical portion 20, respectively. Pipes P1, P2, and P3 are interconnected. Pipe P2 extends radially outward from the lower end of pipe P1, radiating outward from the central axis O1. Pipe P3 extends downward along the central axis O1 from the radially outer end of pipe P2. Pipes P2 and P3 are formed inside the cylindrical portion 20. Multiple second liquid supply sections 50b are provided on the outer circumferential surface 20o of the cylindrical portion 20 at intervals in the vertical direction. When the stirring blade Wf ​​rotates, the rotating shaft 3, the cylindrical portion 20, the connecting rods 11, and the perforated plate 18P rotate as a unit. Multiple connecting rods 11 are equally spaced in the circumferential direction of the cylindrical portion 20. Preferably, there are two or more connecting rods 11. The connecting rods 11 are positioned approximately half the height of the cylindrical portion 20, but this is not limited to this example; they may also be positioned above or below approximately half the height of the cylindrical portion 20.

[0105] In this stirring blade Wf, a second reaction liquid L2 is supplied to the reaction tank 1 from a plurality of second liquid supply sections 50b arranged at intervals in the vertical direction on the outer peripheral surface 20o of the cylindrical portion 20. The second reaction liquid L2 flows through a plurality of holes 18h in the porous plate 18P while mixing and reacting with the first reaction liquid L1 in the reaction tank 1. Therefore, the first reaction liquid L1 and the second reaction liquid L2 can be mixed more uniformly.

[0106] The mixture passing through the multiple holes 18h of the porous plate 18P collides with the inner circumferential surface 1i of the reaction tank 1, and then moves vertically along the inner circumferential surface 1i of the reaction tank 1. The mixture moving vertically is attracted by the radially outward flow caused by the centrifugal force generated by the rotation of the stirring blade Wf, and again collides with the inner circumferential surface 1i of the reaction tank 1 through the multiple holes 18h of the porous plate 18P of the stirring blade Wf. It then moves vertically along the inner circumferential surface 1i of the reaction tank 1, thereby generating convection. Here, as the mixture passes through the multiple holes 18h, it accelerates radially outward due to the effect of the throttling flow path, and therefore the radially outward flow velocity of the mixture is highest near the multiple holes 18h. Furthermore, the mixture between the outer circumferential surface 20o of the cylindrical portion 20 of the stirring blade Wf ​​rotating at a circumferential speed of 5 m / s or more and 50 m / s or less, the inner and outer circumferential surfaces of the porous plate 18P, and the fixed inner circumferential surface 1i of the reaction tank 1 is subjected to shear force in the circumferential direction. The closer the shear force applied to the mixture is to the outer circumferential surface 2o of the cylindrical portion 20 of the stirring blade Wf ​​and the inner and outer circumferential surfaces of the porous plate 18P, the greater the shear force. The shear force applied to the mixture is a major factor determining the particle size and uniformity of the resulting particles. In particular, the greater the applied shear force, the finer the particles can be obtained. When using the stirring blade Wf, the shear force can be applied to a wider area, thus enabling the production of uniform and fine particles.

[0107] The second reaction liquid L2 supplied from the second liquid supply section 50b can be supplied to the inner and outer peripheries of the stirring blade We with the highest shear force, that is, within a very close distance, for example, within 2 mm, from the outer peripheral surface 20o of the cylindrical part 20 and the inner and outer peripheral surfaces of the perforated plate 18P.

[0108] exist Figure 10 In the example, four second liquid supply sections 50b are provided in the vertical direction of the cylindrical section 20, but the number of second liquid supply sections 50b is not limited to this. Figure 10 For example, the size of reaction tank 1 can be increased or decreased.

[0109] Figure 11 This is a schematic diagram of the main parts of the eighth modification of the crystallization apparatus 4 according to the first embodiment. The difference in the eighth modification is that the stirring blade We in the sixth modification of the crystallization apparatus 4 of the first embodiment is a stirring blade Wg. In the following description, only the differences from the stirring blade We will be explained, and repeated descriptions will be omitted.

[0110] like Figure 11As shown, compared to the stirring blade We in the sixth modified example, the spacing between the outer peripheral surface 20o of the cylindrical portion 20 and the inner peripheral surface of the perforated plate 18P is larger in the stirring blade Wg. Furthermore, an extension tube 12 is provided that extends radially outward from the second liquid supply portion 50b, which opens radially outward in the stirring blade We, with the front end of the extension tube 12 being the second liquid supply portion 50b.

