WO2023176146A1 - Crystallization system and crystallization method - Google Patents

Crystallization system and crystallization method Download PDF

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Publication number
WO2023176146A1
WO2023176146A1 PCT/JP2023/001874 JP2023001874W WO2023176146A1 WO 2023176146 A1 WO2023176146 A1 WO 2023176146A1 JP 2023001874 W JP2023001874 W JP 2023001874W WO 2023176146 A1 WO2023176146 A1 WO 2023176146A1
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Prior art keywords
crystallizer
stirring blade
crystallization system
reaction
liquid
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PCT/JP2023/001874
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French (fr)
Japanese (ja)
Inventor
裕也 津崎
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月島機械株式会社
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Publication of WO2023176146A1 publication Critical patent/WO2023176146A1/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/02—Crystallisation from solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/43—Mixing liquids with liquids; Emulsifying using driven stirrers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/40—Mixing liquids with liquids; Emulsifying
    • B01F23/45—Mixing liquids with liquids; Emulsifying using flow mixing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/50—Circulation mixers, e.g. wherein at least part of the mixture is discharged from and reintroduced into a receptacle
    • B01F25/51—Circulation mixers, e.g. wherein at least part of the mixture is discharged from and reintroduced into a receptacle in which the mixture is circulated through a set of tubes, e.g. with gradual introduction of a component into the circulating flow
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
    • B01F27/94—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with rotary cylinders or cones
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons

Definitions

  • the present invention relates to a crystallization system and method. This application claims priority based on Japanese Patent Application No. 2022-040318 filed in Japan on March 15, 2022, the contents of which are incorporated herein.
  • Crystallizers described in Patent Documents 1 to 4 are known as crystallizers that mix multiple raw material solutions and obtain particles derived from the raw materials in the raw material solutions within a certain particle size range. .
  • stirring is promoted by rotating a stirring blade provided in a mixed liquid of a plurality of raw material solutions to apply shear force to the mixed liquid.
  • stirring blades are rotated at high speed in the reaction field, where multiple raw material solutions come into contact with each other and the reaction that generates particles takes place. It is important to efficiently transmit the generated shear force to promote the reaction.
  • attempts have been made to minimize the clearance between the stirring blade, which is a rotor, and the reaction tank, reaction liquid supply nozzle, and the like, which are stators.
  • Non-Patent Document 1 a retention tank is provided, and by retaining the fine particles crystallized in the crystallizer in the retention tank, the crystals can be divided into a certain range. The residence time necessary for growth to particle size is secured.
  • the present invention was developed against this background, and allows fine particles precipitated in a crystallizer to be retained until they grow to a certain particle size range without requiring a retention tank, making it easy to control retention conditions.
  • the purpose of this invention is to provide a crystallization system and method.
  • a first aspect of the present invention includes a crystallizer that mixes a plurality of raw material solutions to generate particles derived from a plurality of raw materials in the plurality of raw material solutions, and a crystallizer that mixes a plurality of raw material solutions to generate particles derived from a plurality of raw materials in the plurality of raw material solutions; a circulation pipe that flows a slurry containing the particles and circulates the slurry from an inlet of the crystallizer into the crystallizer; and a circulation pipe that circulates the slurry between the crystallizer and the circulation pipe.
  • the crystallization system is equipped with a circulation pump that allows the crystallization system to move, and the circulation pipe has a meandering bent portion.
  • the flow rate of the circulation pump can be controlled without the need for complicated flow analysis. This makes it easy to completely and uniformly mix the slurry in the crystallization system.
  • the inner diameter of the circulation pipe is constant.
  • the slurry discharged from the crystallizer flows through the circulation pipe having a constant inner diameter, it is possible to control the flow rate of the circulation pump without requiring complicated flow analysis. , can easily mix the slurry completely homogeneously in the crystallization system.
  • a third aspect of the present invention is the first aspect in which a plurality of the bent portions are provided.
  • the third aspect of the present invention since a plurality of bent portions are provided, even when the volume of slurry is large, crystallization can be easily performed by controlling the flow rate of the circulation pump without requiring complicated flow analysis.
  • the slurry in the analysis system can be thoroughly mixed.
  • a fourth aspect of the present invention is that in the first aspect, at least a portion of the bent portion is provided in the temperature adjustment tank.
  • the slurry in the crystallization system can be easily and completely uniformly mixed by controlling the flow rate of the circulation pump. It is possible to adjust the amount of heat of the slurry.
  • the bent portion is composed of a plurality of separable straight tube portions and a plurality of bent tube portions.
  • the flow path length of the bent portion can be adjusted by changing the number of the plurality of straight pipe portions and the plurality of bent pipe portions, so that complicated flow analysis is possible.
  • the flow path length of the bent portion By adjusting the flow path length of the bent portion, the residence time of the slurry can be adjusted without the need for.
  • the crystallizer includes a stirring blade that is provided with a plurality of holes penetrating in the radial direction and is rotatable around a central axis, and a stirring blade that is arranged concentrically.
  • a cylindrical reaction tank with a bottom that can be accommodated inside the reaction tank; the introduction port that is provided in the reaction tank and is capable of supplying a first reaction liquid into the reaction tank;
  • a liquid supply unit capable of supplying the second reaction liquid into the inside of the reaction tank is provided.
  • the second reaction liquid is supplied from the liquid supply section provided on the stirring blade, which requires high manufacturing costs as in the case where the reaction liquid supply nozzle and the stirring blade are separately provided.
  • the second reaction liquid can be supplied within a short distance, for example within 2 mm, from the inner and outer peripheries of the stirring blade where the shearing force is highest, without requiring precision.
  • the stirring blade is equipped with a plurality of holes penetrating in the radial direction, the mixed liquid of the first reaction liquid and the second reaction liquid passes through the holes toward the outside in the radial direction of the stirring blade due to the influence of centrifugal force.
  • the stirring blade in the fifth aspect, includes a cylindrical cylindrical part, a disc-shaped disc part whose outer edge is fixed to an inner circumferential surface of the cylindrical part, and a rotating shaft extending upwardly along the central axis from the center of the disc part in a plan view, the second reaction liquid can flow through the interior of the disc part and the rotating shaft, and the second reaction liquid can flow inside the disc part and the rotating shaft;
  • the liquid supply section is provided at the outer edge.
  • the second reaction liquid is supplied at a close distance, for example, within 2 mm from the inner and outer periphery of the stirring blade having the highest shearing force. , can be supplied in a range of .
  • the liquid supply section opens downward.
  • the second reaction liquid is supplied at a close distance, for example, within 2 mm, from the inner and outer periphery of the stirring blade where the shear force is highest. Can be supplied to a range.
  • the liquid supply portion opens radially outward and penetrates the cylindrical portion.
  • the second reaction liquid is supplied from the inner and outer periphery of the stirring blade where the shear force is highest. It can be supplied to a close range, for example within 2 mm.
  • a tenth aspect of the present invention includes a crystallization step of mixing a plurality of raw material solutions and growing particles derived from a plurality of raw materials in the plurality of raw material solutions in a crystallizer, and an exhausting of the crystallizer.
  • This crystallization method includes a circulation step of circulating the slurry containing the particles discharged from the outlet to the inlet of the crystallizer by flowing the circulation pipe having a meandering bent portion.
  • the slurry discharged from the crystallizer flows through the circulation pipe, so the residence time of the slurry can be adjusted without the need for complicated flow analysis.
  • FIG. 1 is a schematic diagram of a crystallization system according to a first embodiment of the present invention.
  • FIG. 2 is a schematic diagram of a crystallization system according to a second embodiment of the present invention.
  • FIG. 3 is a schematic diagram of a crystallization system according to a third embodiment of the present invention. It is a schematic diagram of the 1st modification of the crystallization system of 1st Embodiment based on this invention. It is a schematic diagram of the 2nd modification of the crystallization system of 1st Embodiment based on this invention. It is a schematic diagram of the third modification of the crystallization system of the first embodiment according to the present invention.
  • the crystallization system 10A includes a crystallizer 4 that mixes a plurality of raw material solutions to generate particles derived from a plurality of raw materials in the plurality of raw material solutions, and a crystallizer 4 that is provided downstream of the crystallizer 4 and that mixes a plurality of raw material solutions.
  • a circulation pipe Po that circulates the slurry D1 discharged from the discharge port 6 of the crystallizer 4 to the inlet 5a of the crystallizer 4, and a circulation pipe that circulates the slurry D1 between the crystallizer 4 and the circulation pipe Po.
  • a pump 30 is provided.
  • the circulation pipe Po includes a bent portion Pp that is a meandering pipe. Further, the circulation pipe Po includes a pipe 22 that connects the crystallizer 4 and the bent part Pp, a pipe 23 that connects the circulation pump 30 and the bent part Pp, and a pipe 23 that connects the circulation pump 30 and the crystallizer 4. A piping 24 is provided. Note that the bent portion Pp is not limited to a meandering shape, but may have a spiral shape.
  • the circulation pump 30 is a circulation pump that has a function of circulating the slurry D1 between the crystallizer 4 and the bending part Pp in an adjustable flow rate.
  • the device is not necessarily limited to a circulation pump as long as it has a similar function; for example, an impeller whose rotation speed can be controlled may be provided in the piping 23 or the piping 24.
  • the crystallizer 4 includes a cylindrical reaction tank 1 with a bottom and a central axis O1 facing in the vertical direction, and a cylindrical stirring blade Wc.
  • the stirring blade Wc is rotatable around a hollow rotating shaft 3 that extends upward from the center of the stirring blade Wc in plan view along the central axis O1, and rotates around the inside of the reaction tank 1 with the central axis O1 as the same central axis. is housed in.
  • the rotating shaft 3 is rotated by a rotational force supplied via a belt from a prime mover (not shown) provided outside the crystallizer 4 .
  • the prime mover is not particularly limited as long as it is a device that generates rotational power, such as a motor or an engine.
  • the belt for transmitting the rotational force to the rotating shaft 3 is not particularly limited as long as it can transmit rotational force, such as a chain or a gear.
  • the bottom surface of the reaction tank 1 may have a cone shape that is convex downward, instead of being flat as shown in the figure.
  • a discharge port 6 is provided in the upper part of the reaction tank 1 to allow the slurry containing particles (crystals) generated in the reaction tank 1 to be discharged to the next process.
  • a pressure indication controller (PIC) is provided in the pipe 22 to maintain or adjust the pressure of the slurry D1 discharged from the discharge port 6 into the pipe 22.
  • an introduction port 5a is provided to which the first reaction liquid L1 and the slurry D1 flowing through the circulation pipe Po are supplied.
  • the first reaction liquid L1 is generated by supplying and mixing the auxiliary raw materials S A and SB from an unillustrated tank that stores the external auxiliary raw materials S A and SB .
  • the flow rates of the auxiliary raw materials S A and SB of the first reaction liquid L1 are maintained or adjusted by fuel indication controllers (FICs) FIC 2 and FIC 3 .
  • a desired amount of the first reaction liquid L1 is supplied to the reaction tank 1 from the inlet 5a.
  • the amount of the first reaction liquid L1 supplied from the inlet 5a can be adjusted to a desired amount by adjusting the rotation speed of the circulation pump 30, for example.
  • a pressure gauge (PI:Pressure Indicator) PI 1 is provided in the pipe 24 through which the first reaction liquid L1 flows, if necessary. Further, the second reaction liquid L2 is supplied into the reaction tank 1 from the liquid supply part 5b provided on the stirring blade Wc. The second reaction liquid L2 is supplied from an external tank storing the main raw material SM . The flow rate of the second reaction liquid L2 is maintained or adjusted by a fuel indicator controller FIC1 . The first reaction liquid L1 and the second reaction liquid L2 supplied into the reaction tank 1 react to generate crystallized fine particles. Slurry D1 is a fluid containing these fine particles.
  • the bent portion Pp includes a plurality of straight pipe portions (Po1, Po2, Po3, Po4, Po5, Po6) with an inner diameter of r2 , which are arranged at intervals and facing substantially the same direction, and a plurality of adjacent straight pipe portions.
  • a plurality of curved pipe parts C (C 1 , C 2 , C 3 , C 4 , C 5 ) with an inner diameter r 3 that connect parts Po1, Po2 , Po3, Po4 , Po5, and Po6 in a separable or detachable manner.
  • a fixing plate 21 for fixing a plurality of straight pipe sections.
  • the plurality of curved pipe sections C are separable if they are provided so as to connect the straight pipe sections Po5 and Po6, like the curved pipe section C5 indicated by the dotted line in Fig. 1. This means that the curved pipe portion C5 can be separated from the straight pipe portions Po5 and Po6.
  • the flange section (not shown) is attached to both ends of the bent pipe section C5 and the left end of the straight pipe sections Po5 and Po6.
  • the bent pipe portion C5 may be attached to and removed from the straight pipe portion Po5 and the straight pipe portion Po6 by tightening or loosening the flange portion using bolts, nuts, etc.
  • the attachment/detachment method is not limited to this, and as long as it is detachable, for example, it is not limited to the method of using a flange part, and both ends of the curved pipe part C5 can be screwed to the left end parts of the straight pipe part Po5 and the straight pipe part Po6. You can put it on and take it off by letting it go.
  • the fixing plate 21 has a rectangular shape in FIG. 1, the material and shape of the fixing plate 21 can be Not particularly limited. As mentioned above, since the plurality of straight pipe parts and the plurality of curved pipe parts C can be separated, the inner circumferential surfaces of the straight pipe parts and the curved pipe parts C can be easily cleaned by separating them. The maintainability of the crystallization system 10A can be improved.
  • the straight pipe section is composed of six straight pipe sections: straight pipe section Po1, straight pipe section Po2, straight pipe section Po3, straight pipe section Po4, straight pipe section Po5, and straight pipe section Po6.
  • the curved pipe section C is composed of five curved pipe sections: a curved pipe section C 1 , a curved pipe section C 2 , a curved pipe section C 3 , a curved pipe section C 4 , and a curved pipe section C 5 . It is not limited to this example.
  • the straight pipe portion Po may be composed of six or more straight pipe parts Po, or may be composed of six or less straight pipe parts Po.
  • the number of curved pipe parts C also increases or decreases in accordance with the number of straight pipe parts Po. For example, in the example of FIG.
  • the second end of the curved pipe portion C2 whose first end is connected to the right end portion of the straight pipe portion Po3, may be connected to the left end portion of the pipe 22.
  • the curved tube portion C 2 may be provided with a bellows portion that can be expanded and contracted, so that the curved tube portion C 2 can be expanded and contracted.
  • the pipe length of the bent portion Pp that is, the total length of the straight pipe portion and the bent pipe portion C (the number of the straight pipe portion and the bent pipe portion C) is such that the slurry D1 is kept for the desired residence time. It can be adjusted as desired to achieve retention. That is, when a longer residence time is desired, it is desirable to increase the number of straight pipe sections and bent pipe sections C to lengthen the pipe length of the bent section Pp, and when a shorter residence time is desired, It is desirable to reduce the number of straight pipe portions and bent pipe portions C to shorten the pipe length of the bent portion Pp.
  • the flow rate of the slurry D1 is determined by the specific gravity and diameter of the particles that make up the slurry D1. That is, since the settling speed of the particles making up the slurry D1 is determined by the specific gravity and diameter of the particles making up the slurry D1, the flow rate of the slurry D1 is determined so that the slurry D1 flows through the pipe without settling. Therefore, the pipe length of the bent portion Pp can be determined from the desired residence time of the slurry D1 and the flow rate of the slurry D1 to prevent the slurry D1 from settling.
  • the crystallizer 4 and the bent portion Pp are connected by a pipe 22 having an inner diameter r1 .
  • the bent portion Pp and the circulation pump 30 are connected by a pipe 23 having an inner diameter r4 .
  • the circulation pump 30 and the crystallizer 4 are connected by a pipe 24 having an inner diameter r5 .
  • the inner diameter of the circulation pipe Po that is, the inner diameter r 1 of the pipe 22, the inner diameter r 2 of the straight pipe portions Po1, Po2, Po3, Po4, Po5, Po6, the curved pipe portions C 1 , C 2 ,
  • the inner diameter r 3 of C 3 , C 4 , and C 5 , the inner diameter r 4 of the pipe 23, and the inner diameter r 5 of the pipe 24 are the same.
  • the cross-sectional areas of the pipe 22, the straight pipe parts Po1, Po2, Po3, Po4, Po5, Po6, the curved pipe parts C1 , C2 , C3 , C4 , C5 , the pipe 23, and the pipe 24 are constant. Therefore, flow analysis of the slurry D1 flowing through the pipe becomes easy.
  • the example is not limited to the above example, and the inner diameter of the circulation pipe Po, that is, the inner diameter r 1 of the pipe 22, the inner diameter r 2 of the straight pipe portions Po1, Po2, Po3, Po4, Po5, and Po6, the curved pipe portion C 1 , C2 , C3 , C4 , and C5 , the inner diameter r4 of the pipe 23, and the inner diameter r5 of the pipe 24 may be different from each other. In that case, flow analysis may be performed taking different inner diameters into consideration.
  • a pipe line connected to a second circulation pump 31 driven by a motor M is connected to the pipe 23 through which the slurry D1 discharged from the bent portion Pp flows. This pipe line pulls out the slurry D1 from the pipe 23 and accumulates it to form a product.
  • a fuel flow indication controller FIC 4 is provided between the motor M and the second circulation pump 31, and maintains or adjusts the flow rate of the slurry D1 drawn out of the crystallization system 10A.
  • the second circulation pump 31, like the circulation pump 30, is a slurry discharge pump that has a function of circulating the slurry with an adjustable flow rate.
  • the device is not necessarily limited to the slurry discharge pump as long as it has the function of drawing out the slurry D1 from the pipe 23, and for example, an impeller whose rotation speed can be controlled may be provided in the pipe.
  • the pressure of the slurry D1 in the pipe 23 immediately after the slurry D1 is pulled out is monitored by a pressure indicator PI 2 as necessary.
  • the slurry D1 containing particles generated in the crystallizer 4 can be easily and completely uniformly mixed by controlling the flow rate of the circulation pump 30. can do. Furthermore, by adjusting the pipe length of the bent portion Pp, the slurry D1 containing particles generated in the crystallizer 4 can be retained for a desired time without requiring a retention tank. Therefore, the residence time of the slurry D1 at the bent portion Pp can be adjusted without performing complicated flow analysis of the slurry D1, which is required when using a residence tank. Note that a retention tank (not shown) may be added to the crystallization system 10A.
  • the crystallization system 10B differs from the crystallization system 10A of the first embodiment in that a second bent portion Ppa is provided in addition to the bent portion Pp (first bent portion).
  • the second bent portion Ppa has the same configuration as the first bent portion Pp.
  • a pipe 22a extends from the middle of the pipe 22 and branches toward the second bent portion Ppa. Further, the slurry D1 discharged from the second bent portion Ppa passes through the pipe 23a and joins the pipe 23 through which the slurry D1 discharged from the first bent portion Pp flows.
  • a valve V1 and a valve V2 are provided at the inlet of the pipe 22a and the outlet of the pipe 23a.
  • the slurry D1 can flow into both the first bent portion Pp and the second bent portion Ppa.
  • the valves V1 and V2 it is possible to flow the slurry D1 only through the first bent portion Pp, and it is possible to have the same configuration as the crystallization system 10A of the first embodiment.
  • the slurry D1 can be made to flow not only to the first bent portion Pp but also to the second bent portion Ppa depending on the flow rate of the slurry D1.
  • the crystallization system 10C differs from the crystallization system 10A of the first embodiment in that at least a portion of the bent portion Pp is provided in the temperature adjustment tank 13.
  • the temperature adjustment tank 13 is a member that maintains a state in which a refrigerant CW such as cold water flows in one direction inside the temperature adjustment tank 13 by a pump (not shown) or the like.
  • a refrigerant CW such as cold water flows in one direction inside the temperature adjustment tank 13 by a pump (not shown) or the like.
  • the refrigerant collides with the straight pipe portions Po1, Po2, Po3, Po4, Po5, and Po6 of the bent portion Pp.
  • the straight pipe parts Po1, Po2, Po3, Po4, Po5, Po6 are formed between the slurry D1 and the refrigerant CW flowing through the straight pipe parts Po1, Po2, Po3, Po4, Po5, Po6 of the bent part Pp. Heat exchange takes place through the members. Therefore, the slurry D1 can be cooled or heated.
  • the straight pipe portions Po1, Po2, Po3, Po4, Po5, and Po6 are provided approximately perpendicularly to the flow direction of the refrigerant CW, but they are not necessarily provided in the flow direction of the refrigerant CW.
  • the straight pipe portions Po1, Po2, Po3, Po4, Po5, and Po6 do not need to be provided substantially vertically, and may be provided at an angle that is not perpendicular.
  • heat exchange with the refrigerant CW may be performed in the bent pipe portion C of the bent portion Pp, or heat exchange with the refrigerant CW may be performed in both the straight pipe portion and the bent pipe portion C of the bent portion Pp. It's okay.
  • the temperature adjustment ability for slurry D1 can be adjusted. For example, if the heat amount Q1 is transferred to the refrigerant CW by heat exchange from the slurry D1 having the heat amount Q flowing through the straight pipe portion Po1, the heat amount Q2 is transferred from the slurry D1 having the heat amount (Q-Q1) flowing through the straight pipe portion Po2. The refrigerant is transferred to CW by exchange.
  • the heat amount Q3 from the slurry D1 having the heat amount (Q-(Q1+Q2)) flowing through the straight pipe portion Po3 is transferred to the refrigerant CW by heat exchange, the heat amount of the slurry D1 flowing through the straight pipe portion Po4 becomes (Q-(Q1+Q2+Q3) ).
  • the amount of heat of the slurry D1 can be reduced, so that the slurry D1 can be cooled by a desired amount. The same applies when heating the slurry D1.
  • the pipe length of the bent part Pp where heat exchange is performed with the refrigerant CW that is, the pipe length or number of the straight pipe parts Po1, Po2, Po3, Po4, Po5, Po6.
  • slurry D1 can be cooled or heated by a desired amount.
  • a crystallization system 10A1 according to the first modification differs from the crystallizer 4 in that the crystallizer 4a includes a stirring blade W.
  • the stirring blade W includes a cylindrical part 2 and a disc-shaped disc part 8 whose outer edge is fixed to the inner peripheral surface 2i of the cylindrical part 2.
  • the disk portion 8 is provided at a position where the height of the cylindrical portion 2 is approximately half, but is not limited to this example, and may be provided below or above approximately half the height of the cylindrical portion 2. .
  • the rotating shaft 3 is fixed to the center of the disk portion 8 in plan view.
  • the hollow interior of the rotating shaft 3 is defined as a conduit P1.
  • a plurality of conduits P2 extend radially from the center toward the outer edge.
  • the conduit P1 of the rotating shaft 3 and the conduit P2 of the disk portion 8 are in communication.
  • the second reaction liquid L2 is supplied to the rotating shaft 3 of the stirring blade W from a tank (not shown) provided outside the crystallizer 4 and storing the main raw material SM .
  • the second reaction liquid L2 is supplied to the hollow pipe line P1 of the rotating shaft 3 via the rotary joint R, and then to the pipe line P2 of the disc part 8.
  • the tip of the pipe P2 on the outside in the radial direction of the reaction tank 1 is opened downward and serves as a liquid supply section 5b from which the second reaction liquid L2 is discharged. Therefore, the disk portion 8 is provided with a plurality of liquid supply portions 5b at intervals in the circumferential direction of the disk portion. For example, eight liquid supply parts 5b are provided. Although the number of liquid supply parts 5b is not limited, it is desirable to provide them symmetrically with respect to the central axis O1.
  • the distance between the inner circumferential surface 2i of the cylindrical portion 2 of the stirring blade W and the center of the liquid supply portion 5b is 2 mm or less.
  • the distance (clearance) between the outer peripheral surface 2o of the cylindrical part 2 of the stirring blade W and the inner peripheral surface 1i of the reaction tank 1 is L3, and the height along the central axis O1 of the stirring blade W (cylindrical part 2) is H.
  • H/L3, which is the ratio of H to L3, is 10 or more.
  • H/L3 is 25 or more. Therefore, even if a device of a different size from this embodiment is used, a similar device can be manufactured based on this ratio.
  • the stirring blade W rotates at a circumferential speed of 5 m/sec or more and 50 m/sec or less.
  • the H/L3 ratio may differ from the above ratio depending on the purpose. For example, if it is desired to suppress crystal crushing, the ratio may be lowered from the above value.
  • the cylindrical portion 2 of the stirring blade W is provided with a plurality of holes h that penetrate in the radial direction of the cylindrical portion 2.
  • the first reaction liquid L1, the 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 be moved 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. .
  • a plurality of holes 9 may be provided in the disk portion 8 to penetrate in the direction of the central axis O1.
  • the first reaction liquid L1, the second reaction liquid L2, or a mixture thereof can be passed from the inside of the stirring blade W to the outside through the hole 9 in addition to the plurality of holes h, or from the outside of the stirring blade W. Can be moved inward.
  • a desired amount of the first reaction liquid L1 is supplied to the reaction tank 1 from the inlet 5a.
  • the amount of the first reaction liquid L1 supplied may be enough to fill the reaction tank 1 (full liquid state), or the first reaction liquid L1 may be supplied to the center of the reaction tank 1 when the stirring blade W rotates.
  • the first reaction liquid L1 is pressed against the inner peripheral surface 1i of the reaction tank 1 by the centrifugal force generated in the first reaction liquid L1 by performing a circular motion around the axis O1, and the first reaction liquid L1 is pressed against the inner peripheral surface 1i of the reaction tank 1. It may be supplied to such an extent that a liquid film of L1 is formed.
  • the supply of the first reaction liquid L1 may be stopped and then the reaction may be carried out in the reaction tank 1.
  • the reaction in the reaction tank 1 may be continuously carried out while maintaining the first reaction liquid L1 at a flow rate sufficient to reach the above-mentioned full liquid state or liquid film forming state.
  • an opening adjustment valve (not shown) in the discharge port 6 and adjusting the opening of this opening adjustment valve, the reaction tank 1 can be adjusted between a full liquid state and a liquid film state in which a liquid film is formed. You can choose either one.
  • the stirring blade W is rotated and the second reaction liquid L2 is supplied from the liquid supply part 5b to the inner peripheral surface 2i of the cylindrical part 2 of the stirring blade W.
  • the second reaction liquid L2 is supplied into the reaction tank 1.
  • the second reaction liquid L2 discharged from the liquid supply part 5b along the inner circumferential surface 2i of the cylindrical part 2 of the stirring blade W enters the reaction tank 1 filled with the first reaction liquid L1. It comes into contact with the first reaction liquid L1 that is rotating with the rotation of the stirring blade W near the inner circumferential surface 2i of the cylindrical portion 2 of the stirring blade W. In this way, the first reaction liquid L1 and the second reaction liquid L2 come into contact with each other, whereby a reaction occurs and particles are generated.
  • the second reaction liquid L2 is supplied to the first reaction liquid L1 from the liquid supply part 5b of the stirring blade W rotating at a circumferential speed of 5 m/sec to 50 m/sec.
  • the reaction liquid L2 can be uniformly mixed with the first reaction liquid L1.
  • the first reaction liquid L1 that is rotating with the rotation of the stirring blade W is discharged from the liquid supply part 5b of the stirring blade W that is rotating at a circumferential speed of 5 m/sec to 50 m/sec.
  • the centrifugal force generated in the second reaction liquid L2 and the mixed liquid causes the first reaction liquid L1, the second reaction liquid L2, and the mixed liquid (hereinafter sometimes referred to collectively as the mixed liquid) moves radially outward of the cylindrical portion 2 of the stirring blade W, passes through the plurality of holes h provided in the cylindrical portion 2 of the stirring blade W, and collides with the inner circumferential surface 1i of the reaction tank 1, and then 1 in the vertical direction along the inner circumferential surface 1i.
  • the mixed liquid that has mainly moved downward is drawn by the radially outward flow caused by the centrifugal force generated by the rotation of the stirring blade W, and passes through the plurality of holes h provided in the cylindrical part 2 of the stirring blade W again.
  • the particles collide with the inner peripheral surface 1i of the reaction tank 1, and then move in the vertical direction along the inner peripheral surface 1i of the reaction tank 1, thereby generating convection.
  • the mixed liquid passes through the plurality of holes h, the mixed liquid is accelerated radially outward due to the effect of the throttle channel, so the flow velocity of the mixed liquid outward in the radial direction is highest in Further, 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/sec or more and 50 m/sec or less and the inner circumferential surface 1i of the fixed reaction tank 1.
  • a shearing force is applied to the existing mixed liquid in the circumferential direction. The closer the shearing force applied to the mixed liquid is to the inner circumferential surface 2i and outer circumferential surface 2o of the cylindrical portion 2 of the stirring blade W, the greater it is.
  • the shearing force applied to the liquid mixture is a major factor in determining the particle size and uniformity of the resulting particles. In particular, the larger the applied shearing force, the more fine the particles can be obtained.
  • the liquid supply section 5b is provided at the outer edge of the disk section 8. Specifically, as described above, the distance between the inner circumferential surface 2i of the cylindrical portion 2 of the stirring blade W and the center of the liquid supply portion 5b is 2 mm or less. Therefore, the second reaction liquid L2 discharged from the liquid supply part 5b along the inner peripheral surface 2i of the cylindrical portion 2 of the stirring blade W, and the second reaction liquid L2 discharged from the liquid supply portion 5b along the inner peripheral surface 2i of the cylindrical portion 2 of the stirring blade W At the reaction start point where the first reaction liquid L1, which is rotating with the rotation of Maximum shear force is applied. Therefore, the region where the applied shearing force is the largest can be set as the reaction initiation point.
  • the reaction start point can be formed in a region within a close distance, for example, within 2 mm, from the inner circumferential surface 2i and outer circumferential surface 2o of the cylindrical portion 2 of the stirring blade W.
  • the mixed liquid can move from the inner circumferential side to the outer circumferential side of the cylindrical portion 2 through the plurality of holes h described above. Therefore, stirring of the first reaction liquid L1 and the second reaction liquid L2 at the reaction starting point is promoted by the shear force. Therefore, the more uniform mixing of the first reaction liquid L1 and the second reaction liquid L2 is started from the reaction start point, and the mixing and reaction are performed in the reaction field where the reaction occurs along the flow of the mixed liquid. By doing so, it is possible to produce particles with fine and uniform diameters.
  • the reaction initiation point refers to the area where the reaction starts
  • the reaction field refers to the entire area where the reaction occurs. Therefore, the reaction initiation point is included in the reaction field.
  • a baffle (not shown) may be provided on the inner peripheral surface of the reaction tank 1 corresponding to the upper part of the stirring blade W.
  • the baffle has the effect of suppressing the generation of vortices and promoting stirring of the mixed liquid when the reaction tank 1 is full of liquid.
  • the baffle is not an essential component and may not be provided.
  • the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4a is affected.
  • the shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
  • a crystallization system 10A2 according to a second modification of the crystallization system 10A according to the first embodiment will be described with reference to FIG. 5.
  • the crystallizer 4b of the second modification is different from the crystallizer 4a of the first modification in that the stirring blade W is a stirring blade Wa.
  • the stirring blade Wa differs from the stirring blade W in that a liquid supply portion 5b provided at the outer edge of the disk portion 8 penetrates the cylindrical portion 2 and opens radially outward.
  • the second reaction liquid L2 is discharged from the liquid supply part 5b that opens radially outward, so that the second reaction liquid L2, the first reaction liquid L1, and the second reaction are mixed.
  • the mixed liquid with liquid L2 has high dispersibility in the radial direction (horizontal direction).
  • a plurality of holes 9 may be provided in the disk portion 8 to penetrate in the direction of the central axis O1.
  • Such a plurality of holes 9 allows a portion of the mixed liquid to flow between the lower side and the upper side of the stirring blade W through the plurality of holes 9, thereby reducing the dynamic load on the stirring blade W. Although it has the effect of reducing The effectiveness of producing uniform and fine particles is reduced. Therefore, the application of the holes 9 can be selected depending on the desired particle quality and the required power.
  • the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4b is affected.
  • the shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
  • the crystallizer 4c of the third modification differs in that the stirring blade Wa in the second modification is replaced by a stirring blade Wb.
  • the stirring blade Wb has a plurality of holes h penetrating in the radial direction in the cylindrical part 2 above the disk part 8 of the stirring blade Wa (which are closed), and an outer edge part on the inner circumferential surface 2i of the cylindrical part 8.
  • a second disk portion 15 to which is fixed is provided at the upper end of the cylindrical portion 2.
  • the second disc part 15 is a disc-shaped member, and has a hole in the center of the second disc part 15, through which the rotating shaft 3 passes. There are no holes that pass through the second disk portion 15 in the direction of the central axis O1, except for the hole that the rotating shaft 3 passes through. Therefore, the first reaction liquid L1, the second reaction liquid L2, and the mixed liquid thereof do not enter the inside of the second disk portion 15.
  • the plurality of holes h penetrating in the radial direction are not provided in the cylindrical part 2 above the disk part 8, and the outer edge part is fixed to the inner circumferential surface 2i of the cylindrical part 8.
  • a second disk portion 15 is provided at the upper end of the cylindrical portion 2. Therefore, the resistance force of the stirring blade Wb when the stirring blade Wb rotates is reduced, and the stirring blade Wb can be operated with less power than the stirring blade Wa.
  • the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4c is affected.
  • the shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
  • the stirring blade Wc has a plurality of holes h penetrating in the radial direction in the cylindrical portion 2 above the disk portion 8 of the stirring blade W (which are closed), and the cylindrical portion 8
  • a second disk portion 15 whose outer edge portion is fixed to the inner circumferential surface 2i of the cylinder portion 2 is provided at the upper end portion of the cylindrical portion 2.
  • the second disc part 15 is a disc-shaped member, and has a hole in the center of the second disc part 15, through which the rotating shaft 3 passes. There are no holes that pass through the second disk portion 15 in the direction of the central axis O1, except for the hole that the rotating shaft 3 passes through. Therefore, the first reaction liquid L1, the second reaction liquid L2, and the mixed liquid thereof do not enter the inside of the second disk portion 15.
  • the stirring blade Wc In such a stirring blade Wc, the plurality of holes h penetrating in the radial direction are not provided in the cylindrical part 2 above the disk part 8, and the outer edge part is fixed to the inner circumferential surface 2i of the cylindrical part 8. Since the second disk portion 15 is provided at the upper end of the cylindrical portion 2, the resistance force of the stirring blade Wc when the stirring blade Wc rotates is reduced. Therefore, the stirring blade Wc can be operated with less power than the stirring blade W.
  • the crystallization system 10A according to the first embodiment including such a crystallizer 4 shearing that affects particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4
  • the force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be individually adjusted, and the control performance of particle quality can be further improved.
  • a crystallization system 10A4 according to a fourth modification of the crystallization system 10A according to the first embodiment will be described with reference to FIG. 7.
  • the crystallizer 4d of the fourth modification is different from the crystallizer 4a of the first modification in that the stirring blade W is a stirring blade Wd.
  • the stirring blade Wd differs from the stirring blade W in that the disk portion 8 is provided at the upper end of the cylindrical portion 2, as shown in FIG. Further, the height of the cylindrical portion 2 is approximately half the height of the cylindrical portion 2 of the stirring blade W.
  • the same effect as the crystallizer 4 provided with the stirring blade W can also be achieved by using the crystallizer 4d equipped with such a stirring blade Wd.
  • the stirring blade Wd can be made lighter than the stirring blade W.
  • the stirring blade Wd can have a simple structure, the stirring blade Wd can be operated with less power than the stirring blade W, resulting in energy saving of the crystallizer 4 and easier manufacturing of the stirring blade Wd. can be expected.
  • the crystallizer 4d can be downsized.
  • a plurality of holes 9 may be provided in the disk portion 8 to penetrate in the direction of the central axis O1. In that case, the same effects as in the case where the disk portion 8 of the stirring blade Wa is provided with a plurality of holes 9 penetrating in the direction of the central axis O1 can be expected.
  • the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4d is affected.
  • the shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
  • the stirring blade W is a stirring blade We.
  • the stirring blade We includes a cylindrical columnar section 20, a disk base 18 provided concentrically with the columnar section 20 at the upper end of the columnar section 20, and a center of the disk base 18 in a plan view.
  • the rotating shaft 3 extends upward along the central axis O1 from the center, and a cylindrical perforated plate 18P provided concentrically with the cylindrical portion 20 on the outside in the radial direction of the cylindrical portion 20.
  • the porous plate 18P is provided with a plurality of holes 18h that penetrate the porous plate 18P in the radial direction, and the first reaction liquid L1, the second reaction liquid L2, and the mixed liquid flow through the plurality of holes 18h. It is possible.
  • the porous plate 18P extends downward from the outer edge of the disc base 18.
  • the second reaction liquid can flow through the pipes P1, P2, and P3 provided inside the rotating shaft 3, the disc base 18, and the cylindrical part 20, respectively.
  • the pipes P1, P2, and P3 are in communication with each other.
  • the pipe P2 extends radially outward from the lower end of the pipe P1 about the central axis O1.
  • the pipe P3 extends downward from the radially outer end of the pipe P2 along the central axis O1.
  • Pipe line P2 and pipe line P3 are formed inside the cylindrical part 20.
  • a plurality of liquid supply parts 50b are provided on the outer peripheral surface 20o of the columnar part 20 at intervals in the vertical direction.
  • the second reaction liquid L2 is supplied into the reaction tank 1 from the plurality of liquid supply parts 50b provided at intervals in the vertical direction on the outer peripheral surface 20o of the columnar part 20, and the second reaction liquid L2 is supplied into the reaction tank 1. It flows through the plurality of holes 18h of the porous plate 18P while mixing and reacting with the first reaction liquid L1 in the porous plate 18P. Therefore, the first reaction liquid L1 and the second reaction liquid L2 can be mixed more uniformly.
  • the mixed liquid that has passed through the plurality of holes 18h of the porous plate 18P collides with the inner circumference 1i of the reaction tank 1, and then moves in the vertical direction along the inner circumference 1i of the reaction vessel 1.
  • the mixed liquid that has moved downward is drawn by the radially outward flow caused by the centrifugal force generated by the rotation of the stirring blade We, and passes through the plurality of holes 18h of the perforated plate 18P of the stirring blade We again to the reaction tank 1. Convection is generated by colliding with the inner circumferential surface 1i and then moving vertically along the inner circumferential surface 1i of the reaction tank 1.
  • the mixed liquid passes through the plurality of holes 18h, the mixed liquid is accelerated radially outward due to the effect of the throttle channel, so the flow velocity of the mixed liquid outward in the radial direction is reduced near the plurality of holes 18h.
  • a shearing force is applied in the circumferential direction to the liquid mixture existing between the two.
  • the shearing force applied to the mixed liquid is greater as the shearing force is closer 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 perforated plate 18P.
  • the shearing force applied to the liquid mixture is a major factor in determining the particle size and uniformity of the resulting particles.
  • the second reaction liquid L2 supplied from the liquid supply part 50b is at a close distance from the inner and outer circumferences of the stirring blade We having the highest shearing force, that is, the outer circumferential surface 20o of the columnar part 20 and the inner and outer circumferential surfaces of the perforated plate 18P, for example. It can be supplied within a range of 2 mm or less.
  • four liquid supply parts 50b are provided in the vertical direction of the columnar part 20, but the number of liquid supply parts 50b is not limited to the example of FIG. It may be increased or decreased.
  • the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4e is affected.
  • the shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
  • the stirring blade Wf includes a cylindrical columnar section 20, a rotating shaft 3 extending upward from the center of the columnar section 20 in plan view along the central axis O1, and a radial direction of the columnar section 20.
  • the porous plate 18P includes a cylindrical perforated plate 18P provided on the outside concentrically with the columnar part 20.
  • the porous plate 18P is provided with a plurality of holes 18h that penetrate the porous plate 18P in the radial direction, and the first reaction liquid L1, the second reaction liquid L2, and the mixed liquid flow through the plurality of holes 18h. It is possible.
  • the porous plate 18P is fixed to the connecting rod 11 extending radially outward from the outer circumferential surface 2o of the cylindrical portion 20.
  • the second reaction liquid can flow through the pipes P1, P2, and P3 provided inside the rotating shaft 3 and the cylindrical portion 20, respectively.
  • the pipes P1, P2, and P3 are in communication with each other.
  • the pipe P2 extends radially outward from the lower end of the pipe P1 about the central axis O1.
  • the pipe P3 extends downward from the radially outer end of the pipe P2 along the central axis O1.
  • Pipe line P2 and pipe line P3 are formed inside the cylindrical part 20.