[0111] According to this stirring blade Wg, since the distance between the outer peripheral surface 20o of the cylindrical portion 20 and the inner peripheral surface of the porous plate 18P can be increased, the first reaction liquid L1, the second reaction liquid L2, and their mixture can easily flow into the space between the cylindrical portion 20 and the porous plate 18P. Therefore, the circulation of the reaction liquid can be promoted, thus producing uniform and fine particles. In addition, the second reaction liquid L2 supplied from the second liquid supply section 50b can be supplied to the inner and outer peripheral surfaces of the stirring blade Wg, which has the highest shear force, i.e., within a very close distance, for example, within 2 mm, of the inner and outer peripheral surfaces of the porous plate 18P.

[0112] Figure 12 This is a schematic diagram of the main parts of the ninth modification of the crystallization apparatus 4 according to the first embodiment. The difference in the ninth modification is that the stirring blade Wf ​​in the seventh modification of the crystallization apparatus 4 according to the first embodiment is a stirring blade Wh. In the following description, only the differences from the stirring blade Wf ​​will be explained, and repeated descriptions will be omitted.

[0113] like Figure 12 As shown, compared to the stirring blade Wf ​​in the seventh modified example, the spacing between the outer peripheral surface 20o of the cylindrical portion 20 and the perforated plate 18P is larger in the stirring blade Wh. In addition, an extension tube 12 is provided that extends radially outward from the second liquid supply portion 50b that opens radially outward in the stirring blade Wf, and the front end of the extension tube 12 is the second liquid supply portion 50b.

[0114] Based on this stirring blade Wh, the gap between the outer peripheral surface 20o of the cylindrical portion 20 and the inner peripheral surface of the porous plate 18P can be increased, thus allowing the first reaction liquid L1, the second reaction liquid L2, and their mixture to easily flow into the space between the cylindrical portion 20 and the porous plate 18P. Therefore, the circulation of the reaction liquid can be promoted, resulting in the production of uniform and fine particles. Furthermore, the second reaction liquid L2 supplied from the second liquid supply section 50b can be supplied to a very close range, for example, within 2 mm, of the inner and outer peripheral surfaces of the stirring blade Wg, where the shear force is highest.

[0115] In the above-described modifications, the stirring blade W of the crystallization apparatus 4 in the first embodiment, the stirring blade Wc of the fourth modification, and the stirring blade Wd of the fifth modification are able to mix the first reaction liquid L1 and the second reaction liquid L2 more uniformly.

[0116] Furthermore, generating particles by using the crystallization apparatus described in the above embodiments can be regarded as a crystallization method.

[0117] For example, this can be considered a crystallization method, which includes the following steps in the crystallization apparatus 4 of the first embodiment: a first liquid supply step, supplying a first reaction liquid L1 from a first liquid supply section 5a to a reaction tank 1; and a second liquid supply step, supplying a second reaction liquid L2 from a second liquid supply section 5b to the reaction tank 1, wherein the crystallization apparatus 4 includes: a cylindrical stirring blade W having a plurality of radially penetrating holes h and rotating about a central axis O1; a bottomed cylindrical reaction tank 1, concentrically housing the stirring blade W inside; a first liquid supply section 5a, disposed in the reaction tank 1 and supplying the first reaction liquid L1 into the interior of the reaction tank 1; and a second liquid supply section 5b, disposed on the stirring blade W and capable of supplying the second reaction liquid L2 into the interior of the reaction tank 1. According to this crystallization method, the same effect as that of the crystallization apparatus 4 of the first embodiment can be obtained.

[0118] Furthermore, this can be considered a crystallization method, wherein the stirring blade W of the crystallization apparatus 4 of the first embodiment further comprises: a cylindrical portion 2; a disc-shaped portion 8, the outer edge of which is fixed to the inner circumferential surface 2i of the cylindrical portion; and a rotating shaft 3, which extends upward along the central axis O1 from the center when viewed from above the disc portion 8. The second reaction liquid can flow inside the disc portion 8 and the rotating shaft 3, and in the second liquid supply step, the second reaction liquid L2 is supplied downward from the outer edge of the disc portion 8. According to this crystallization method, the same effect as that of the crystallization apparatus 4 of the first embodiment can be obtained.