  • a plurality of liquid supply parts 50b are provided on the outer peripheral surface 20o of the columnar part 20 at intervals in the vertical direction.
  • the stirring blade Wf rotates, the rotating shaft 3, the cylindrical portion 20, the connecting rod 11, and the perforated plate 18P rotate together.
  • a plurality of connecting rods 11 are provided at equal intervals in the circumferential direction of the cylindrical portion 20 . It is preferable that two or more connecting rods 11 are provided.
  • the connecting rod 11 is provided at a position approximately half the height of the cylindrical portion 20, the connection rod 11 is not limited to this example, and may be provided above or below approximately half the height of the cylindrical portion 20. .
  • the second reaction liquid L2 is supplied into the reaction tank 1 from a plurality of liquid supply parts 50b provided at intervals in the vertical direction on the outer circumferential surface 20o of the columnar part 20, and the second reaction liquid L2 is supplied into the reaction tank 1. It flows through the plurality of holes 18h of the porous plate 18P while mixing and reacting with the first reaction liquid L1 in the porous plate 18P. Therefore, the first reaction liquid L1 and the second reaction liquid L2 can be mixed more uniformly.
  • the mixed liquid that has passed through the plurality of holes 18h of the porous plate 18P collides with the inner circumference 1i of the reaction tank 1, and then moves in the vertical direction along the inner circumference 1i of the reaction vessel 1.
  • the mixed liquid that has moved in the vertical direction is attracted by the flow directed outward in the radial direction due to the centrifugal force generated by the rotation of the stirring blade Wf, and passes through the plurality of holes 18h of the perforated plate 18P of the stirring blade Wf again to the reaction tank 1.
  • the reaction vessel 1 collides with the inner circumferential surface 1i of the reactor 1, and then moves vertically along the inner circumferential surface 1i of the reaction tank 1, thereby generating convection.
  • the mixed liquid passes through the plurality of holes 18h, the mixed liquid is accelerated radially outward due to the effect of the throttle channel, so the flow velocity of the mixed liquid outward in the radial direction is reduced near the plurality of holes 18h.
  • a shearing force is applied in the circumferential direction to the liquid mixture existing between the two.
  • the shearing force applied to the mixed liquid increases as the shearing force approaches the outer circumferential surface 2o of the cylindrical portion 20 of the stirring blade Wf and the inner and outer circumferential surfaces of the perforated plate 18P.
  • the shearing force applied to the liquid mixture is a major factor in determining the particle size and uniformity of the resulting particles. In particular, the greater the applied shearing force, the finer the particle size can be obtained.
  • the stirring blade Wf is used, the influence of shear force can be applied to more parts of the liquid mixture, so that uniform and fine particles can be produced.
  • the second reaction liquid L2 supplied from the liquid supply part 50b is at a close distance from the inner and outer circumferences of the stirring blade Wf having the highest shearing force, that is, the outer circumferential surface 20o of the columnar part 20 and the inner and outer circumferential surfaces of the perforated plate 18P, for example. It can be supplied within a range of 2 mm or less. In the example of FIG. 9, four liquid supply parts 50b are provided in the vertical direction of the columnar part 20, but the number of liquid supply parts 50b is not limited to the example of FIG. It may be increased or decreased.
  • the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4f is affected.
  • the shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
  • a crystallization system 10A7 according to a seventh modification of the crystallization system 10A according to the first embodiment will be described with reference to FIG. 10.
  • the crystallizer 4g of the seventh modification is different from the crystallizer 4e of the fifth modification in that the stirring blade We is a stirring blade Wg.
  • the stirring blade Wg has a wider distance between the outer peripheral surface 20o of the columnar part 2 and the inner peripheral surface of the perforated plate 18P than the stirring blade We of the fifth modification.
  • an extension pipe 12 is provided that extends further radially outward from a liquid supply part 50b that opens radially outward in the stirring blade We, and the tip of the extension pipe 12 is the liquid supply part 50b.
  • a stirring blade Wg the distance between the outer circumferential surface 20o of the columnar part 20 and the inner circumferential surface of the perforated plate 18P can be widened, so that the first The reaction liquid L1, the second reaction liquid L2, and a mixed liquid thereof become easier to flow in. Therefore, circulation of the reaction solution can be promoted, and uniform and fine particles can be produced.
  • the second reaction liquid L2 supplied from the liquid supply part 50b is delivered to the inner and outer periphery of the stirring blade Wg having the highest shearing force, that is, within a close distance, for example, within 2 mm, from the inner and outer periphery of the perforated plate 18P. can be supplied.
  • the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4g is affected.
  • the shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
  • a crystallization system 10A8 according to an eighth modification of the crystallization system 10A according to the first embodiment will be described with reference to FIG. 11.
  • the crystallizer 4h of the eighth modification is different from the crystallizer 4f of the sixth modification in that the stirring blade Wf is a stirring blade Wh.
  • the stirring blade Wh has a wider distance between the outer circumferential surface 20o of the columnar part 20 and the perforated plate 18P than the stirring blade Wf of the eighth modification.
  • an extension tube 12 is provided that extends further radially outward from a liquid supply section 50b that opens radially outward in the stirring blade Wf, and the tip of the extension tube 12 is the liquid supply section 50b.
  • a stirring blade Wh since the distance between the outer circumferential surface 20o of the columnar part 20 and the inner circumferential surface of the perforated plate 18P can be widened, the first The reaction liquid L1, the second reaction liquid L2, and a mixed liquid thereof become easier to flow in. Therefore, circulation of the reaction solution can be promoted, and uniform and fine particles can be produced.
  • the second reaction liquid L2 supplied from the liquid supply part 50b is delivered to the inner and outer periphery of the stirring blade Wg having the highest shearing force, that is, within a close distance, for example, within 2 mm, from the inner and outer periphery of the perforated plate 18P. can be supplied.
  • the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4h is affected.
  • the shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
  • the stirring blade Wc of the crystallizer 4 according to the first embodiment the stirring blade W of the crystallizer 4a according to the first modification, in which the liquid supply part 5b is open downward, Further, in the stirring blade Wd of the crystallizer 4d according to the fourth modification, the first reaction liquid L1 and the second reaction liquid L2 can be mixed more uniformly.
  • the crystallization system 10A of the first embodiment includes a crystallization step in which a plurality of raw material solutions are mixed and particles derived from a plurality of raw materials in the plurality of raw material solutions are grown in the crystallizer 4; a circulation step in which the slurry D1 containing particles discharged from the discharge port 6 of the crystallizer 4 is circulated to the inlet 5a of the crystallizer 4 by flowing the circulation pipe Po having a meandering bent portion Pp; It can be considered as a crystallization method including . According to such a crystallization method, effects similar to those of the crystallizer system 10A of the first embodiment can be obtained.
  • the crystallization system 10A of the first embodiment can be considered as a crystallization method in which the inner diameter of the circulation pipe Po is constant. According to such a crystallization method, effects similar to those of the crystallization system 10A of the first embodiment can be obtained.
  • the crystallization system 10B of the second embodiment can be considered as a crystallization method in which a plurality of bent portions Pp are provided in the crystallization system 10A. According to such a crystallization method, effects similar to those of the crystallization system 10B of the second embodiment can be obtained.
  • the crystallization system 10C of the third embodiment can be considered as a crystallization method in which at least a portion of the bent portion Pp is provided in the temperature control tank in the crystallization system 10A. According to such a crystallization method, effects similar to those of the crystallization system 10C of the third embodiment can be obtained.
  • the crystallization system 10A of the first embodiment can be regarded as a crystallization method in which the bent portion Pp is composed of a plurality of separable straight pipe portions and a plurality of bent pipe portions C. According to such a crystallization method, effects similar to those of the crystallization system 10A of the first embodiment can be obtained.
  • the crystallizer 4a is provided with a plurality of holes h penetrating in the radial direction, and a central A stirring blade W rotating around an axis O1, a cylindrical reaction tank 1 with a bottom that concentrically accommodates the stirring blade W, and an introduction for supplying a first reaction liquid L1 into the reaction tank 1.
  • the first reaction liquid L1 is supplied from the inlet 5a to the reaction tank 1.
  • This can be regarded as a crystallization method comprising a first liquid supply step of supplying the second reaction liquid L2 to the reaction tank 1 from the liquid supply part 5b. According to such a crystallization method, effects similar to those of the crystallization system 10A1 according to the first modification of the crystallization system 10A of the first embodiment can be obtained.
  • the stirring blade W is connected to the cylindrical portion 2 and the inner periphery of the cylindrical portion 2. It further includes a disc-shaped disc part 8 whose outer edge is fixed to a surface, and a rotating shaft 3 extending upward from the center of the disc part 8 in plan view along the central axis O1, and the disc part 8 and the rotating shaft O1
  • the second reaction liquid L2 can flow through the inside of the disk, and the second liquid supply step can be considered as a crystallization method in which the second reaction liquid L2 is supplied downward from the outer edge of the disk part 8. . According to such a crystallization method, effects similar to those of the crystallization system 10A1 according to the first modification of the crystallization system 10A of the first embodiment can be obtained.
  • the crystallization system 10A2 according to the second modification of the crystallization system 10A of the first embodiment has a stirring blade in the crystallization system 10A1 according to the first modification of the crystallization system 10A of the first embodiment.
  • W includes a cylindrical cylindrical part 2, a disc-shaped disc part 8 whose outer edge is fixed to the inner circumferential surface 2i of the cylindrical part 2, and a part W extending upward along the central axis from the center of the disc part 8 in a plan view.
  • the second reaction liquid L2 can flow through the interior of the disc part 8 and the rotating shaft O1, and in the second liquid supply step, the cylindrical part 2 is supplied from the outer edge of the disc part 8.
  • the crystallization system 10A of the first embodiment and the crystallization system 10A3 according to the third modification of the crystallization system 10A of the first embodiment are the first modification of the crystallization system 10A of the first embodiment.
  • the diameter A second disc part 15 is provided at the upper end of the cylindrical part 2, and the plurality of holes h penetrating in the direction are not (closed), and the outer edge part is fixed to the inner circumferential surface of the cylindrical part 2.
  • the crystallization system 10A5 according to the fifth modification of the crystallization system 10A of the first embodiment has a stirring blade in the crystallization system 10A1 according to the first modification of the crystallization system 10A of the first embodiment.
  • W extends upward along the central axis O1 from the center of the circular columnar part 20, the disk base 18 provided at the upper end of the circular column part 20 concentrically with the columnar part 20, and the disk base 18 in plan view. It includes an extending rotating shaft 3 and a cylindrical perforated plate 18P provided concentrically with the cylindrical part 20 on the outside in the radial direction of the cylindrical part 20, and the perforated plate 18P extends downward from the outer edge of the disc base 18.
  • the second reaction liquid L2 can flow through the interior of the rotating shaft O1, the disc base 18, and the cylindrical part 20, and in the second liquid supply step, the second reaction liquid L2 is formed on the outer circumferential surface 20o of the cylindrical part 20 at intervals in the vertical direction.
  • This can be considered as a crystallization method in which the second reaction liquid L2 is supplied radially outward from a plurality of provided liquid supply parts 50b. According to such a crystallization method, effects similar to those of the crystallization system 10A4 according to the fifth modification of the crystallization system 10A of the first embodiment can be obtained.
  • the crystallization system 10A6 according to the sixth modification of the crystallization system 10A of the first embodiment has a stirring blade in the crystallization system 10A1 according to the first modification of the crystallization system 10A of the first embodiment.
  • W is provided concentrically with the columnar section 20 on the radially outer side of the columnar section 20, and the rotating shaft 3 extending upward from the center of the columnar section 20 in plan view along the central axis O1.
  • the perforated plate 18P is fixed to a connecting rod 11 extending radially outward from the outer circumferential surface 20o of the cylindrical part 20, and the perforated plate 18P is fixed to a connecting rod 11 extending radially outward from the outer peripheral surface 20o of the cylindrical part 20.
  • the second reaction liquid L2 can flow, and in the second liquid supply step, the second reaction liquid L2 is distributed radially outward from a plurality of liquid supply parts 50b provided on the outer circumferential surface 20o of the columnar part 20 at intervals in the vertical direction.
  • This can be considered as a crystallization method for supplying the second reaction solution L2. According to such a crystallization method, the same effects as the crystallization system 10A6 according to the sixth modification of the crystallization system 10A of the first embodiment can be obtained.
  • the crystallization system 10A7 according to the seventh modification of the crystallization system 10A of the first embodiment is the crystallization system 10A5 according to the fifth modification of the crystallization system 10A of the first embodiment, or the first In a crystallization system 10A6 according to a sixth modification of the crystallization system 10A of the embodiment, extension pipes 12 extending radially outward from the plurality of liquid supply parts 50b are provided, and in the second liquid supply step, the extension pipes 12 are This can be considered as a crystallization method in which the second reaction liquid L2 is supplied from the tip of the tube 12. According to such a crystallization method, effects similar to those of the crystallization system 10A7 according to the seventh modification of the crystallization system 10A of the first embodiment and the crystallization system 10A8 according to the eighth modification can be obtained. I can do it.
  • the product was obtained by mixing two types of reaction liquids, the first reaction liquid L1 and the second reaction liquid L2, but three or more types of reaction liquids may be mixed. .
  • fine particles crystallized in a crystallizer can be retained without requiring a retention tank.

Abstract

A crystallization system (10A) comprises: a crystallizer (4) that mixes a plurality of raw material solutions to produce particles derived from a plurality of raw materials in the plurality of raw material solutions; a circulation pipeline (Po) for causing slurry (D1) containing the particles discharged from an outlet (6) of the crystallizer (4) to flow and circulating the slurry (D1) from an inlet (5a) of the crystallizer (4) into the crystallizer (4); and a circulation pump (30) that circulates the slurry (D1) between the crystallizer (4) and the circulation pipeline (Po). The circulation pipeline (Po) has a bend (Pp) that forms a meandering shape.

Description

晶析システムおよび晶析方法Crystallization system and method
　本発明は、晶析システムおよび晶析方法に関する。
　本願は、２０２２年３月１５日に、日本に出願された特願２０２２－０４０３１８号に基づき優先権を主張し、その内容をここに援用する。 The present invention relates to a crystallization system and method.
This application claims priority based on Japanese Patent Application No. 2022-040318 filed in Japan on March 15, 2022, the contents of which are incorporated herein.
　複数の原料溶液を混合し、原料溶液中の原料に由来する粒子を一定の粒径範囲内で得る晶析装置として、特許文献１から特許文献４に記載される晶析装置が知られている。 Crystallizers described in Patent Documents 1 to 4 are known as crystallizers that mix multiple raw material solutions and obtain particles derived from the raw materials in the raw material solutions within a certain particle size range. .
　上記のような晶析装置においては、複数の原料溶液の混合液中に設けられた撹拌翼を回転させて、混合液に剪断力を与えることで撹拌を促進させている。より粒子径が均一で高品質な微粒子を生成するためには、複数の原料溶液が互いに接触して粒子が生成する反応が行われる場である反応場に、撹拌翼を高速で回転して発生させた剪断力を効率的に伝達して反応を促進することが重要である。効率的な剪断力の伝達を達成するために、回転子である撹拌翼と、固定子である反応槽や反応液供給ノズルなどとのクリアランスを最小化する試みがなされている。
　上記のような晶析装置においては、非特許文献１に記載されるように、滞留槽が設けられ、晶析装置で結晶化された微粒子を滞留槽で滞留させることで、結晶を一定範囲の粒径までに成長させるのに必要な滞留時間を確保している。 In the crystallizer as described above, stirring is promoted by rotating a stirring blade provided in a mixed liquid of a plurality of raw material solutions to apply shear force to the mixed liquid. In order to generate high-quality fine particles with more uniform particle sizes, stirring blades are rotated at high speed in the reaction field, where multiple raw material solutions come into contact with each other and the reaction that generates particles takes place. It is important to efficiently transmit the generated shear force to promote the reaction. In order to achieve efficient transmission of shear force, attempts have been made to minimize the clearance between the stirring blade, which is a rotor, and the reaction tank, reaction liquid supply nozzle, and the like, which are stators.
In the above-mentioned crystallizer, as described in Non-Patent Document 1, a retention tank is provided, and by retaining the fine particles crystallized in the crystallizer in the retention tank, the crystals can be divided into a certain range. The residence time necessary for growth to particle size is secured.
　しかしながら、滞留槽を用いる場合、滞留槽の液レベルを調節することで、滞留槽での滞留時間を調整する必要があるが、滞留槽の液レベルを調節すると滞留槽内の流動状態が変化するため、複雑な流動解析が必要となり、粒径のコントロールが難しく、晶析装置が高価となる要因となる。 However, when using a retention tank, it is necessary to adjust the residence time in the retention tank by adjusting the liquid level in the retention tank, but adjusting the liquid level in the retention tank changes the flow state in the retention tank. Therefore, complicated flow analysis is required, particle size is difficult to control, and crystallization equipment becomes expensive.
日本国特開２０１０－１３７１８３号公報Japanese Patent Application Publication No. 2010-137183 日本国特開２０１０－０２２８９４号公報Japanese Patent Application Publication No. 2010-022894 日本国特許第３２５６８０１号公報Japanese Patent No. 3256801 日本国特開２０１６－８７５９０号公報Japanese Patent Application Publication No. 2016-87590
　本発明は、このような背景の下になされ、滞留槽を必須とせずに、晶析装置で析出した微粒子を一定の粒径範囲に成長するまで滞留させることができ、滞留条件のコントールが容易な晶析システムおよび晶析方法を提供することを目的とする。 The present invention was developed against this background, and allows fine particles precipitated in a crystallizer to be retained until they grow to a certain particle size range without requiring a retention tank, making it easy to control retention conditions. The purpose of this invention is to provide a crystallization system and method.
　本発明の第１の態様は、複数の原料溶液を混合して前記複数の原料溶液の中の複数の原料に由来する粒子を生成させる晶析装置と、前記晶析装置の排出口から排出される前記粒子を含むスラリを流動させ前記晶析装置の導入口から前記晶析装置内に前記スラリを循環させる循環管路と、前記スラリを前記晶析装置と前記循環管路との間で循環させる循環ポンプとを備え、前記循環管路は、蛇行形状をなす屈曲部を有する晶析システムである。 A first aspect of the present invention includes a crystallizer that mixes a plurality of raw material solutions to generate particles derived from a plurality of raw materials in the plurality of raw material solutions, and a crystallizer that mixes a plurality of raw material solutions to generate particles derived from a plurality of raw materials in the plurality of raw material solutions; a circulation pipe that flows a slurry containing the particles and circulates the slurry from an inlet of the crystallizer into the crystallizer; and a circulation pipe that circulates the slurry between the crystallizer and the circulation pipe. The crystallization system is equipped with a circulation pump that allows the crystallization system to move, and the circulation pipe has a meandering bent portion.
　本発明の第１の態様によれば、晶析装置から排出されるスラリが循環管路を流量に応じた流速で流動するため、複雑な流動解析を必要とせずに、前記循環ポンプの流量制御により、容易に晶析システム内のスラリを完全均一混合することができる。 According to the first aspect of the present invention, since the slurry discharged from the crystallizer flows through the circulation pipe at a flow rate depending on the flow rate, the flow rate of the circulation pump can be controlled without the need for complicated flow analysis. This makes it easy to completely and uniformly mix the slurry in the crystallization system.
　本発明の第２の態様は、第１に態様において、前記循環管路の内径が一定である。 In a second aspect of the present invention, in the first aspect, the inner diameter of the circulation pipe is constant.
　本発明の第２の態様によれば、晶析装置から排出されるスラリが、内径が一定の循環管路を流動するため、複雑な流動解析を必要とせずに、前記循環ポンプの流量制御により、容易に晶析システム内のスラリを完全均一混合することができる。 According to the second aspect of the present invention, since the slurry discharged from the crystallizer flows through the circulation pipe having a constant inner diameter, it is possible to control the flow rate of the circulation pump without requiring complicated flow analysis. , can easily mix the slurry completely homogeneously in the crystallization system.
　本発明の第３の態様は、第１の態様において、前記屈曲部が複数設けられている。 A third aspect of the present invention is the first aspect in which a plurality of the bent portions are provided.
　本発明の第３の態様によれば、屈曲部が複数設けられているため、スラリの容量が多い場合でも、複雑な流動解析を必要とせずに、前記循環ポンプの流量制御により、容易に晶析システム内のスラリを完全均一混合することができる。 According to the third aspect of the present invention, since a plurality of bent portions are provided, even when the volume of slurry is large, crystallization can be easily performed by controlling the flow rate of the circulation pump without requiring complicated flow analysis. The slurry in the analysis system can be thoroughly mixed.
　本発明の第４の態様は、第１の態様において、前記屈曲部の少なくとも一部が温度調節槽の中に設けられている。 A fourth aspect of the present invention is that in the first aspect, at least a portion of the bent portion is provided in the temperature adjustment tank.
　本発明の第４の態様によれば、屈曲部の少なくとも一部が温度調節槽の中に設けられているため、前記循環ポンプの流量制御により、容易に晶析システム内のスラリを完全均一混合することができるとともにスラリの熱量を調整することができる。 According to the fourth aspect of the present invention, since at least a portion of the bent portion is provided in the temperature control tank, the slurry in the crystallization system can be easily and completely uniformly mixed by controlling the flow rate of the circulation pump. It is possible to adjust the amount of heat of the slurry.
　本発明の第５の態様は、第１の態様において、前記屈曲部が、分離可能な、複数の直管部と複数の曲管部と、から構成されている。 In a fifth aspect of the present invention, in the first aspect, the bent portion is composed of a plurality of separable straight tube portions and a plurality of bent tube portions.
　本発明の第５の態様によれば、前記複数の直管部と前記複数の曲管部の本数を変えることで、前記屈曲部の流路長を調節することができるので、複雑な流動解析を必要とせずに、前記屈曲部の流路長の調節により、スラリの滞留時間を調整することができる。 According to the fifth aspect of the present invention, the flow path length of the bent portion can be adjusted by changing the number of the plurality of straight pipe portions and the plurality of bent pipe portions, so that complicated flow analysis is possible. By adjusting the flow path length of the bent portion, the residence time of the slurry can be adjusted without the need for.
　本発明の第６の態様は、第１の態様において、前記晶析装置は、径方向に貫通する複数の孔を備えるとともに中心軸の回りに回転可能な撹拌翼と、前記撹拌翼を同心状に内部に収容可能な有底円筒状の反応槽と、前記反応槽に設けられるとともに前記反応槽の内部に第１の反応液を供給可能な前記導入口と、前記撹拌翼に設けられるとともに前記反応槽の内部に第２の反応液を供給可能な給液部と、を備える。 In a sixth aspect of the present invention, in the first aspect, the crystallizer includes a stirring blade that is provided with a plurality of holes penetrating in the radial direction and is rotatable around a central axis, and a stirring blade that is arranged concentrically. a cylindrical reaction tank with a bottom that can be accommodated inside the reaction tank; the introduction port that is provided in the reaction tank and is capable of supplying a first reaction liquid into the reaction tank; A liquid supply unit capable of supplying the second reaction liquid into the inside of the reaction tank is provided.
　本発明の第６の態様によれば、第２の反応液が、撹拌翼に設けられる給液部から供給されるため、反応液供給ノズルと撹拌翼とが別に設けられる場合のような高い製作精度を必要とせず、第２の反応液を剪断力が最も高い撹拌翼の内外周から至近距離、例えば２ｍｍ以内、の範囲に供給することができる。さらに、撹拌翼が径方向に貫通する複数の孔を備えるため、遠心力の影響により第１の反応液と第２の反応液との混合液が撹拌翼の径方向外側に向かって孔を通過して撹拌翼の外周側に移動しながら反応するため、剪断力が最も高い撹拌翼の内外周から至近距離、例えば２ｍｍ以内、の範囲での混合液の撹拌をさらに促進させることができる。 According to the sixth aspect of the present invention, the second reaction liquid is supplied from the liquid supply section provided on the stirring blade, which requires high manufacturing costs as in the case where the reaction liquid supply nozzle and the stirring blade are separately provided. The second reaction liquid can be supplied within a short distance, for example within 2 mm, from the inner and outer peripheries of the stirring blade where the shearing force is highest, without requiring precision. Furthermore, since the stirring blade is equipped with a plurality of holes penetrating in the radial direction, the mixed liquid of the first reaction liquid and the second reaction liquid passes through the holes toward the outside in the radial direction of the stirring blade due to the influence of centrifugal force. Since the reaction occurs while moving toward the outer periphery of the stirring blade, it is possible to further promote stirring of the liquid mixture within a close distance, for example, within 2 mm, from the inner and outer peripheries of the stirring blade where shearing force is highest.
　本発明の第７の態様は、第５の態様において、前記撹拌翼は、円筒状の円筒部と、前記円筒部の内周面に外縁部が固定される円盤状の円盤部と、前記円盤部の平面視の中心から前記中心軸に沿って上方に延びる回転軸と、を備え、前記円盤部と前記回転軸との内部を前記第２の反応液が流通可能であり、前記円盤部の前記外縁部に前記給液部が設けられている。 In a seventh aspect of the present invention, in the fifth aspect, the stirring blade includes a cylindrical cylindrical part, a disc-shaped disc part whose outer edge is fixed to an inner circumferential surface of the cylindrical part, and a rotating shaft extending upwardly along the central axis from the center of the disc part in a plan view, the second reaction liquid can flow through the interior of the disc part and the rotating shaft, and the second reaction liquid can flow inside the disc part and the rotating shaft; The liquid supply section is provided at the outer edge.
　本発明の第７の態様によれば、円盤部の外縁部に給液部が設けられているため、第２の反応液を剪断力が最も高い撹拌翼の内外周から至近距離、例えば２ｍｍ以内、の範囲に供給することができる。 According to the seventh aspect of the present invention, since the liquid supply part is provided at the outer edge of the disc part, the second reaction liquid is supplied at a close distance, for example, within 2 mm from the inner and outer periphery of the stirring blade having the highest shearing force. , can be supplied in a range of .
　本発明の第８の態様は、第６の態様において、前記給液部は下方に向けて開口している。 In an eighth aspect of the present invention, in the sixth aspect, the liquid supply section opens downward.
　本発明の第８の態様によれば、給液部は下方に向けて開口しているため、第２の反応液を剪断力が最も高い撹拌翼の内外周から至近距離、例えば２ｍｍ以内、の範囲に供給することができる。 According to the eighth aspect of the present invention, since the liquid supply part opens downward, the second reaction liquid is supplied at a close distance, for example, within 2 mm, from the inner and outer periphery of the stirring blade where the shear force is highest. Can be supplied to a range.
　本発明の第９の態様は、第６の態様において、前記給液部は径方向外側に向けて開口し前記円筒部を貫通している。 In a ninth aspect of the present invention, in the sixth aspect, the liquid supply portion opens radially outward and penetrates the cylindrical portion.
　本発明の第９の態様によれば、給液部は径方向外側に向けて開口し前記円筒部を貫通しているため、第２の反応液を剪断力が最も高い撹拌翼の内外周から至近距離、例えば２ｍｍ以内、の範囲に供給することができる。 According to the ninth aspect of the present invention, since the liquid supply part opens radially outward and penetrates the cylindrical part, the second reaction liquid is supplied from the inner and outer periphery of the stirring blade where the shear force is highest. It can be supplied to a close range, for example within 2 mm.
　本発明の第１０の態様は、複数の原料溶液を混合して前記複数の原料溶液の中の複数の原料に由来する粒子を晶析装置で成長させる晶析ステップと、前記晶析装置の排出口から排出される前記粒子を含むスラリを、蛇行形状をなす屈曲部を有する循環管路を流動させることで前記晶析装置の導入口まで循環させる循環ステップと、を含む晶析方法である。 A tenth aspect of the present invention includes a crystallization step of mixing a plurality of raw material solutions and growing particles derived from a plurality of raw materials in the plurality of raw material solutions in a crystallizer, and an exhausting of the crystallizer. This crystallization method includes a circulation step of circulating the slurry containing the particles discharged from the outlet to the inlet of the crystallizer by flowing the circulation pipe having a meandering bent portion.
　本発明の第１０の態様によれば、晶析装置から排出されるスラリが循環管路を流動するため、複雑な流動解析を必要とせずに、スラリの滞留時間を調整することができる。 According to the tenth aspect of the present invention, the slurry discharged from the crystallizer flows through the circulation pipe, so the residence time of the slurry can be adjusted without the need for complicated flow analysis.
　本発明によれば、滞留槽を必須とせずに、晶析装置で結晶化された微粒子を滞留させることができる晶析システムおよび晶析方法を得ることができる。 According to the present invention, it is possible to obtain a crystallization system and a crystallization method that can retain fine particles crystallized in a crystallizer without requiring a retention tank.
本発明に係る第１実施形態の晶析システムの概略図である。1 is a schematic diagram of a crystallization system according to a first embodiment of the present invention. 本発明に係る第２実施形態の晶析システムの概略図である。FIG. 2 is a schematic diagram of a crystallization system according to a second embodiment of the present invention. 本発明に係る第３実施形態の晶析システムの概略図である。FIG. 3 is a schematic diagram of a crystallization system according to a third embodiment of the present invention. 本発明に係る第１実施形態の晶析システムの第１の変形例の概略図である。It is a schematic diagram of the 1st modification of the crystallization system of 1st Embodiment based on this invention. 本発明に係る第１実施形態の晶析システムの第２の変形例の概略図である。It is a schematic diagram of the 2nd modification of the crystallization system of 1st Embodiment based on this invention. 本発明に係る第１実施形態の晶析システムの第３の変形例の概略図である。It is a schematic diagram of the third modification of the crystallization system of the first embodiment according to the present invention. 本発明に係る第１実施形態の晶析システムの第４の変形例の概略図である。It is a schematic diagram of the 4th modification of the crystallization system of 1st Embodiment based on this invention. 本発明に係る第１実施形態の晶析システムの第５の変形例の概略図である。It is a schematic diagram of the 5th modification of the crystallization system of 1st Embodiment based on this invention. 本発明に係る第１実施形態の晶析システムの第６の変形例の概略図である。It is a schematic diagram of the 6th modification of the crystallization system of 1st Embodiment based on this invention. 本発明に係る第１実施形態の晶析システムの第７の変形例の概略図である。It is a schematic diagram of the 7th modification of the crystallization system of 1st Embodiment based on this invention. 本発明に係る第１実施形態の晶析システムの第８の変形例の概略図である。It is a schematic diagram of the 8th modification of the crystallization system of 1st Embodiment based on this invention.
＜第１実施形態＞
　以下、第１実施形態に係る晶析システム１０Ａを、図１を参照しながら説明する。
　晶析システム１０Ａは、複数の原料溶液を混合して、これら複数の原料溶液の中の複数の原料に由来する粒子を生成させる晶析装置４と、晶析装置４の下流に設けられ、晶析装置４の排出口６から排出されるスラリＤ１を晶析装置４の導入口５ａまで循環させる循環管路Ｐｏと、スラリＤ１を晶析装置４と循環管路Ｐｏとの間で循環させる循環ポンプ３０と、を備える。 <First embodiment>
Hereinafter, a crystallization system 10A according to a first embodiment will be described with reference to FIG. 1.
The crystallization system 10A includes a crystallizer 4 that mixes a plurality of raw material solutions to generate particles derived from a plurality of raw materials in the plurality of raw material solutions, and a crystallizer 4 that is provided downstream of the crystallizer 4 and that mixes a plurality of raw material solutions. A circulation pipe Po that circulates the slurry D1 discharged from the discharge port 6 of the crystallizer 4 to the inlet 5a of the crystallizer 4, and a circulation pipe that circulates the slurry D1 between the crystallizer 4 and the circulation pipe Po. A pump 30 is provided.
　循環管路Ｐｏは、蛇行形状の管路である屈曲部Ｐｐを備えている。さらに、循環管路Ｐｏは、晶析装置４と屈曲部Ｐｐとを接続する配管２２と、循環ポンプ３０と屈曲部Ｐｐとを接続する配管２３と、循環ポンプ３０と晶析装置４とを接続する配管２４と、を備えている。なお、屈曲部Ｐｐは、蛇行形状に限定されず、螺旋形状をなしていても良い。 The circulation pipe Po includes a bent portion Pp that is a meandering pipe. Further, the circulation pipe Po includes a pipe 22 that connects the crystallizer 4 and the bent part Pp, a pipe 23 that connects the circulation pump 30 and the bent part Pp, and a pipe 23 that connects the circulation pump 30 and the crystallizer 4. A piping 24 is provided. Note that the bent portion Pp is not limited to a meandering shape, but may have a spiral shape.
　循環ポンプ３０は、スラリＤ１を、晶析装置４と屈曲部Ｐｐとの間で流量を調整可能に循環させる機能を有する循環ポンプである。しかしながら、同様の機能を有する装置であれば必ずしも循環ポンプに限定されず、例えば、回転数を制御可能な羽根車が配管２３或いは配管２４に設けられていても良い。 The circulation pump 30 is a circulation pump that has a function of circulating the slurry D1 between the crystallizer 4 and the bending part Pp in an adjustable flow rate. However, the device is not necessarily limited to a circulation pump as long as it has a similar function; for example, an impeller whose rotation speed can be controlled may be provided in the piping 23 or the piping 24.
　晶析装置４は、鉛直方向を向いた中心軸Ｏ１を備える有底円筒状の反応槽１と、円筒状の撹拌翼Ｗｃと、を備える。撹拌翼Ｗｃは、撹拌翼Ｗｃの平面視の中心から中心軸Ｏ１に沿って上方に延びる中空の回転軸３を中心に回転可能であり、中心軸Ｏ１を同一の中心軸として反応槽１の内部に収容されている。回転軸３は、晶析装置４の外部に設けられる不図示の原動機からベルトを介して供給される回転力により回転する。なお、原動機はモータやエンジンなど回転動力を発生させる装置であれば特に限定されない。また、回転力を回転軸３に伝達するベルトはチェーンや歯車など回転力を伝達できれば特に限定されない。なお、反応槽１の底面は、図示されるような平面状である他に、下方に対して凸となるコーン形状であっても良い。反応槽１の上部には反応槽１で生成された粒子（結晶）を含むスラリを次工程に排出可能な排出口６が設けられている。排出口６から配管２２に排出されたスラリＤ１の圧力を維持又は調節する圧力指示調整計（PIC：Pressure Indication Controller）が配管２２に設けられている。 The crystallizer 4 includes a cylindrical reaction tank 1 with a bottom and a central axis O1 facing in the vertical direction, and a cylindrical stirring blade Wc. The stirring blade Wc is rotatable around a hollow rotating shaft 3 that extends upward from the center of the stirring blade Wc in plan view along the central axis O1, and rotates around the inside of the reaction tank 1 with the central axis O1 as the same central axis. is housed in. The rotating shaft 3 is rotated by a rotational force supplied via a belt from a prime mover (not shown) provided outside the crystallizer 4 . Note that the prime mover is not particularly limited as long as it is a device that generates rotational power, such as a motor or an engine. Further, the belt for transmitting the rotational force to the rotating shaft 3 is not particularly limited as long as it can transmit rotational force, such as a chain or a gear. The bottom surface of the reaction tank 1 may have a cone shape that is convex downward, instead of being flat as shown in the figure. A discharge port 6 is provided in the upper part of the reaction tank 1 to allow the slurry containing particles (crystals) generated in the reaction tank 1 to be discharged to the next process. A pressure indication controller (PIC) is provided in the pipe 22 to maintain or adjust the pressure of the slurry D1 discharged from the discharge port 6 into the pipe 22.
　反応槽１の下部には第１の反応液Ｌ１と循環管路Ｐｏを流動したスラリＤ１が供給される導入口５ａが設けられている。第１の反応液Ｌ１は、外部の副原料ＳＡやＳＢを貯蔵する不図示のタンクから副原料ＳＡやＳＢが供給され混合されることで生成される。第１の反応液Ｌ１の副原料ＳＡやＳＢの流量は、燃料指示調節計（FIC：Flow Indication Controller）ＦＩＣ２、ＦＩＣ３で維持又は調節される。第１の反応液Ｌ１は、導入口５ａから反応槽１に所望の量だけ供給される。第１の反応液Ｌ１の導入口５ａからの供給量は、例えば循環ポンプ３０の回転数を調節することで所望の量に調整することができる。第１の反応液Ｌ１が流れる配管２４には必要に応じて圧力計（PI:Pressure Indicator）ＰＩ１が設けられる。
　また、撹拌翼Ｗｃに設けられる給液部５ｂから第２の反応液Ｌ２が反応槽１の中に供給される。第２の反応液Ｌ２は、外部の主原料ＳＭを貯蔵するタンクから供給される。第２の反応液Ｌ２の流量は、燃料指示調節計ＦＩＣ１で維持又は調節される。
　反応槽１の中に供給された第１の反応液Ｌ１と第２の反応液Ｌ２とが反応することで、結晶化された微粒子が生成される。スラリＤ１は、この微粒子を含んだ流体である。 At the lower part of the reaction tank 1, an introduction port 5a is provided to which the first reaction liquid L1 and the slurry D1 flowing through the circulation pipe Po are supplied. The first reaction liquid L1 is generated by supplying and mixing the auxiliary raw materials S A and SB from an unillustrated tank that stores the external auxiliary raw materials S A and SB . The flow rates of the auxiliary raw materials S A and SB of the first reaction liquid L1 are maintained or adjusted by fuel indication controllers (FICs) FIC 2 and FIC 3 . A desired amount of the first reaction liquid L1 is supplied to the reaction tank 1 from the inlet 5a. The amount of the first reaction liquid L1 supplied from the inlet 5a can be adjusted to a desired amount by adjusting the rotation speed of the circulation pump 30, for example. A pressure gauge (PI:Pressure Indicator) PI 1 is provided in the pipe 24 through which the first reaction liquid L1 flows, if necessary.
Further, the second reaction liquid L2 is supplied into the reaction tank 1 from the liquid supply part 5b provided on the stirring blade Wc. The second reaction liquid L2 is supplied from an external tank storing the main raw material SM . The flow rate of the second reaction liquid L2 is maintained or adjusted by a fuel indicator controller FIC1 .
The first reaction liquid L1 and the second reaction liquid L2 supplied into the reaction tank 1 react to generate crystallized fine particles. Slurry D1 is a fluid containing these fine particles.
　屈曲部Ｐｐは、互いに間隔を空けて略同じ方向を向くように配置された内径ｒ２の複数の直管部（Ｐｏ１、Ｐｏ２、Ｐｏ３、Ｐｏ４、Ｐｏ５、Ｐｏ６）と、隣接する複数の直管部Ｐｏ１、Ｐｏ２、Ｐｏ３、Ｐｏ４、Ｐｏ５、Ｐｏ６同士を分離可能、或いは着脱可能に連結する内径ｒ３の複数の曲管部Ｃ（Ｃ１、Ｃ２、Ｃ３、Ｃ４、Ｃ５）と、複数の直管部を固定する固定板２１と、から構成されている。複数の曲管部Ｃが分離可能であるとは、図１に点線で表示された曲管部Ｃ５のように、直管部Ｐｏ５及び直管部Ｐｏ６とを接続するように設けられていた曲管部Ｃ５を、直管部Ｐｏ５及び直管部Ｐｏ６とから分離させることができることを意味する。
　曲管部Ｃ５と、直管部Ｐｏ５及び直管部Ｐｏ６との着脱方法としては、不図示のフランジ部が曲管部Ｃ５の両端部と、直管部Ｐｏ５及び直管部Ｐｏ６の左端部に設けられており、ボルトやナット等を用いてフランジ部を締め付けたり緩めたりすることで、直管部Ｐｏ５及び直管部Ｐｏ６に対して、曲管部Ｃ５を着脱しても良い。着脱方法はこれに限定されず、着脱自在であれば、例えば、フランジ部を使用する方法に限らず、直管部Ｐｏ５及び直管部Ｐｏ６の左端部に曲管部Ｃ５の両端を螺合させることで着脱しても良い。
　固定板２１は、図１では矩形状となっているが、複数の直管部Ｐｏ１、Ｐｏ２、Ｐｏ３、Ｐｏ４、Ｐｏ５、Ｐｏ６が固定板２１に固定された状態で保持できれば、その素材や形状は特に限定されない。
　上記のように、分離可能な、複数の直管部と複数の曲管部Ｃにおいては、分離させることで容易に直管部及び曲管部Ｃの内周面を清掃することができるので、晶析システム１０Ａのメンテナンス性を向上させることができる。 The bent portion Pp includes a plurality of straight pipe portions (Po1, Po2, Po3, Po4, Po5, Po6) with an inner diameter of r2 , which are arranged at intervals and facing substantially the same direction, and a plurality of adjacent straight pipe portions. A plurality of curved pipe parts C (C 1 , C 2 , C 3 , C 4 , C 5 ) with an inner diameter r 3 that connect parts Po1, Po2 , Po3, Po4 , Po5, and Po6 in a separable or detachable manner. , and a fixing plate 21 for fixing a plurality of straight pipe sections. The plurality of curved pipe sections C are separable if they are provided so as to connect the straight pipe sections Po5 and Po6, like the curved pipe section C5 indicated by the dotted line in Fig. 1. This means that the curved pipe portion C5 can be separated from the straight pipe portions Po5 and Po6.