[0119] Furthermore, this can be considered a crystallization method, wherein the stirring blade Wa of the second variation of the crystallization apparatus 4 of the first embodiment further comprises: a cylindrical portion 2; a disk-shaped portion 8, the outer edge of which is fixed to the inner circumferential surface of the cylindrical portion 2; and a rotating shaft 3, which extends upward along the central axis O1 from the center when viewed from above the disk portion 8. The second reaction liquid L2 can flow inside the disk portion 8 and the rotating shaft 3. In the second liquid supply step, the second reaction liquid L2 is supplied radially outward from the outer edge of the disk portion 8 through the cylindrical portion. According to this crystallization method, the same effect as that of the crystallization apparatus 4 of the first embodiment can be obtained.

[0120] Furthermore, this can be considered a crystallization method, wherein the stirring blade We of the sixth modification of the crystallization apparatus 4 of the first embodiment includes: a cylindrical portion 20; a disk base 18, which is arranged concentrically with the cylindrical portion 20 at the upper end of the cylindrical portion 20; a rotating shaft 3, which extends upward along the central axis O1 from the center when viewed from above the disk base 18; and a cylindrical perforated plate 18P, which is arranged concentrically with the cylindrical portion 20 on the radially outer side of the cylindrical portion 20. The perforated plate 18P extends downward from the outer edge of the disk base 18. The second reaction liquid L2 can flow inside the rotating shaft 3, the disk base 18, and the cylindrical portion 20. In the second liquid supply step, the second reaction liquid L2 is supplied radially outward from a plurality of second liquid supply portions 50b arranged at intervals in the vertical direction on the outer peripheral surface 20o of the cylindrical portion 20. According to this crystallization method, the first reaction liquid and the second reaction liquid can be mixed more uniformly. In addition, the second reaction liquid L2 can be supplied to the inner and outer peripheries of the stirring blade We with the highest shear force, that is, within a very close distance of, for example, 2 mm from the outer peripheral surface 20o of the cylindrical part 20 and the inner and outer peripheries of the porous plate 18P, and the effect of shear force can be applied to more places, thus producing uniform and fine particles.

[0121] Furthermore, this can be considered a crystallization method, wherein the stirring blade Wf ​​of the seventh modification of the crystallization apparatus 4 of the first embodiment includes: a cylindrical portion 20; a rotating shaft 3 extending upward along the central axis O1 from the center of the cylindrical portion 20 when viewed from above; and a cylindrical perforated plate 18P arranged concentrically with the cylindrical portion 20 on the radially outer side of the cylindrical portion 20. The perforated plate 18P is fixed to a connecting rod 11 extending radially outward from the outer peripheral surface 20o of the cylindrical portion 20. The second reaction liquid L2 can flow inside the rotating shaft 3 and the cylindrical portion 20. In the second liquid supply step, the second reaction liquid L2 is supplied radially outward from a plurality of second liquid supply portions 50b arranged at intervals in the vertical direction on the outer peripheral surface 20o of the cylindrical portion 20. According to this crystallization method, the first reaction liquid and the second reaction liquid can be mixed more uniformly. In addition, the second reaction liquid can be supplied to the inner and outer peripheries of the stirring blade Wf ​​with the highest shear force, that is, within a very close distance of, for example, 2 mm from the outer peripheral surface 20o of the cylindrical part 20 and the inner and outer peripheries of the porous plate 18P, and the effect of shear force can be applied to more places, thus producing uniform and fine particles.

[0122] The embodiments and variations of the present invention have been described in detail above with reference to the accompanying drawings. However, the specific structure is not limited to the embodiments and variations, and also includes designs that do not depart from the scope of the present invention, as well as combinations of embodiments and variations.

[0123] For example, in the above embodiment, the first reaction solution L1 and the second reaction solution L2 are mixed to obtain the product, but three or more reaction solutions can also be mixed.

[0124] According to the embodiments of the present invention, a crystallization apparatus, crystallization system and crystallization method can be obtained that can minimize the gap between the stirring blade and the reaction liquid supply nozzle without requiring high manufacturing precision, and can take the extremely close distance, for example within 2 mm, from the inner and outer peripheries of the stirring blade with the highest shear force as the reaction start point.