As for how to attach and detach the bent pipe section C5 and the straight pipe sections Po5 and Po6, the flange section (not shown) is attached to both ends of the bent pipe section C5 and the left end of the straight pipe sections Po5 and Po6. The bent pipe portion C5 may be attached to and removed from the straight pipe portion Po5 and the straight pipe portion Po6 by tightening or loosening the flange portion using bolts, nuts, etc. The attachment/detachment method is not limited to this, and as long as it is detachable, for example, it is not limited to the method of using a flange part, and both ends of the curved pipe part C5 can be screwed to the left end parts of the straight pipe part Po5 and the straight pipe part Po6. You can put it on and take it off by letting it go.
Although the fixing plate 21 has a rectangular shape in FIG. 1, the material and shape of the fixing plate 21 can be Not particularly limited.
As mentioned above, since the plurality of straight pipe parts and the plurality of curved pipe parts C can be separated, the inner circumferential surfaces of the straight pipe parts and the curved pipe parts C can be easily cleaned by separating them. The maintainability of the crystallization system 10A can be improved.
　図１の例では、直管部は、直管部Ｐｏ１、直管部Ｐｏ２、直管部Ｐｏ３、直管部Ｐｏ４、直管部Ｐｏ５、直管部Ｐｏ６の６つの直管部により構成されており、曲管部Ｃは、曲管部Ｃ１、曲管部Ｃ２、曲管部Ｃ３、曲管部Ｃ４、曲管部Ｃ５の５つの曲管部から構成されているが、この例に限定されない。
　直管部Ｐｏは、６つ以上の直管部Ｐｏから構成されていても良いし、６つ以下の直管部Ｐｏから構成されていても良い。直管部Ｐｏの個数に合わせて、曲管部Ｃの個数も増減する。例えば、図１の例において、直管部Ｐｏ３の右端部に第一端が接続されている曲管部Ｃ２の第二端を配管２２の左端部に接続しても良い。この場合、曲管部Ｃ２に伸縮及び湾曲自在の蛇腹部が設けられていることにより、曲管部Ｃ２が伸縮自在であっても良い。 In the example of FIG. 1, the straight pipe section is composed of six straight pipe sections: straight pipe section Po1, straight pipe section Po2, straight pipe section Po3, straight pipe section Po4, straight pipe section Po5, and straight pipe section Po6. The curved pipe section C is composed of five curved pipe sections: a curved pipe section C 1 , a curved pipe section C 2 , a curved pipe section C 3 , a curved pipe section C 4 , and a curved pipe section C 5 . It is not limited to this example.
The straight pipe portion Po may be composed of six or more straight pipe parts Po, or may be composed of six or less straight pipe parts Po. The number of curved pipe parts C also increases or decreases in accordance with the number of straight pipe parts Po. For example, in the example of FIG. 1, the second end of the curved pipe portion C2 , whose first end is connected to the right end portion of the straight pipe portion Po3, may be connected to the left end portion of the pipe 22. In this case, the curved tube portion C 2 may be provided with a bellows portion that can be expanded and contracted, so that the curved tube portion C 2 can be expanded and contracted.
　このように、屈曲部Ｐｐの管路長、即ち、直管部と曲管部Ｃの合計の長さ（直管部と曲管部Ｃの個数）は、スラリＤ１を所望の滞留時間だけ、滞留させることを目的に要望に応じて調節することができる。即ち、より長い滞留時間が望まれる場合には、直管部と曲管部Ｃの数を増して屈曲部Ｐｐの管路長を長くすることが望ましく、より短い滞留時間が望まれる場合には、直管部と曲管部Ｃの数を減らして屈曲部Ｐｐの管路長を短くすることが望ましい。 In this way, the pipe length of the bent portion Pp, that is, the total length of the straight pipe portion and the bent pipe portion C (the number of the straight pipe portion and the bent pipe portion C) is such that the slurry D1 is kept for the desired residence time. It can be adjusted as desired to achieve retention. That is, when a longer residence time is desired, it is desirable to increase the number of straight pipe sections and bent pipe sections C to lengthen the pipe length of the bent section Pp, and when a shorter residence time is desired, It is desirable to reduce the number of straight pipe portions and bent pipe portions C to shorten the pipe length of the bent portion Pp.
　ここで、スラリＤ１の流速は、スラリＤ１を構成する粒子の比重と径により決まる。即ち、スラリＤ１を構成する粒子の比重と径により、スラリＤ１を構成する粒子の沈降速度が決まるので、スラリＤ１が配管内で沈降することなく流通されるようにスラリＤ１の流速を決める。そのため、所望のスラリＤ１の滞留時間と、スラリＤ１を沈降させないためのスラリＤ１の流速とから、屈曲部Ｐｐの管路長を求めることができる。 Here, the flow rate of the slurry D1 is determined by the specific gravity and diameter of the particles that make up the slurry D1. That is, since the settling speed of the particles making up the slurry D1 is determined by the specific gravity and diameter of the particles making up the slurry D1, the flow rate of the slurry D1 is determined so that the slurry D1 flows through the pipe without settling. Therefore, the pipe length of the bent portion Pp can be determined from the desired residence time of the slurry D1 and the flow rate of the slurry D1 to prevent the slurry D1 from settling.
　晶析装置４と屈曲部Ｐｐは内径ｒ１の配管２２により接続されている。屈曲部Ｐｐと循環ポンプ３０は内径ｒ４の配管２３により接続されている。循環ポンプ３０と晶析装置４は内径ｒ５の配管２４により接続されている。
　図１の例では、循環管路Ｐｏの内径、即ち、配管２２の内径ｒ１、直管部Ｐｏ１、Ｐｏ２、Ｐｏ３、Ｐｏ４、Ｐｏ５、Ｐｏ６の内径ｒ２、曲管部Ｃ１、Ｃ２、Ｃ３、Ｃ４、Ｃ５の内径ｒ３、配管２３の内径ｒ４、配管２４の内径ｒ５は、同一とされている。この場合、配管２２、直管部Ｐｏ１、Ｐｏ２、Ｐｏ３、Ｐｏ４、Ｐｏ５、Ｐｏ６、曲管部Ｃ１、Ｃ２、Ｃ３、Ｃ４、Ｃ５、配管２３、配管２４の断面積が一定となるため、管路を流れるスラリＤ１の流動解析が容易となる。しかしながら、上記の例に限定されず、循環管路Ｐｏの内径、即ち、配管２２の内径ｒ１、直管部Ｐｏ１、Ｐｏ２、Ｐｏ３、Ｐｏ４、Ｐｏ５、Ｐｏ６の内径ｒ２、曲管部Ｃ１、Ｃ２、Ｃ３、Ｃ４、Ｃ５の内径ｒ３、配管２３の内径ｒ４、配管２４の内径ｒ５が互いに異なっていても良い。その場合、異なった内径を考慮して流動解析を行えばよい。 The crystallizer 4 and the bent portion Pp are connected by a pipe 22 having an inner diameter r1 . The bent portion Pp and the circulation pump 30 are connected by a pipe 23 having an inner diameter r4 . The circulation pump 30 and the crystallizer 4 are connected by a pipe 24 having an inner diameter r5 .
In the example of FIG. 1, the inner diameter of the circulation pipe Po, that is, the inner diameter r 1 of the pipe 22, the inner diameter r 2 of the straight pipe portions Po1, Po2, Po3, Po4, Po5, Po6, the curved pipe portions C 1 , C 2 , The inner diameter r 3 of C 3 , C 4 , and C 5 , the inner diameter r 4 of the pipe 23, and the inner diameter r 5 of the pipe 24 are the same. In this case, the cross-sectional areas of the pipe 22, the straight pipe parts Po1, Po2, Po3, Po4, Po5, Po6, the curved pipe parts C1 , C2 , C3 , C4 , C5 , the pipe 23, and the pipe 24 are constant. Therefore, flow analysis of the slurry D1 flowing through the pipe becomes easy. However, the example is not limited to the above example, and the inner diameter of the circulation pipe Po, that is, the inner diameter r 1 of the pipe 22, the inner diameter r 2 of the straight pipe portions Po1, Po2, Po3, Po4, Po5, and Po6, the curved pipe portion C 1 , C2 , C3 , C4 , and C5 , the inner diameter r4 of the pipe 23, and the inner diameter r5 of the pipe 24 may be different from each other. In that case, flow analysis may be performed taking different inner diameters into consideration.
　屈曲部Ｐｐから排出されるスラリＤ１が流れる配管２３には、モータＭで駆動される第２循環ポンプ３１に接続される管路が接続されている。この管路が配管２３からスラリＤ１を引き抜き、これを集積する事で製品となる。モータＭと第２循環ポンプ３１との間に燃料指示調節計（Flow Indication Controller）ＦＩＣ４が設けられ、晶析システム１０Ａの外部に引き抜かれるスラリＤ１の流量の維持又は調節を行う。第２循環ポンプ３１は、循環ポンプ３０と同様に、流量を調整可能に循環させる機能を有するスラリ排出ポンプである。しかしながら、配管２３からスラリＤ１を引き抜く機能を有する装置であれば必ずしもスラリ排出ポンプに限定されず、例えば、回転数を制御可能な羽根車が管路に設けられていても良い。
　スラリＤ１が外部に引き抜かれた直後の配管２３におけるスラリＤ１の圧力を必要に応じて圧力計（Pressure Indicator）ＰＩ２でモニターする。 A pipe line connected to a second circulation pump 31 driven by a motor M is connected to the pipe 23 through which the slurry D1 discharged from the bent portion Pp flows. This pipe line pulls out the slurry D1 from the pipe 23 and accumulates it to form a product. A fuel flow indication controller FIC 4 is provided between the motor M and the second circulation pump 31, and maintains or adjusts the flow rate of the slurry D1 drawn out of the crystallization system 10A. The second circulation pump 31, like the circulation pump 30, is a slurry discharge pump that has a function of circulating the slurry with an adjustable flow rate. However, the device is not necessarily limited to the slurry discharge pump as long as it has the function of drawing out the slurry D1 from the pipe 23, and for example, an impeller whose rotation speed can be controlled may be provided in the pipe.
The pressure of the slurry D1 in the pipe 23 immediately after the slurry D1 is pulled out is monitored by a pressure indicator PI 2 as necessary.
　このような屈曲部Ｐｐを有する循環管路Ｐｏを備える晶析システム１０Ａによれば、晶析装置４において生成される粒子を含むスラリＤ１を、循環ポンプ３０の流量制御により、容易に完全均一混合することができる。さらに、晶析装置４において生成される粒子を含むスラリＤ１を、屈曲部Ｐｐの管路長を調節することで、滞留槽を必須とすることなく、所望の時間だけ滞留させることができる。従って、滞留槽を用いる場合に要求されたスラリＤ１の複雑な流動解析を行うことなく、屈曲部ＰｐにおけるスラリＤ１の滞留時間を調節することができる。なお、不図示の滞留槽を晶析システム１０Ａに加えても良い。 According to the crystallization system 10A including the circulation pipe Po having such a bent portion Pp, the slurry D1 containing particles generated in the crystallizer 4 can be easily and completely uniformly mixed by controlling the flow rate of the circulation pump 30. can do. Furthermore, by adjusting the pipe length of the bent portion Pp, the slurry D1 containing particles generated in the crystallizer 4 can be retained for a desired time without requiring a retention tank. Therefore, the residence time of the slurry D1 at the bent portion Pp can be adjusted without performing complicated flow analysis of the slurry D1, which is required when using a residence tank. Note that a retention tank (not shown) may be added to the crystallization system 10A.
＜第２実施形態＞
　次に、第２実施形態に係る晶析システム１０Ｂを、図２を参照しながら説明する。以下では、第１実施形態と異なる点のみ説明し、第１実施形態と同じ部材には同じ参照番号を付し説明を省略する。 <Second embodiment>
Next, a crystallization system 10B according to a second embodiment will be described with reference to FIG. 2. In the following, only the points different from the first embodiment will be explained, and the same reference numbers will be given to the same members as in the first embodiment, and the explanation will be omitted.
　晶析システム１０Ｂは、屈曲部Ｐｐ（第１屈曲部）に加えて第２屈曲部Ｐｐａが設けられている点で第１実施形態の晶析システム１０Ａと異なっている。 The crystallization system 10B differs from the crystallization system 10A of the first embodiment in that a second bent portion Ppa is provided in addition to the bent portion Pp (first bent portion).
　第２屈曲部Ｐｐａは、第１屈曲部Ｐｐと同様の構成を有する。配管２２の途中から、第２屈曲部Ｐｐａに向かって分岐する配管２２ａが延びている。また、第２屈曲部Ｐｐａから排出されるスラリＤ１は、配管２３ａを経由して、第１屈曲部Ｐｐから排出されるスラリＤ１が流通する配管２３に合流する。 The second bent portion Ppa has the same configuration as the first bent portion Pp. A pipe 22a extends from the middle of the pipe 22 and branches toward the second bent portion Ppa. Further, the slurry D1 discharged from the second bent portion Ppa passes through the pipe 23a and joins the pipe 23 through which the slurry D1 discharged from the first bent portion Pp flows.
　図２に示されるように、配管２２ａの入り口と配管２３ａの出口には、弁Ｖ１と弁Ｖ２が設けられている。弁Ｖ１と弁Ｖ２とを開弁することで、第１屈曲部Ｐｐと第２屈曲部Ｐｐａの両方にスラリＤ１を流すことができる。一方、弁Ｖ１と弁Ｖ２とを閉弁することで、第１屈曲部ＰｐのみにスラリＤ１を流すことができ、第１実施形態の晶析システム１０Ａと同様の構成とすることができる。 As shown in FIG. 2, a valve V1 and a valve V2 are provided at the inlet of the pipe 22a and the outlet of the pipe 23a. By opening the valves V1 and V2, the slurry D1 can flow into both the first bent portion Pp and the second bent portion Ppa. On the other hand, by closing the valves V1 and V2, it is possible to flow the slurry D1 only through the first bent portion Pp, and it is possible to have the same configuration as the crystallization system 10A of the first embodiment.
　このような晶析システム１０Ｂによれば、スラリＤ１の流量に応じて、第１屈曲部Ｐｐに加えて第２屈曲部ＰｐａにもスラリＤ１を流すことができる。 According to such a crystallization system 10B, the slurry D1 can be made to flow not only to the first bent portion Pp but also to the second bent portion Ppa depending on the flow rate of the slurry D1.
＜第３実施形態＞
　次に、第３実施形態に係る晶析システム１０Ｃを、図３を参照しながら説明する。以下では、第１実施形態と異なる点のみ説明し、第１実施形態と同じ部材には同じ参照番号を付し説明を省略する。 <Third embodiment>
Next, a crystallization system 10C according to a third embodiment will be described with reference to FIG. 3. In the following, only the points different from the first embodiment will be explained, and the same reference numbers will be given to the same members as in the first embodiment, and the explanation will be omitted.
　晶析システム１０Ｃは、屈曲部Ｐｐの少なくとも一部が温度調節槽１３の中に設けられている点で第１実施形態の晶析システム１０Ａと異なっている。 The crystallization system 10C differs from the crystallization system 10A of the first embodiment in that at least a portion of the bent portion Pp is provided in the temperature adjustment tank 13.
　温度調節槽１３は、不図示のポンプ等により、冷水等の冷媒ＣＷが温度調節槽１３の内部を一方向に流れる状態を維持している部材である。このような温度調節槽１３の中に、屈曲部Ｐｐの少なくとも一部を設けた場合、屈曲部Ｐｐの直管部Ｐｏ１、Ｐｏ２、Ｐｏ３、Ｐｏ４、Ｐｏ５、Ｐｏ６に冷媒が衝突する。この場合、屈曲部Ｐｐの直管部Ｐｏ１、Ｐｏ２、Ｐｏ３、Ｐｏ４、Ｐｏ５、Ｐｏ６を流れるスラリＤ１と冷媒ＣＷとの間で、直管部Ｐｏ１、Ｐｏ２、Ｐｏ３、Ｐｏ４、Ｐｏ５、Ｐｏ６を構成する部材を介して熱交換が行われる。よって、スラリＤ１を冷却又は加熱することができる。
　ここで、図３の場合は、冷媒ＣＷの流れ方向に対して直管部Ｐｏ１、Ｐｏ２、Ｐｏ３、Ｐｏ４、Ｐｏ５、Ｐｏ６が略垂直に設けられているが、必ずしも冷媒ＣＷの流れ方向に対して直管部Ｐｏ１、Ｐｏ２、Ｐｏ３、Ｐｏ４、Ｐｏ５、Ｐｏ６が略垂直に設けられていなくとも良く、垂直ではない角度を付けて設けられていても良い。また、屈曲部Ｐｐの曲管部Ｃにおいて冷媒ＣＷとの熱交換が行われても良いし、屈曲部Ｐｐの直管部と曲管部Ｃとの両方で冷媒ＣＷとの熱交換が行われても良い。 The temperature adjustment tank 13 is a member that maintains a state in which a refrigerant CW such as cold water flows in one direction inside the temperature adjustment tank 13 by a pump (not shown) or the like. When at least a portion of the bent portion Pp is provided in such a temperature adjustment tank 13, the refrigerant collides with the straight pipe portions Po1, Po2, Po3, Po4, Po5, and Po6 of the bent portion Pp. In this case, the straight pipe parts Po1, Po2, Po3, Po4, Po5, Po6 are formed between the slurry D1 and the refrigerant CW flowing through the straight pipe parts Po1, Po2, Po3, Po4, Po5, Po6 of the bent part Pp. Heat exchange takes place through the members. Therefore, the slurry D1 can be cooled or heated.
Here, in the case of FIG. 3, the straight pipe portions Po1, Po2, Po3, Po4, Po5, and Po6 are provided approximately perpendicularly to the flow direction of the refrigerant CW, but they are not necessarily provided in the flow direction of the refrigerant CW. The straight pipe portions Po1, Po2, Po3, Po4, Po5, and Po6 do not need to be provided substantially vertically, and may be provided at an angle that is not perpendicular. Further, heat exchange with the refrigerant CW may be performed in the bent pipe portion C of the bent portion Pp, or heat exchange with the refrigerant CW may be performed in both the straight pipe portion and the bent pipe portion C of the bent portion Pp. It's okay.
　ここで、屈曲部Ｐｐのうち、直管部Ｐｏ１、Ｐｏ２、Ｐｏ３、Ｐｏ４、Ｐｏ５、Ｐｏ６の長さ、或いは直管部Ｐｏ１、Ｐｏ２、Ｐｏ３、Ｐｏ４、Ｐｏ５、Ｐｏ６の数を調節することで、スラリＤ１に対する温度調整能力を調整することができる。例えば、直管部Ｐｏ１を流れる熱量Ｑを有するスラリＤ１から熱量Ｑ１が熱交換により冷媒ＣＷに移動したとすると、直管部Ｐｏ２を流れる熱量（Ｑ－Ｑ１）を有するスラリＤ１から熱量Ｑ２が熱交換により冷媒ＣＷに移動する。さらに、直管部Ｐｏ３を流れる熱量（Ｑ－（Ｑ１＋Ｑ２））を有するスラリＤ１から熱量Ｑ３が熱交換により冷媒ＣＷに移動すると、直管部Ｐｏ４を流れるスラリＤ１の熱量は（Ｑ－（Ｑ１＋Ｑ２＋Ｑ３））となる。これを所望の回数繰り返すことで、スラリＤ１の熱量を低減させることができるので、スラリＤ１を所望の量だけ冷却することができる。スラリＤ１を加熱する場合も同様である。 Here, by adjusting the length of the straight pipe parts Po1, Po2, Po3, Po4, Po5, Po6 or the number of straight pipe parts Po1, Po2, Po3, Po4, Po5, Po6 among the bent parts Pp, The temperature adjustment ability for slurry D1 can be adjusted. For example, if the heat amount Q1 is transferred to the refrigerant CW by heat exchange from the slurry D1 having the heat amount Q flowing through the straight pipe portion Po1, the heat amount Q2 is transferred from the slurry D1 having the heat amount (Q-Q1) flowing through the straight pipe portion Po2. The refrigerant is transferred to CW by exchange. Furthermore, when the heat amount Q3 from the slurry D1 having the heat amount (Q-(Q1+Q2)) flowing through the straight pipe portion Po3 is transferred to the refrigerant CW by heat exchange, the heat amount of the slurry D1 flowing through the straight pipe portion Po4 becomes (Q-(Q1+Q2+Q3) ). By repeating this a desired number of times, the amount of heat of the slurry D1 can be reduced, so that the slurry D1 can be cooled by a desired amount. The same applies when heating the slurry D1.
　このような晶析システム１０Ｃによれば、冷媒ＣＷと熱交換が行われる屈曲部Ｐｐの管路長、即ち、直管部Ｐｏ１、Ｐｏ２、Ｐｏ３、Ｐｏ４、Ｐｏ５、Ｐｏ６の管路長、或いは数を調節することで、スラリＤ１を所望の量だけ冷却又は加熱することができる。 According to such a crystallization system 10C, the pipe length of the bent part Pp where heat exchange is performed with the refrigerant CW, that is, the pipe length or number of the straight pipe parts Po1, Po2, Po3, Po4, Po5, Po6. By adjusting the amount, slurry D1 can be cooled or heated by a desired amount.
＜第１実施形態の第１の変形例＞
　以下、第１実施形態に係る晶析システム１０Ａの第１の変形例に係る晶析システム１０Ａ１を、図４を参照して説明する。以下の説明では、第１実施形態に係る晶析システム１０Ａと異なる点のみ説明し、同じ部材には同じ参照番号を付し、その説明を省略する。 <First modification of the first embodiment>
Hereinafter, a crystallization system 10A1 according to a first modification of the crystallization system 10A according to the first embodiment will be described with reference to FIG. 4. In the following description, only the points different from the crystallization system 10A according to the first embodiment will be explained, the same members will be given the same reference numbers, and the description thereof will be omitted.
　第１の変形例に係る晶析システム１０Ａ１では、晶析装置４ａが撹拌翼Ｗを備えている点で晶析装置４と異なっている。 A crystallization system 10A1 according to the first modification differs from the crystallizer 4 in that the crystallizer 4a includes a stirring blade W.
　撹拌翼Ｗは、円筒部２と、円筒部２の内周面２ｉに外縁部が固定される円盤状の円盤部８と、を備えている。円盤部８は、円筒部２の高さが概ね半分となる位置に設けられるが、この例に限定されず、円筒部２の高さの概ね半分よりも下側や上側に設けられても良い。円盤部８の平面視の中心に回転軸３が固定されている。回転軸３の中空の内部は管路Ｐ１とされている。円盤部８の内部には複数の管路Ｐ２が中心から放射状に外縁部に向かって延びている。回転軸３の管路Ｐ１と円盤部８の管路Ｐ２とは連通している。撹拌翼Ｗの回転軸３には、晶析装置４の外部に設けられる主原料ＳＭを貯蔵する不図示のタンクから第２の反応液Ｌ２が供給される。第２の反応液Ｌ２は、ロータリージョイントＲを介して回転軸３の中空の管路Ｐ１に供給され、その後、円盤部８の管路Ｐ２に供給される。管路Ｐ２の反応槽１の径方向外側の先端は下方に向けて開口しており第２の反応液Ｌ２が排出される給液部５ｂとされている。従って、円盤部８には、給液部５ｂが円盤部の周方向に間隔を空けて複数設けられている。給液部５ｂの個数は例えば８個設けられている。給液部５ｂの個数は限定されないが、中心軸Ｏ１に対して対称に設けることが望ましい。 The stirring blade W includes a cylindrical part 2 and a disc-shaped disc part 8 whose outer edge is fixed to the inner peripheral surface 2i of the cylindrical part 2. The disk portion 8 is provided at a position where the height of the cylindrical portion 2 is approximately half, but is not limited to this example, and may be provided below or above approximately half the height of the cylindrical portion 2. . The rotating shaft 3 is fixed to the center of the disk portion 8 in plan view. The hollow interior of the rotating shaft 3 is defined as a conduit P1. Inside the disk portion 8, a plurality of conduits P2 extend radially from the center toward the outer edge. The conduit P1 of the rotating shaft 3 and the conduit P2 of the disk portion 8 are in communication. The second reaction liquid L2 is supplied to the rotating shaft 3 of the stirring blade W from a tank (not shown) provided outside the crystallizer 4 and storing the main raw material SM . The second reaction liquid L2 is supplied to the hollow pipe line P1 of the rotating shaft 3 via the rotary joint R, and then to the pipe line P2 of the disc part 8. The tip of the pipe P2 on the outside in the radial direction of the reaction tank 1 is opened downward and serves as a liquid supply section 5b from which the second reaction liquid L2 is discharged. Therefore, the disk portion 8 is provided with a plurality of liquid supply portions 5b at intervals in the circumferential direction of the disk portion. For example, eight liquid supply parts 5b are provided. Although the number of liquid supply parts 5b is not limited, it is desirable to provide them symmetrically with respect to the central axis O1.
　本変形例においては、撹拌翼Ｗの円筒部２の内周面２ｉと給液部５ｂの中心との距離は２ｍｍ以下とされている。また、撹拌翼Ｗの円筒部２の外周面２ｏと反応槽１の内周面１ｉとの距離（クリアランス）をＬ３、撹拌翼Ｗ（円筒部２）の中心軸Ｏ１に沿う高さをＨとすると、ＨとＬ３との比であるＨ／Ｌ３が１０以上であることが好ましい。また、Ｈ／Ｌ３が２５以上であることがより好ましい。従って、この実施例と異なるサイズの装置を使用する場合であっても、この比を基に同様の装置を製作することができる。撹拌翼Ｗは、５ｍ／秒以上５０ｍ／秒以下の周速で回転する。
　なお、Ｈ／Ｌ３の比率は、目的によって、上述の比率と異なる場合がある。例えば、結晶破砕を抑制したい場合には、比率を上記の値から下げても良い。 In this modification, the distance between the inner circumferential surface 2i of the cylindrical portion 2 of the stirring blade W and the center of the liquid supply portion 5b is 2 mm or less. Further, the distance (clearance) between the outer peripheral surface 2o of the cylindrical part 2 of the stirring blade W and the inner peripheral surface 1i of the reaction tank 1 is L3, and the height along the central axis O1 of the stirring blade W (cylindrical part 2) is H. Then, it is preferable that H/L3, which is the ratio of H to L3, is 10 or more. Moreover, it is more preferable that H/L3 is 25 or more. Therefore, even if a device of a different size from this embodiment is used, a similar device can be manufactured based on this ratio. The stirring blade W rotates at a circumferential speed of 5 m/sec or more and 50 m/sec or less.
Note that the H/L3 ratio may differ from the above ratio depending on the purpose. For example, if it is desired to suppress crystal crushing, the ratio may be lowered from the above value.
　撹拌翼Ｗの円筒部２には、円筒部２の径方向に貫通する複数の孔ｈが設けられている。これらの孔ｈは、第１の反応液Ｌ１、第２の反応液Ｌ２、或いはその混合液が流通可能とされている。そのため、第１の反応液Ｌ１、第２の反応液Ｌ２、或いはその混合液は、複数の孔ｈを通じて、撹拌翼Ｗの内側から外側に、又は撹拌翼Ｗの外側から内側に移動可能である。なお、孔ｈに加えて、円盤部８に中心軸Ｏ１方向に貫通する複数の不図示の孔９が設けられていても良い。この場合、第１の反応液Ｌ１、第２の反応液Ｌ２、或いはその混合液は、複数の孔ｈに加えて孔９を通じても撹拌翼Ｗの内側から外側に、又は撹拌翼Ｗの外側から内側に移動可能となる。 The cylindrical portion 2 of the stirring blade W is provided with a plurality of holes h that penetrate in the radial direction of the cylindrical portion 2. The first reaction liquid L1, the 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 be moved 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 hole h, a plurality of holes 9 (not shown) may be provided in the disk portion 8 to penetrate in the direction of the central axis O1. In this case, the first reaction liquid L1, the second reaction liquid L2, or a mixture thereof can be passed from the inside of the stirring blade W to the outside through the hole 9 in addition to the plurality of holes h, or from the outside of the stirring blade W. Can be moved inward.
　このような晶析装置４ａにおいて、導入口５ａから所望量の第１の反応液Ｌ１を反応槽１に供給する。供給される第１の反応液Ｌ１の量は、反応槽１を満たす程度（満液状態）でも良いし、或いは、撹拌翼Ｗが回転した際に第１の反応液Ｌ１が反応槽１の中心軸Ｏ１を中心として円運動を行うことにより第１の反応液Ｌ１に発生する遠心力により反応槽１の内周面１ｉに押し付けられて、反応槽１の内周面１ｉに第１の反応液Ｌ１の液膜が形成される程度に供給しても良い。以下では、第１の反応液Ｌ１が満液状態になる程度供給される場合を想定して説明する。また、第１の反応液Ｌ１を上述の満液状態または液膜形成状態となる程度に供給した後に第１の反応液Ｌ１の供給を止めてから反応槽１で反応をさせても良いし、第１の反応液Ｌ１を上述の満液状態または液膜形成状態となる程度の流量に維持しながら反応槽１での反応を継続的に行っても良い。
　例えば、排出口６に不図示の開度調整バルブを設け、この開度調整バルブの開度を調整することにより、反応槽１を、満液状態と液膜が形成される液膜状態とのいずれかに選択することができる。 In such a crystallizer 4a, a desired amount of the first reaction liquid L1 is supplied to the reaction tank 1 from the inlet 5a. The amount of the first reaction liquid L1 supplied may be enough to fill the reaction tank 1 (full liquid state), or the first reaction liquid L1 may be supplied to the center of the reaction tank 1 when the stirring blade W rotates. The first reaction liquid L1 is pressed against the inner peripheral surface 1i of the reaction tank 1 by the centrifugal force generated in the first reaction liquid L1 by performing a circular motion around the axis O1, and the first reaction liquid L1 is pressed against the inner peripheral surface 1i of the reaction tank 1. It may be supplied to such an extent that a liquid film of L1 is formed. The following description will be made on the assumption that the first reaction liquid L1 is supplied to the extent that it is in a full liquid state. Further, after the first reaction liquid L1 is supplied to the above-mentioned full liquid state or liquid film forming state, the supply of the first reaction liquid L1 may be stopped and then the reaction may be carried out in the reaction tank 1. The reaction in the reaction tank 1 may be continuously carried out while maintaining the first reaction liquid L1 at a flow rate sufficient to reach the above-mentioned full liquid state or liquid film forming state.
For example, by providing an opening adjustment valve (not shown) in the discharge port 6 and adjusting the opening of this opening adjustment valve, the reaction tank 1 can be adjusted between a full liquid state and a liquid film state in which a liquid film is formed. You can choose either one.
　反応槽１が第１の反応液Ｌ１で満たされた状態において、撹拌翼Ｗを回転させるとともに、第２の反応液Ｌ２を給液部５ｂから撹拌翼Ｗの円筒部２の内周面２ｉに沿って排出することで、第２の反応液Ｌ２を反応槽１内に供給する。こうすることで、給液部５ｂから撹拌翼Ｗの円筒部２の内周面２ｉに沿って排出された第２の反応液Ｌ２が、第１の反応液Ｌ１で満たされた反応槽１のうちで撹拌翼Ｗの円筒部２の内周面２ｉ近傍で撹拌翼Ｗの回転に伴って回転している第１の反応液Ｌ１と接触する。こうして第１の反応液Ｌ１と第２の反応液Ｌ２とが接触することにより反応が発生して粒子が生成される。 While the reaction tank 1 is filled with the first reaction liquid L1, the stirring blade W is rotated and the second reaction liquid L2 is supplied from the liquid supply part 5b to the inner peripheral surface 2i of the cylindrical part 2 of the stirring blade W. By discharging along the line, the second reaction liquid L2 is supplied into the reaction tank 1. By doing this, the second reaction liquid L2 discharged from the liquid supply part 5b along the inner circumferential surface 2i of the cylindrical part 2 of the stirring blade W enters the reaction tank 1 filled with the first reaction liquid L1. It comes into contact with the first reaction liquid L1 that is rotating with the rotation of the stirring blade W near the inner circumferential surface 2i of the cylindrical portion 2 of the stirring blade W. In this way, the first reaction liquid L1 and the second reaction liquid L2 come into contact with each other, whereby a reaction occurs and particles are generated.
　この際、第１の反応液Ｌ１に、５ｍ／秒以上５０ｍ／秒以下の周速で回転している撹拌翼Ｗの給液部５ｂから第２の反応液Ｌ２を供給することで、第２の反応液Ｌ２を第１の反応液Ｌ１と均一に混合することができる。 At this time, the second reaction liquid L2 is supplied to the first reaction liquid L1 from the liquid supply part 5b of the stirring blade W rotating at a circumferential speed of 5 m/sec to 50 m/sec. The reaction liquid L2 can be uniformly mixed with the first reaction liquid L1.
　ここで、撹拌翼Ｗの回転に伴って回転している第１の反応液Ｌ１と、５ｍ／秒以上５０ｍ／秒以下の周速で回転している撹拌翼Ｗの給液部５ｂから排出される第２の反応液Ｌ２と、これらの混合液に発生する遠心力により、第１の反応液Ｌ１、第２の反応液Ｌ２、及び混合液（以下、まとめて混合液と呼ぶ場合がある）は撹拌翼Ｗの円筒部２の径方向外側に移動し、撹拌翼Ｗの円筒部２に設けられた複数の孔ｈを通って反応槽１の内周面１ｉに衝突し、その後、反応槽１の内周面１ｉに沿って上下方向に移動する。主に下方に移動した混合液は、撹拌翼Ｗの回転により生じる遠心力に起因する径方向外側に向かう流れに引き寄せられて再び撹拌翼Ｗの円筒部２に設けられた複数の孔ｈを通って反応槽１の内周面１ｉに衝突し、その後、反応槽１の内周面１ｉに沿って上下方向に移動することで対流が生まれる。ここで、複数の孔ｈを混合液が通過する際、絞り流路の効果により、混合液は径方向外側に加速されるので、混合液の径方向外向きの流速は、複数の孔ｈ近傍で最も高い。さらに、５ｍ／秒以上５０ｍ／秒以下の周速で回転する撹拌翼Ｗの円筒部２の外周面２ｏ及び内周面２ｉと、固定されている反応槽１の内周面１ｉとの間に存在する混合液には、周方向に剪断力が与えられる。混合液に与えられる剪断力は撹拌翼Ｗの円筒部２の内周面２ｉと外周面２ｏとに近ければ近い程大きい。混合液に与えられる剪断力は、得られる粒子の粒子径と均一性を決定する大きな要因となる。特に与えられる剪断力が大きければ大きい程、微細な粒子径を持つ粒子を得ることができる。 Here, the first reaction liquid L1 that is rotating with the rotation of the stirring blade W is discharged from the liquid supply part 5b of the stirring blade W that is rotating at a circumferential speed of 5 m/sec to 50 m/sec. The centrifugal force generated in the second reaction liquid L2 and the mixed liquid causes the first reaction liquid L1, the second reaction liquid L2, and the mixed liquid (hereinafter sometimes referred to collectively as the mixed liquid) moves radially outward of the cylindrical portion 2 of the stirring blade W, passes through the plurality of holes h provided in the cylindrical portion 2 of the stirring blade W, and collides with the inner circumferential surface 1i of the reaction tank 1, and then 1 in the vertical direction along the inner circumferential surface 1i. The mixed liquid that has mainly moved downward is drawn by the radially outward flow caused by the centrifugal force generated by the rotation of the stirring blade W, and passes through the plurality of holes h provided in the cylindrical part 2 of the stirring blade W again. The particles collide with the inner peripheral surface 1i of the reaction tank 1, and then move in the vertical direction along the inner peripheral surface 1i of the reaction tank 1, thereby generating convection. Here, when the mixed liquid passes through the plurality of holes h, the mixed liquid is accelerated radially outward due to the effect of the throttle channel, so the flow velocity of the mixed liquid outward in the radial direction is highest in Further, 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/sec or more and 50 m/sec or less and the inner circumferential surface 1i of the fixed reaction tank 1. A shearing force is applied to the existing mixed liquid in the circumferential direction. The closer the shearing force applied to the mixed liquid is to the inner circumferential surface 2i and outer circumferential surface 2o of the cylindrical portion 2 of the stirring blade W, the greater it is. The shearing force applied to the liquid mixture is a major factor in determining the particle size and uniformity of the resulting particles. In particular, the larger the applied shearing force, the more fine the particles can be obtained.
　本変形例の晶析装置４ａでは、給液部５ｂが、円盤部８の外縁部に設けられている。具体的には上記のように撹拌翼Ｗの円筒部２の内周面２ｉと給液部５ｂの中心との距離が２ｍｍ以下とされている。そのため、給液部５ｂから撹拌翼Ｗの円筒部２の内周面２ｉに沿って排出される第２の反応液Ｌ２と、撹拌翼Ｗの円筒部２の内周面２ｉ近傍で撹拌翼Ｗの回転に伴って回転している第１の反応液Ｌ１と、が初めて接触して反応を開始する反応開始ポイントには、遠心力と絞り流路の効果による径方向外側に向かう流れに加えて剪断力が最大限に与えられる。よって、与えられる剪断力が最も大きい領域を反応開始ポイントとすることができる。具体的には、撹拌翼Ｗの円筒部２の内周面２ｉと外周面２ｏから至近距離、例えば２ｍｍ以内、の領域に反応開始ポイントを形成することができる。ここで、混合液は上記の複数の孔ｈを通って円筒部２の内周側から外周側に移動可能である。従って、反応開始ポイントにおける第１の反応液Ｌ１と第２の反応液Ｌ２との撹拌が剪断力により促進される。そのため、より均一な第１の反応液Ｌ１と第２の反応液Ｌ２との混合が反応開始ポイントから開始され、混合液の流れに沿って反応が起こる場である反応場で混合及び反応が行われることで微細かつ均一な径を有する粒子を生成することができる。ここで、反応開始ポイントは反応が開始される領域を指し、反応場は反応が起きる場全体を指す。従って、反応開始ポイントは反応場に含まれる。
　なお、撹拌翼Ｗの上部に相当する反応槽１の内周面に不図示のバッフル（邪魔板）が設けられていても良い。バッフルは、反応槽１が満液の状態においては、渦の発生を抑制し混合液の撹拌を促進させる効果がある。一方、反応槽１が満液ではなく混合液の液膜が形成される状態においてはバッフルを設ける必要はない。
　なお、バッフルは必須の構成ではなく、設けなくても良い。例えば、反応槽１における回転軸３が挿入される箇所に不図示のメカニカルシールを設け、気相部の無い完全な満液状態とする場合、渦の発生が抑制されるため、バッフルを設けなくても良い。バッフルを設けない場合、流路抵抗が低減され、原動機Ｍの動力を低減できる。 In the crystallizer 4a of this modification, the liquid supply section 5b is provided at the outer edge of the disk section 8. Specifically, as described above, the distance between the inner circumferential surface 2i of the cylindrical portion 2 of the stirring blade W and the center of the liquid supply portion 5b is 2 mm or less. Therefore, the second reaction liquid L2 discharged from the liquid supply part 5b along the inner peripheral surface 2i of the cylindrical portion 2 of the stirring blade W, and the second reaction liquid L2 discharged from the liquid supply portion 5b along the inner peripheral surface 2i of the cylindrical portion 2 of the stirring blade W At the reaction start point where the first reaction liquid L1, which is rotating with the rotation of Maximum shear force is applied. Therefore, the region where the applied shearing force is the largest can be set as the reaction initiation point. Specifically, the reaction start point can be formed in a region within a close distance, for example, within 2 mm, from the inner circumferential surface 2i and outer circumferential surface 2o of the cylindrical portion 2 of the stirring blade W. Here, the mixed liquid can move from the inner circumferential side to the outer circumferential side of the cylindrical portion 2 through the plurality of holes h described above. Therefore, stirring of the first reaction liquid L1 and the second reaction liquid L2 at the reaction starting point is promoted by the shear force. Therefore, the more uniform mixing of the first reaction liquid L1 and the second reaction liquid L2 is started from the reaction start point, and the mixing and reaction are performed in the reaction field where the reaction occurs along the flow of the mixed liquid. By doing so, it is possible to produce particles with fine and uniform diameters. Here, the reaction initiation point refers to the area where the reaction starts, and the reaction field refers to the entire area where the reaction occurs. Therefore, the reaction initiation point is included in the reaction field.