[0125] Explanation of reference numerals in the attached figures

[0126] 1. Reaction tank 2. Cylindrical section

[0127] 3 rotating shafts 4 crystallization apparatus

[0128] 5a First liquid supply section 5b Second liquid supply section

[0129] 6 outlets, 7 buffer plates (baffles)

[0130] 8. Disc section; 9. h-hole

Claims

1. A crystallization apparatus, characterized in that, include: The stirring blade has multiple holes that extend radially and is capable of rotating about a central axis; A bottomed cylindrical reaction tank can concentrically house the stirring blades inside; A first liquid supply unit is provided in the reaction tank and is capable of supplying a first reaction liquid into the interior of the reaction tank; as well as The second liquid supply unit is disposed on the stirring blades and is capable of supplying a second reaction liquid into the interior of the reaction tank. The stirring blade comprises: a cylindrical portion; a disc-shaped portion, the outer edge of which is fixed to the inner circumferential surface of the cylindrical portion; and a rotating shaft extending upward along the central axis when viewed from above the center of the disc portion. The second reaction liquid can flow inside the disk portion and the rotating shaft, and the second liquid supply portion is provided at the outer edge of the disk portion.

2. The crystallization apparatus according to claim 1, characterized in that, The second liquid supply section opens downwards.

3. The crystallization apparatus according to claim 1, characterized in that, The second liquid supply section opens radially outward and extends through the cylindrical section.

4. The crystallization apparatus according to claim 2 or 3, characterized in that, At a point on the upper side of the cylindrical portion compared to the disc portion, the plurality of radially penetrating holes are blocked, and a disc-shaped second disc portion is provided at the upper end of the cylindrical portion, the outer edge of the second disc portion being fixed to the inner circumferential surface of the cylindrical portion.

5. The crystallization apparatus according to claim 2, characterized in that, The disc portion is located at the upper end of the cylindrical portion.

6. The crystallization apparatus according to any one of claims 1 to 3 and 5, characterized in that, The circumferential speed of the stirring blade is above 5 m / s and below 50 m / s.

7. The crystallization apparatus according to any one of claims 1 to 3 and 5, characterized in that, When the gap between the outer circumferential surface of the cylindrical part and the inner circumferential surface of the reaction tank is set to L3, and the height of the cylindrical part is set to H, H / L3 is 10 or more.

8. The crystallization apparatus according to any one of claims 1 to 3 and 5, characterized in that, The second liquid supply section is configured as multiple.

9. A crystallization apparatus, characterized in that, include: The stirring blade has multiple holes that extend radially and is capable of rotating about a central axis; A bottomed cylindrical reaction tank can concentrically house the stirring blades inside; A first liquid supply unit is provided in the reaction tank and is capable of supplying a first reaction liquid into the interior of the reaction tank; as well as The second liquid supply unit is disposed on the stirring blades and is capable of supplying a second reaction liquid into the interior of the reaction tank. The stirring blade comprises: a cylindrical portion; a disk base concentrically disposed at the upper end of the cylindrical portion; a rotating shaft extending upward along the central axis when viewed from above the center of the disk base; and a cylindrical perforated plate concentrically disposed on the radially outer side of the cylindrical portion, the perforated plate extending downward from the outer edge of the disk base. The second reaction liquid can flow inside the rotating shaft, the disk base, and the cylindrical portion. A plurality of second liquid supply portions are provided on the outer circumferential surface of the cylindrical portion at vertical intervals. When the gap between the outer peripheral surface of the porous plate and the inner peripheral surface of the reaction tank is set to L3, and the height of the stirring blade is set to H, H / L3 is greater than 10.

10. A crystallization apparatus, characterized in that, include: The stirring blade has multiple holes that extend radially and is capable of rotating about a central axis; A bottomed cylindrical reaction tank can concentrically house the stirring blades inside; A first liquid supply unit is provided in the reaction tank and is capable of supplying a first reaction liquid into the interior of the reaction tank; as well as The second liquid supply unit is disposed on the stirring blades and is capable of supplying a second reaction liquid into the interior of the reaction tank. The stirring blade comprises: a cylindrical portion; a rotating shaft extending upward along the central axis when viewed from above; and a cylindrical perforated plate arranged concentrically with the cylindrical portion on its radially outer side. The perforated plate is fixed to a connecting rod extending radially outward from the outer circumference of the cylindrical portion. The second reaction liquid can flow inside the rotating shaft and the cylindrical portion. A plurality of second liquid supply portions are provided on the outer circumferential surface of the cylindrical portion at intervals in the vertical direction. When the gap between the outer peripheral surface of the porous plate and the inner peripheral surface of the reaction tank is set to L3, and the height of the stirring blade is set to H, H / L3 is greater than 10.

11. The crystallization apparatus according to claim 9 or 10, characterized in that, An extension tube is provided that extends radially outward from a plurality of second liquid supply sections.