Note that a baffle (not shown) may be provided on the inner peripheral surface of the reaction tank 1 corresponding to the upper part of the stirring blade W. The baffle has the effect of suppressing the generation of vortices and promoting stirring of the mixed liquid when the reaction tank 1 is full of liquid. On the other hand, in a state where the reaction tank 1 is not full of liquid and a liquid film of the mixed liquid is formed, there is no need to provide a baffle.
Note that the baffle is not an essential component and may not be provided. For example, if a mechanical seal (not shown) is provided at the location where the rotating shaft 3 is inserted in the reaction tank 1 to create a completely full liquid state with no gas phase, the generation of vortices will be suppressed, so no baffle will be provided. It's okay. When no baffle is provided, the flow path resistance is reduced and the power of the prime mover M can be reduced.
　なお、満液状態ではなく液膜が形成される状態においても満液状態の場合と同様の効果が得られる。 Note that the same effect as in the case of a full liquid state can be obtained even in a state where a liquid film is formed instead of a full liquid state.
　このような晶析装置４ａを含む第１の変形例に係る晶析システム１０Ａ１によれば、晶析装置４ａにおける反応生成物の粒子径、粒度分布、真球度などの粒子品質に影響を与える剪断力、第１の反応液Ｌ１の循環量、スラリの滞留時間を個別に調整することができ、より一層、粒子品質の制御性能を向上することができる。 According to the crystallization system 10A1 according to the first modification including such a crystallizer 4a, the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4a is affected. The shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
＜第１実施形態の第２の変形例＞
　以下、第１実施形態に係る晶析システム１０Ａの第２の変形例に係る晶析システム１０Ａ２を、図５を参照して説明する。第２の変形例の晶析装置４ｂでは、第１の変形例の晶析装置４ａの撹拌翼Ｗが撹拌翼Ｗａである点に相違がある。以下の説明では、撹拌翼Ｗとの相違点のみ説明し、重複している箇所の説明は省略する。
　撹拌翼Ｗａは、円盤部８の外縁部に設けられる給液部５ｂが円筒部２を貫通して径方向外側に開口している点において撹拌翼Ｗと異なっている。このような撹拌翼Ｗａでは、径方向外側に開口する給液部５ｂから第２の反応液Ｌ２が排出されるので、第２の反応液Ｌ２と、第１の反応液Ｌ１と第２の反応液Ｌ２との混合液の径方向（水平方向）への分散性が高い。このような撹拌翼Ｗａを備える晶析装置４ｂを用いることでも、撹拌翼Ｗを備える晶析装置４ａと同様の効果を奏することができる。なお、円盤部８に中心軸Ｏ１方向に貫通する不図示の複数の孔９が設けられていても良い。このような、複数の孔９は、混合液の一部を複数の孔９を介して攪拌翼Ｗの下側と上側とを流通可能とすることで、攪拌翼Ｗにかかる動力的な負荷を低減する効果があるが、複数の孔９を通過した混合液は攪拌翼Ｗ廻りの反応場を通過せずに反応場をショートパスしてしまうため、複数の孔９を設けない場合に比べ、均一で微細な粒子を製造する効果は低下する。従って、目的の粒子品質と所要動力を鑑みて、孔９の適用を選択することができる。 <Second modification of the first embodiment>
Hereinafter, a crystallization system 10A2 according to a second modification of the crystallization system 10A according to the first embodiment will be described with reference to FIG. 5. The crystallizer 4b of the second modification is different from the crystallizer 4a of the first modification in that the stirring blade W is a stirring blade Wa. In the following explanation, only the differences from the stirring blade W will be explained, and the explanation of the overlapping parts will be omitted.
The stirring blade Wa differs from the stirring blade W in that a liquid supply portion 5b provided at the outer edge of the disk portion 8 penetrates the cylindrical portion 2 and opens radially outward. In such a stirring blade Wa, the second reaction liquid L2 is discharged from the liquid supply part 5b that opens radially outward, so that the second reaction liquid L2, the first reaction liquid L1, and the second reaction are mixed. The mixed liquid with liquid L2 has high dispersibility in the radial direction (horizontal direction). Even by using the crystallizer 4b provided with such a stirring blade Wa, the same effects as the crystallizer 4a provided with the stirring blade W can be achieved. Incidentally, a plurality of holes 9 (not shown) may be provided in the disk portion 8 to penetrate in the direction of the central axis O1. Such a plurality of holes 9 allows a portion of the mixed liquid to flow between the lower side and the upper side of the stirring blade W through the plurality of holes 9, thereby reducing the dynamic load on the stirring blade W. Although it has the effect of reducing The effectiveness of producing uniform and fine particles is reduced. Therefore, the application of the holes 9 can be selected depending on the desired particle quality and the required power.
　このような晶析装置４ｂを含む第２の変形例に係る晶析システム１０Ａ２によれば、晶析装置４ｂにおける反応生成物の粒子径、粒度分布、真球度などの粒子品質に影響を与える剪断力、第１の反応液Ｌ１の循環量、スラリの滞留時間を個別に調整することができ、より一層、粒子品質の制御性能を向上することができる。 According to the crystallization system 10A2 according to the second modification including such a crystallizer 4b, the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4b is affected. The shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
＜第１実施形態の第３の変形例＞
　以下、第１実施形態に係る晶析システム１０Ａの第３の変形例に係る晶析システム１０Ａ３を、図６を参照して説明する。
　第３の変形例の晶析装置４ｃでは、第２の変形例における撹拌翼Ｗａが撹拌翼Ｗｂである点に相違がある。以下の説明では、撹拌翼Ｗａとの相違点のみ説明し、重複している箇所の説明は省略する。
　撹拌翼Ｗｂは、撹拌翼Ｗａにおける円盤部８より上側の円筒部２において、径方向に貫通する複数の孔ｈがない（閉塞されている）とともに、円筒部８の内周面２ｉに外縁部が固定される第２円盤部１５が円筒部２の上端部に設けられている。第２円盤部１５は円盤状の部材であり、その平面視の中心に回転軸３が貫通する孔を有する。回転軸３が貫通する孔を除き、中心軸Ｏ１方向に第２円盤部１５を貫通する孔はない。従って、第２円盤部１５の内側に第１の反応液Ｌ１、第２の反応液Ｌ２、及びその混合液が入り込むことはない。
　このような撹拌翼Ｗｂでは、円盤部８より上側の円筒部２に径方向に貫通する複数の孔ｈが設けられておらず、また、円筒部８の内周面２ｉに外縁部が固定される第２円盤部１５が円筒部２の上端部に設けられている。そのため、撹拌翼Ｗｂが回転する際の撹拌翼Ｗｂの抵抗力が低減され、撹拌翼Ｗａよりも少ない動力で撹拌翼Ｗｂを運転することができる。 <Third modification of first embodiment>
Hereinafter, a crystallization system 10A3 according to a third modification of the crystallization system 10A according to the first embodiment will be described with reference to FIG. 6.
The crystallizer 4c of the third modification differs in that the stirring blade Wa in the second modification is replaced by a stirring blade Wb. In the following explanation, only the differences from the stirring blade Wa will be explained, and the explanation of the overlapping parts will be omitted.
The stirring blade Wb has a plurality of holes h penetrating in the radial direction in the cylindrical part 2 above the disk part 8 of the stirring blade Wa (which are closed), and an outer edge part on the inner circumferential surface 2i of the cylindrical part 8. A second disk portion 15 to which is fixed is provided at the upper end of the cylindrical portion 2. The second disc part 15 is a disc-shaped member, and has a hole in the center of the second disc part 15, through which the rotating shaft 3 passes. There are no holes that pass through the second disk portion 15 in the direction of the central axis O1, except for the hole that the rotating shaft 3 passes through. Therefore, the first reaction liquid L1, the second reaction liquid L2, and the mixed liquid thereof do not enter the inside of the second disk portion 15.
In such a stirring blade Wb, the plurality of holes h penetrating in the radial direction are not provided in the cylindrical part 2 above the disk part 8, and the outer edge part is fixed to the inner circumferential surface 2i of the cylindrical part 8. A second disk portion 15 is provided at the upper end of the cylindrical portion 2. Therefore, the resistance force of the stirring blade Wb when the stirring blade Wb rotates is reduced, and the stirring blade Wb can be operated with less power than the stirring blade Wa.
　このような晶析装置４ｃを含む第３の変形例に係る晶析システム１０Ａ３によれば、晶析装置４ｃにおける反応生成物の粒子径、粒度分布、真球度などの粒子品質に影響を与える剪断力、第１の反応液Ｌ１の循環量、スラリの滞留時間を個別に調整することができ、より一層、粒子品質の制御性能を向上することができる。 According to the crystallization system 10A3 according to the third modification including such a crystallizer 4c, the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4c is affected. The shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
＜第１実施形態の補足説明＞
　ここで、図１～図３に戻って、第１～第３の実施形態の撹拌翼Ｗｃを詳細に説明する。
　第１実施形態における晶析装置４では、図４に示される、第１の変形例の晶析装置４ａの撹拌翼Ｗが撹拌翼Ｗｃである点に相違がある。以下の説明では、撹拌翼Ｗとの相違点のみ説明し、重複している箇所の説明は省略する。
　撹拌翼Ｗｃは、図１に示されるように、撹拌翼Ｗにおける円盤部８より上側の円筒部２において、径方向に貫通する複数の孔ｈがない（閉塞されている）とともに、円筒部８の内周面２ｉに外縁部が固定される第２円盤部１５が円筒部２の上端部に設けられている。第２円盤部１５は円盤状の部材であり、その平面視の中心に回転軸３が貫通する孔を有する。回転軸３が貫通する孔を除き、中心軸Ｏ１方向に第２円盤部１５を貫通する孔はない。従って、第２円盤部１５の内側に第１の反応液Ｌ１、第２の反応液Ｌ２、及びその混合液が入り込むことはない。
　このような撹拌翼Ｗｃでは、円盤部８より上側の円筒部２に径方向に貫通する複数の孔ｈが設けられておらず、また、円筒部８の内周面２ｉに外縁部が固定される第２円盤部１５が円筒部２の上端部に設けられているので、撹拌翼Ｗｃが回転する際の撹拌翼Ｗｃの抵抗力が低減される。そのため、撹拌翼Ｗよりも少ない動力で撹拌翼Ｗｃを運転することができる。 <Supplementary explanation of the first embodiment>
Now, returning to FIGS. 1 to 3, the stirring blades Wc of the first to third embodiments will be described in detail.
The crystallizer 4 in the first embodiment is different from the crystallizer 4a of the first modification shown in FIG. 4 in that the stirring blade W is a stirring blade Wc. In the following explanation, only the differences from the stirring blade W will be explained, and the explanation of the overlapping parts will be omitted.
As shown in FIG. 1, the stirring blade Wc has a plurality of holes h penetrating in the radial direction in the cylindrical portion 2 above the disk portion 8 of the stirring blade W (which are closed), and the cylindrical portion 8 A second disk portion 15 whose outer edge portion is fixed to the inner circumferential surface 2i of the cylinder portion 2 is provided at the upper end portion of the cylindrical portion 2. The second disc part 15 is a disc-shaped member, and has a hole in the center of the second disc part 15, through which the rotating shaft 3 passes. There are no holes that pass through the second disk portion 15 in the direction of the central axis O1, except for the hole that the rotating shaft 3 passes through. Therefore, the first reaction liquid L1, the second reaction liquid L2, and the mixed liquid thereof do not enter the inside of the second disk portion 15.
In such a stirring blade Wc, the plurality of holes h penetrating in the radial direction are not provided in the cylindrical part 2 above the disk part 8, and the outer edge part is fixed to the inner circumferential surface 2i of the cylindrical part 8. Since the second disk portion 15 is provided at the upper end of the cylindrical portion 2, the resistance force of the stirring blade Wc when the stirring blade Wc rotates is reduced. Therefore, the stirring blade Wc can be operated with less power than the stirring blade W.
　このような晶析装置４を含む第１実施形態に係る晶析システム１０Ａによれば、晶析装置４における反応生成物の粒子径、粒度分布、真球度などの粒子品質に影響を与える剪断力、第１の反応液Ｌ１の循環量、スラリの滞留時間を個別に調整することができ、より一層、粒子品質の制御性能を向上することができる。 According to the crystallization system 10A according to the first embodiment including such a crystallizer 4, shearing that affects particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4 The force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be individually adjusted, and the control performance of particle quality can be further improved.
＜第１実施形態の第４の変形例＞
　以下、第１実施形態に係る晶析システム１０Ａの第４の変形例に係る晶析システム１０Ａ４を、図７を参照して説明する。
　第４の変形例の晶析装置４ｄでは、第１の変形例の晶析装置４ａの撹拌翼Ｗが撹拌翼Ｗｄである点に相違がある。以下の説明では、撹拌翼Ｗとの相違点のみ説明し、重複している箇所の説明は省略する。
　撹拌翼Ｗｄは、図７に示されるように、円盤部８が円筒部２の上端部に設けられている点において撹拌翼Ｗと異なっている。また、円筒部２の高さが撹拌翼Ｗの円筒部２の高さの半分程度である。このような撹拌翼Ｗｄを備える晶析装置４ｄを用いることでも、撹拌翼Ｗを備える晶析装置４と同様の効果を奏することができる。また、円盤部８よりも上方に円筒部２が設けられていないため、撹拌翼Ｗｄを撹拌翼Ｗよりも軽量とすることができる。また撹拌翼Ｗｄを簡易な構造とすることができるので、撹拌翼Ｗよりも少ない動力で撹拌翼Ｗｄを運転することができ、晶析装置４の省エネ化と、撹拌翼Ｗｄの製造の容易化が期待できる。さらに、円筒部２の高さが短く抑えられているため、晶析装置４ｄを小型化することができる。なお、円盤部８に中心軸Ｏ１方向に貫通する不図示の複数の孔９が設けられていても良い。その場合、撹拌翼Ｗａの円盤部８に中心軸Ｏ１方向に貫通する複数の孔９が設けられている場合と同様の効果が期待できる。 <Fourth modification of the first embodiment>
Hereinafter, a crystallization system 10A4 according to a fourth modification of the crystallization system 10A according to the first embodiment will be described with reference to FIG. 7.
The crystallizer 4d of the fourth modification is different from the crystallizer 4a of the first modification in that the stirring blade W is a stirring blade Wd. In the following explanation, only the differences from the stirring blade W will be explained, and the explanation of the overlapping parts will be omitted.
The stirring blade Wd differs from the stirring blade W in that the disk portion 8 is provided at the upper end of the cylindrical portion 2, as shown in FIG. Further, the height of the cylindrical portion 2 is approximately half the height of the cylindrical portion 2 of the stirring blade W. The same effect as the crystallizer 4 provided with the stirring blade W can also be achieved by using the crystallizer 4d equipped with such a stirring blade Wd. Further, since the cylindrical portion 2 is not provided above the disk portion 8, the stirring blade Wd can be made lighter than the stirring blade W. Furthermore, since the stirring blade Wd can have a simple structure, the stirring blade Wd can be operated with less power than the stirring blade W, resulting in energy saving of the crystallizer 4 and easier manufacturing of the stirring blade Wd. can be expected. Furthermore, since the height of the cylindrical portion 2 is kept short, the crystallizer 4d can be downsized. Incidentally, a plurality of holes 9 (not shown) may be provided in the disk portion 8 to penetrate in the direction of the central axis O1. In that case, the same effects as in the case where the disk portion 8 of the stirring blade Wa is provided with a plurality of holes 9 penetrating in the direction of the central axis O1 can be expected.
　このような晶析装置４ｄを含む第４の変形例に係る晶析システム１０Ａ４によれば、晶析装置４ｄにおける反応生成物の粒子径、粒度分布、真球度などの粒子品質に影響を与える剪断力、第１の反応液Ｌ１の循環量、スラリの滞留時間を個別に調整することができ、より一層、粒子品質の制御性能を向上することができる。 According to the crystallization system 10A4 according to the fourth modification including such a crystallizer 4d, the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4d is affected. The shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
＜第１実施形態の第５の変形例＞
　以下、第１実施形態に係る晶析システム１０Ａの第５の変形例に係る晶析システム１０Ａ５を、図８を参照して説明する。
　第５の変形例の晶析装置４ｅでは、第１の変形例の晶析装置４ａの撹拌翼Ｗが撹拌翼Ｗｅである点に相違がある。以下の説明では、主に撹拌翼Ｗとの相違点のみ説明し、重複している箇所の説明は省略する。
　撹拌翼Ｗｅは、図８に示されるように、円柱状の円柱部２０と、円柱部２０の上端部に円柱部２０と同心状に設けられる円盤基部１８と、円盤基部１８の平面視の中心から中心軸Ｏ１に沿って上方に延びる回転軸３と、円柱部２０の径方向外側に円柱部２０と同心状に設けられる円筒状の多孔板１８Ｐと、を備えている。多孔板１８Ｐには多孔板１８Ｐを径方向に貫通する複数の孔１８ｈが設けられており、第１の反応液Ｌ１と第２の反応液Ｌ２と、その混合液は、複数の孔１８ｈを流通可能である。多孔板１８Ｐは、円盤基部１８の外縁から下方に延びている。回転軸３と円盤基部１８と円柱部２０とのそれぞれの内部に設けられる管路Ｐ１、Ｐ２、Ｐ３を第２の反応液が流通可能である。管路Ｐ１、Ｐ２、Ｐ３はそれぞれ連通している。管路Ｐ２は、管路Ｐ１の下端部から中心軸Ｏ１を中心に放射状に径方向外側に向かって延びている。管路Ｐ３は、管路Ｐ２の径方向外側の端部から中心軸Ｏ１に沿って下方に延びている。管路Ｐ２と管路Ｐ３は円柱部２０の内部に形成されている。円柱部２０の外周面２０ｏに上下方向に間隔を空けて複数の給液部５０ｂが設けられている。撹拌翼Ｗｅが回転すると、回転軸３と円盤基部１８と円柱部２０と多孔板１８Ｐとが一体に回転する。
　このような撹拌翼Ｗｅでは、円柱部２０の外周面２０ｏに上下方向に間隔を空けて設けられた複数の給液部５０ｂから第２の反応液Ｌ２が反応槽１内に供給され、反応槽１内の第１の反応液Ｌ１と混合し反応しながら、多孔板１８Ｐの複数の孔１８ｈを流通する。そのため、第１の反応液Ｌ１と第２の反応液Ｌ２とを、より均一に混合することができる。
　多孔板１８Ｐの複数の孔１８ｈを通過した混合液は、反応槽１の内周１ｉに衝突し、その後、反応槽１の内周面１ｉに沿って上下方向に移動する。下方に移動した混合液は、撹拌翼Ｗｅの回転により生じる遠心力に起因する径方向外側に向かう流れに引き寄せられて再び撹拌翼Ｗｅの多孔板１８Ｐの複数の孔１８ｈを通って反応槽１の内周面１ｉに衝突し、その後、反応槽１の内周面１ｉに沿って上下方向に移動することで対流が生まれる。ここで、複数の孔１８ｈを混合液が通過する際、絞り流路の効果により、混合液は径方向外側に加速されるので、混合液の径方向外向きの流速は、複数の孔１８ｈ近傍で最も高い。さらに、５ｍ／秒以上５０ｍ／秒以下の周速で回転する撹拌翼Ｗｅの円柱部２０の外周面２０ｏ及び多孔板１８Ｐの内外周面と、固定されている反応槽１の内周面１ｉとの間に存在する混合液には、周方向に剪断力が与えられる。混合液に与えられる剪断力は撹拌翼Ｗｅの円柱部２０の外周面２ｏと多孔板１８Ｐの内外周面に近ければ近い程大きい。混合液に与えられる剪断力は、得られる粒子の粒子径と均一性を決定する大きな要因となる。特に与えられる剪断力が大きければ大きい程、微細な粒子径を持つ粒子を得ることができる。撹拌翼Ｗｅを用いた場合、撹拌翼Ｗを用いる場合よりも、剪断力の影響を混合液のより多くの箇所に与えることができるため、均一で微細な粒子を製造することができる。
　給液部５０ｂから供給される第２の反応液Ｌ２は、剪断力の最も高い撹拌翼Ｗｅの内外周、即ち、円柱部２０の外周面２０ｏ及び多孔板１８Ｐの内外周面から至近距離、例えば２ｍｍ以内、の範囲に供給することができる。
　図８の例では、給液部５０ｂが、円柱部２０の上下方向に４個設けられているが、給液部５０ｂの個数は図８の例に限定されず、反応槽１のサイズに応じて増減しても良い。 <Fifth modification of the first embodiment>
Hereinafter, a crystallization system 10A5 according to a fifth modification of the crystallization system 10A according to the first embodiment will be described with reference to FIG. 8.