12. A crystallization system, characterized in that, include: The crystallization apparatus according to any one of claims 1 to 11; A retention tank is used to retain the products transferred from the reaction tank; as well as A circulation pump is used to circulate the product between the retention tank and the crystallization apparatus.

13. A crystallization method, characterized in that, The following steps are included in the crystallization apparatus: In the first liquid supply step, the first reaction liquid is supplied from the first liquid supply unit to the reaction tank; as well as In the second liquid supply step, the second reaction liquid is supplied from the second liquid supply unit. The crystallization apparatus includes: The stirring blade has multiple holes that extend radially and rotates about a central axis; The reaction tank, which is a bottomed cylindrical shape, houses the stirring blades concentrically inside. The first liquid supply unit is disposed in the reaction tank and supplies the first reaction liquid into the interior of the reaction tank; and The second liquid supply unit is disposed on the stirring blade and is capable of supplying the second reaction liquid into the interior of the reaction tank. The stirring blade comprises: a cylindrical portion; a disc-shaped portion, the outer edge of which is fixed to the inner circumferential surface of the cylindrical portion; and a rotating shaft extending upward along the central axis when viewed from above the center of the disc portion. The second reaction liquid can flow inside the disk portion and the rotating shaft, and the second liquid supply portion is provided at the outer edge of the disk portion.

14. The crystallization method according to claim 13, characterized in that, In the second liquid supply step, the second reaction liquid is supplied downward from the outer edge of the disk portion.

15. The crystallization method according to claim 13, characterized in that, In the second liquid supply step, the second reaction liquid is supplied radially outward from the outer edge of the disc portion through the cylindrical portion.

16. A crystallization method, characterized in that, The following steps are included in the crystallization apparatus: In the first liquid supply step, the first reaction liquid is supplied from the first liquid supply unit to the reaction tank; as well as In the second liquid supply step, the second reaction liquid is supplied from the second liquid supply unit. The crystallization apparatus includes: The stirring blade has multiple holes that extend radially and rotates about a central axis; The reaction tank, which is a bottomed cylindrical shape, houses the stirring blades concentrically inside. The first liquid supply unit is disposed in the reaction tank and supplies the first reaction liquid into the interior of the reaction tank; and The second liquid supply unit is disposed on the stirring blade and is capable of supplying the second reaction liquid into the interior of the reaction tank. The stirring blade comprises: a cylindrical portion; a disk base disposed concentrically with the upper end of the cylindrical portion; a rotating shaft extending upward along the central axis when viewed from above the center of the disk base; and a cylindrical perforated plate disposed concentrically with the cylindrical portion on its radially outer side, the perforated plate extending downward from the outer edge of the disk base. The second reaction liquid can flow inside the rotating shaft, the disk base, and the cylindrical portion. In the second liquid supply step, the second reaction liquid is supplied radially outward from a plurality of second liquid supply portions disposed at vertical intervals on the outer circumferential surface of the cylindrical portion. When the gap between the outer peripheral surface of the porous plate and the inner peripheral surface of the reaction tank is set to L3, and the height of the stirring blade is set to H, H / L3 is greater than 10.

17. A crystallization method, characterized in that, The following steps are included in the crystallization apparatus: In the first liquid supply step, the first reaction liquid is supplied from the first liquid supply unit to the reaction tank; as well as In the second liquid supply step, the second reaction liquid is supplied from the second liquid supply unit. The crystallization apparatus includes: The stirring blade has multiple holes that extend radially and rotates about a central axis; The reaction tank, which is a bottomed cylindrical shape, houses the stirring blades concentrically inside. The first liquid supply unit is disposed in the reaction tank and supplies the first reaction liquid into the interior of the reaction tank; and The second liquid supply unit is disposed on the stirring blade and is capable of supplying the second reaction liquid into the interior of the reaction tank. The stirring blade comprises: a cylindrical portion; a rotating shaft extending upward along the central axis when viewed from above; and a cylindrical perforated plate arranged concentrically with the cylindrical portion on its radially outer side. The perforated plate is fixed to a connecting rod extending radially outward from the outer circumference of the cylindrical portion. The second reaction liquid can flow through the rotating shaft and the interior of the cylindrical portion. In the second liquid supply step, the second reaction liquid is supplied radially outward from a plurality of second liquid supply portions arranged at vertical intervals on the outer circumference of the cylindrical portion. When the gap between the outer peripheral surface of the porous plate and the inner peripheral surface of the reaction tank is set to L3, and the height of the stirring blade is set to H, H / L3 is greater than 10.

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