The crystallizer 4e of the fifth modification is different from the crystallizer 4a of the first modification in that the stirring blade W is a stirring blade We. In the following explanation, only the differences from the stirring blade W will be mainly explained, and the explanation of the overlapping parts will be omitted.
As shown in FIG. 8, the stirring blade We includes a cylindrical columnar section 20, a disk base 18 provided concentrically with the columnar section 20 at the upper end of the columnar section 20, and a center of the disk base 18 in a plan view. The rotating shaft 3 extends upward along the central axis O1 from the center, and a cylindrical perforated plate 18P provided concentrically with the cylindrical portion 20 on the outside in the radial direction of the cylindrical portion 20. The porous plate 18P is provided with a plurality of holes 18h that penetrate the porous plate 18P in the radial direction, and the first reaction liquid L1, the second reaction liquid L2, and the mixed liquid flow through the plurality of holes 18h. It is possible. The porous plate 18P extends downward from the outer edge of the disc base 18. The second reaction liquid can flow through the pipes P1, P2, and P3 provided inside the rotating shaft 3, the disc base 18, and the cylindrical part 20, respectively. The pipes P1, P2, and P3 are in communication with each other. The pipe P2 extends radially outward from the lower end of the pipe P1 about the central axis O1. The pipe P3 extends downward from the radially outer end of the pipe P2 along the central axis O1. Pipe line P2 and pipe line P3 are formed inside the cylindrical part 20. A plurality of liquid supply parts 50b are provided on the outer peripheral surface 20o of the columnar part 20 at intervals in the vertical direction. When the stirring blade We rotates, the rotating shaft 3, the disc base 18, the cylindrical part 20, and the perforated plate 18P rotate together.
In such a stirring blade We, the second reaction liquid L2 is supplied into the reaction tank 1 from the plurality of liquid supply parts 50b provided at intervals in the vertical direction on the outer peripheral surface 20o of the columnar part 20, and the second reaction liquid L2 is supplied into the reaction tank 1. It flows through the plurality of holes 18h of the porous plate 18P while mixing and reacting with the first reaction liquid L1 in the porous plate 18P. Therefore, the first reaction liquid L1 and the second reaction liquid L2 can be mixed more uniformly.
The mixed liquid that has passed through the plurality of holes 18h of the porous plate 18P collides with the inner circumference 1i of the reaction tank 1, and then moves in the vertical direction along the inner circumference 1i of the reaction vessel 1. The mixed liquid that has moved downward is drawn by the radially outward flow caused by the centrifugal force generated by the rotation of the stirring blade We, and passes through the plurality of holes 18h of the perforated plate 18P of the stirring blade We again to the reaction tank 1. Convection is generated by colliding with the inner circumferential surface 1i and then moving vertically along the inner circumferential surface 1i of the reaction tank 1. Here, when the mixed liquid passes through the plurality of holes 18h, the mixed liquid is accelerated radially outward due to the effect of the throttle channel, so the flow velocity of the mixed liquid outward in the radial direction is reduced near the plurality of holes 18h. highest in Furthermore, the outer circumferential surface 20o of the cylindrical part 20 of the stirring blade We rotating at a circumferential speed of 5 m/sec to 50 m/sec, the inner circumferential surface of the perforated plate 18P, and the inner circumferential surface 1i of the fixed reaction tank 1. A shearing force is applied in the circumferential direction to the liquid mixture existing between the two. The shearing force applied to the mixed liquid is greater as the shearing force is closer 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 perforated plate 18P. The shearing force applied to the liquid mixture is a major factor in determining the particle size and uniformity of the resulting particles. In particular, the larger the applied shearing force, the more fine the particles can be obtained. When using the stirring blade We, the influence of shear force can be applied to more parts of the liquid mixture than when using the stirring blade W, so that uniform and fine particles can be produced.
The second reaction liquid L2 supplied from the liquid supply part 50b is at a close distance from the inner and outer circumferences of the stirring blade We having the highest shearing force, that is, the outer circumferential surface 20o of the columnar part 20 and the inner and outer circumferential surfaces of the perforated plate 18P, for example. It can be supplied within a range of 2 mm or less.
In the example of FIG. 8, four liquid supply parts 50b are provided in the vertical direction of the columnar part 20, but the number of liquid supply parts 50b is not limited to the example of FIG. It may be increased or decreased.
　このような晶析装置４ｅを含む第５の変形例に係る晶析システム１０Ａ５によれば、晶析装置４ｅにおける反応生成物の粒子径、粒度分布、真球度などの粒子品質に影響を与える剪断力、第１の反応液Ｌ１の循環量、スラリの滞留時間を個別に調整することができ、より一層、粒子品質の制御性能を向上することができる。 According to the crystallization system 10A5 according to the fifth modification including such a crystallizer 4e, the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4e is affected. The shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
＜第１実施形態の第６の変形例＞
　以下、第１実施形態に係る晶析システム１０Ａの第６の変形例に係る晶析システム１０Ａ６を、図９を参照して説明する。
　第６の変形例の晶析装置４ｆでは、第１の変形例の晶析装置４ａの撹拌翼Ｗが撹拌翼Ｗｆである点に相違がある。以下の説明では、主に撹拌翼Ｗとの相違点のみ説明し、重複している箇所の説明は省略する。
　撹拌翼Ｗｆは、図９に示されるように、円柱状の円柱部２０と、円柱部２０の平面視の中心から中心軸Ｏ１に沿って上方に延びる回転軸３と、円柱部２０の径方向外側に円柱部２０と同心状に設けられる円筒状の多孔板１８Ｐと、を備えている。多孔板１８Ｐには多孔板１８Ｐを径方向に貫通する複数の孔１８ｈが設けられており、第１の反応液Ｌ１と第２の反応液Ｌ２と、その混合液は、複数の孔１８ｈを流通可能である。多孔板１８Ｐは、円柱部２０の外周面２ｏから径方向外側に延びる接続棒１１に固定されている。回転軸３と円柱部２０のそれぞれの内部に設けられる管路Ｐ１、Ｐ２、Ｐ３を第２の反応液が流通可能である。管路Ｐ１、Ｐ２、Ｐ３はそれぞれ連通している。管路Ｐ２は、管路Ｐ１の下端部から中心軸Ｏ１を中心に放射状に径方向外側に向かって延びている。管路Ｐ３は、管路Ｐ２の径方向外側の端部から中心軸Ｏ１に沿って下方に延びている。管路Ｐ２と管路Ｐ３は円柱部２０の内部に形成されている。円柱部２０の外周面２０ｏに上下方向に間隔を空けて複数の給液部５０ｂが設けられている。撹拌翼Ｗｆが回転すると、回転軸３と円柱部２０と接続棒１１と多孔板１８Ｐとが一体に回転する。接続棒１１は、円柱部２０の周方向に等間隔を空けて複数設けられている。接続棒１１は２個以上設けられていることが好ましい。接続棒１１は円柱部２０の高さの概ね半分の位置に設けられているが、この例に限定されず、円柱部２０の高さの概ね半分より上側か下側に設けられていても良い。
　このような撹拌翼Ｗｆでは、円柱部２０の外周面２０ｏに上下方向に間隔を空けて設けられた複数の給液部５０ｂから第２の反応液Ｌ２が反応槽１内に供給され、反応槽１内の第１の反応液Ｌ１と混合し反応しながら、多孔板１８Ｐの複数の孔１８ｈを流通する。そのため、第１の反応液Ｌ１と第２の反応液Ｌ２とを、より均一に混合することができる。
　多孔板１８Ｐの複数の孔１８ｈを通過した混合液は、反応槽１の内周１ｉに衝突し、その後、反応槽１の内周面１ｉに沿って上下方向に移動する。上下方向に移動した混合液は、撹拌翼Ｗｆの回転により生じる遠心力に起因する径方向外側に向かう流れに引き寄せられて再び撹拌翼Ｗｆの多孔板１８Ｐの複数の孔１８ｈを通って反応槽１の内周面１ｉに衝突し、その後、反応槽１の内周面１ｉに沿って上下方向に移動することで対流が生まれる。ここで、複数の孔１８ｈを混合液が通過する際、絞り流路の効果により、混合液は径方向外側に加速されるので、混合液の径方向外向きの流速は、複数の孔１８ｈ近傍で最も高い。さらに、５ｍ／秒以上５０ｍ／秒以下の周速で回転する撹拌翼Ｗｆの円柱部２０の外周面２０ｏ及び多孔板１８Ｐの内外周面と、固定されている反応槽１の内周面１ｉとの間に存在する混合液には、周方向に剪断力が与えられる。混合液に与えられる剪断力は撹拌翼Ｗｆの円柱部２０の外周面２ｏと多孔板１８Ｐの内外周面に近ければ近い程大きい。混合液に与えられる剪断力は、得られる粒子の粒子径と均一性を決定する大きな要因となる。特に与えられる剪断力が大きければ大きい程、微細な粒子径を持つ粒子を得ることができる。撹拌翼Ｗｆを用いた場合、剪断力の影響を混合液のより多くの箇所に与えることができるため、均一で微細な粒子を製造することができる。
　給液部５０ｂから供給される第２の反応液Ｌ２は、剪断力の最も高い撹拌翼Ｗｆの内外周、即ち、円柱部２０の外周面２０ｏ及び多孔板１８Ｐの内外周面から至近距離、例えば２ｍｍ以内、の範囲に供給することができる。
　図９の例では、給液部５０ｂが、円柱部２０の上下方向に４個設けられているが、給液部５０ｂの個数は図１０の例に限定されず、反応槽１のサイズに応じて増減しても良い。 <Sixth modification of the first embodiment>
Hereinafter, a crystallization system 10A6 according to a sixth modification of the crystallization system 10A according to the first embodiment will be described with reference to FIG. 9.
The crystallizer 4f of the sixth modification is different from the crystallizer 4a of the first modification in that the stirring blade W is a stirring blade Wf. In the following explanation, only the differences from the stirring blade W will be mainly explained, and the explanation of the overlapping parts will be omitted.
As shown in FIG. 9, the stirring blade Wf includes a cylindrical columnar section 20, a rotating shaft 3 extending upward from the center of the columnar section 20 in plan view along the central axis O1, and a radial direction of the columnar section 20. It includes a cylindrical perforated plate 18P provided on the outside concentrically with the columnar part 20. The porous plate 18P is provided with a plurality of holes 18h that penetrate the porous plate 18P in the radial direction, and the first reaction liquid L1, the second reaction liquid L2, and the mixed liquid flow through the plurality of holes 18h. It is possible. The porous plate 18P is fixed to the connecting rod 11 extending radially outward from the outer circumferential surface 2o of the cylindrical portion 20. The second reaction liquid can flow through the pipes P1, P2, and P3 provided inside the rotating shaft 3 and the cylindrical portion 20, respectively. The pipes P1, P2, and P3 are in communication with each other. The pipe P2 extends radially outward from the lower end of the pipe P1 about the central axis O1. The pipe P3 extends downward from the radially outer end of the pipe P2 along the central axis O1. Pipe line P2 and pipe line P3 are formed inside the cylindrical part 20. A plurality of liquid supply parts 50b are provided on the outer peripheral surface 20o of the columnar part 20 at intervals in the vertical direction. When the stirring blade Wf rotates, the rotating shaft 3, the cylindrical portion 20, the connecting rod 11, and the perforated plate 18P rotate together. A plurality of connecting rods 11 are provided at equal intervals in the circumferential direction of the cylindrical portion 20 . It is preferable that two or more connecting rods 11 are provided. Although the connecting rod 11 is provided at a position approximately half the height of the cylindrical portion 20, the connection rod 11 is not limited to this example, and may be provided above or below approximately half the height of the cylindrical portion 20. .
In such a stirring blade Wf, the second reaction liquid L2 is supplied into the reaction tank 1 from a plurality of liquid supply parts 50b provided at intervals in the vertical direction on the outer circumferential surface 20o of the columnar part 20, and the second reaction liquid L2 is supplied into the reaction tank 1. It flows through the plurality of holes 18h of the porous plate 18P while mixing and reacting with the first reaction liquid L1 in the porous plate 18P. Therefore, the first reaction liquid L1 and the second reaction liquid L2 can be mixed more uniformly.
The mixed liquid that has passed through the plurality of holes 18h of the porous plate 18P collides with the inner circumference 1i of the reaction tank 1, and then moves in the vertical direction along the inner circumference 1i of the reaction vessel 1. The mixed liquid that has moved in the vertical direction is attracted by the flow directed outward in the radial direction due to the centrifugal force generated by the rotation of the stirring blade Wf, and passes through the plurality of holes 18h of the perforated plate 18P of the stirring blade Wf again to the reaction tank 1. The reaction vessel 1 collides with the inner circumferential surface 1i of the reactor 1, and then moves vertically along the inner circumferential surface 1i of the reaction tank 1, thereby generating convection. Here, when the mixed liquid passes through the plurality of holes 18h, the mixed liquid is accelerated radially outward due to the effect of the throttle channel, so the flow velocity of the mixed liquid outward in the radial direction is reduced near the plurality of holes 18h. highest in Furthermore, the outer circumferential surface 20o of the columnar part 20 of the stirring blade Wf rotating at a circumferential speed of 5 m/sec to 50 m/sec, the inner circumferential surface of the perforated plate 18P, and the inner circumferential surface 1i of the fixed reaction tank 1. A shearing force is applied in the circumferential direction to the liquid mixture existing between the two. The shearing force applied to the mixed liquid increases as the shearing force approaches the outer circumferential surface 2o of the cylindrical portion 20 of the stirring blade Wf and the inner and outer circumferential surfaces of the perforated plate 18P. The shearing force applied to the liquid mixture is a major factor in determining the particle size and uniformity of the resulting particles. In particular, the greater the applied shearing force, the finer the particle size can be obtained. When the stirring blade Wf is used, the influence of shear force can be applied to more parts of the liquid mixture, so that uniform and fine particles can be produced.
The second reaction liquid L2 supplied from the liquid supply part 50b is at a close distance from the inner and outer circumferences of the stirring blade Wf having the highest shearing force, that is, the outer circumferential surface 20o of the columnar part 20 and the inner and outer circumferential surfaces of the perforated plate 18P, for example. It can be supplied within a range of 2 mm or less.
In the example of FIG. 9, four liquid supply parts 50b are provided in the vertical direction of the columnar part 20, but the number of liquid supply parts 50b is not limited to the example of FIG. It may be increased or decreased.
　このような晶析装置４ｆを含む第６の変形例に係る晶析システム１０Ａ６によれば、晶析装置４ｆにおける反応生成物の粒子径、粒度分布、真球度などの粒子品質に影響を与える剪断力、第１の反応液Ｌ１の循環量、スラリの滞留時間を個別に調整することができ、より一層、粒子品質の制御性能を向上することができる。 According to the crystallization system 10A6 according to the sixth modification including such a crystallizer 4f, the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4f is affected. The shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
＜第１実施形態の第７の変形例＞
　以下、第１実施形態に係る晶析システム１０Ａの第７の変形例に係る晶析システム１０Ａ７を、図１０を参照して説明する。
　第７の変形例の晶析装置４ｇでは、第５の変形例の晶析装置４ｅの撹拌翼Ｗｅが撹拌翼Ｗｇである点に相違がある。以下の説明では、撹拌翼Ｗｅとの相違点のみ説明し、重複している箇所の説明は省略する。
　撹拌翼Ｗｇは、図１０に示されるように、第５の変形例の撹拌翼Ｗｅよりも、円柱部２の外周面２０ｏと多孔板１８Ｐの内周面との間隔が広い。また、撹拌翼Ｗｅにおける、径方向外側に開口する給液部５０ｂから、さらに径方向外側に延びる延長管１２が設けられており、延長管１２の先端が給液部５０ｂとされている。
　このような撹拌翼Ｗｇによれば、円柱部２０の外周面２０ｏと多孔板１８Ｐの内周面との間隔を広くすることができるので、円柱部２０と多孔板１８Ｐとの間に、第１の反応液Ｌ１と、第２の反応液Ｌ２と、これらの混合液と、が流入し易くなる。そのため、反応液の循環を促進させることができるので、均一で微細な粒子を製造することができる。また、給液部５０ｂから供給される第２の反応液Ｌ２は、剪断力の最も高い撹拌翼Ｗｇの内外周、即ち、多孔板１８Ｐの内外周面から至近距離、例えば２ｍｍ以内、の範囲に供給することができる。 <Seventh modification of the first embodiment>
Hereinafter, a crystallization system 10A7 according to a seventh modification of the crystallization system 10A according to the first embodiment will be described with reference to FIG. 10.
The crystallizer 4g of the seventh modification is different from the crystallizer 4e of the fifth modification in that the stirring blade We is a stirring blade Wg. In the following explanation, only the differences from the stirring blade We will be explained, and the explanation of the overlapping parts will be omitted.
As shown in FIG. 10, the stirring blade Wg has a wider distance between the outer peripheral surface 20o of the columnar part 2 and the inner peripheral surface of the perforated plate 18P than the stirring blade We of the fifth modification. Further, an extension pipe 12 is provided that extends further radially outward from a liquid supply part 50b that opens radially outward in the stirring blade We, and the tip of the extension pipe 12 is the liquid supply part 50b.
According to such a stirring blade Wg, the distance between the outer circumferential surface 20o of the columnar part 20 and the inner circumferential surface of the perforated plate 18P can be widened, so that the first The reaction liquid L1, the second reaction liquid L2, and a mixed liquid thereof become easier to flow in. Therefore, circulation of the reaction solution can be promoted, and uniform and fine particles can be produced. Further, the second reaction liquid L2 supplied from the liquid supply part 50b is delivered to the inner and outer periphery of the stirring blade Wg having the highest shearing force, that is, within a close distance, for example, within 2 mm, from the inner and outer periphery of the perforated plate 18P. can be supplied.
　このような晶析装置４ｇを含む第７の変形例に係る晶析システム１０Ａ７によれば、晶析装置４ｇにおける反応生成物の粒子径、粒度分布、真球度などの粒子品質に影響を与える剪断力、第１の反応液Ｌ１の循環量、スラリの滞留時間を個別に調整することができ、より一層、粒子品質の制御性能を向上することができる。 According to the crystallization system 10A7 according to the seventh modification including such a crystallizer 4g, the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4g is affected. The shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
＜第１実施形態の第８の変形例＞
　以下、第１実施形態に係る晶析システム１０Ａの第８の変形例に係る晶析システム１０Ａ８を、図１１を参照して説明する。
　第８の変形例の晶析装置４ｈでは、第６の変形例の晶析装置４ｆの撹拌翼Ｗｆが撹拌翼Ｗｈである点に相違がある。以下の説明では、撹拌翼Ｗｆとの相違点のみ説明し、重複している箇所の説明は省略する。
　撹拌翼Ｗｈは、図１１に示されるように、第８の変形例の撹拌翼Ｗｆよりも、円柱部２０の外周面２０ｏと多孔板１８Ｐとの間隔が広い。また、撹拌翼Ｗｆにおける、径方向外側に開口する給液部５０ｂから、さらに径方向外側に延びる延長管１２が設けられており、延長管１２の先端が給液部５０ｂとされている。
　このような撹拌翼Ｗｈによれば、円柱部２０の外周面２０ｏと多孔板１８Ｐの内周面との間隔を広くすることができるので、円柱部２０と多孔板１８Ｐとの間に、第１の反応液Ｌ１と、第２の反応液Ｌ２と、これらの混合液と、が流入し易くなる。そのため、反応液の循環を促進させることができるので、均一で微細な粒子を製造することができる。また、給液部５０ｂから供給される第２の反応液Ｌ２は、剪断力の最も高い撹拌翼Ｗｇの内外周、即ち、多孔板１８Ｐの内外周面から至近距離、例えば２ｍｍ以内、の範囲に供給することができる。 <Eighth modification of the first embodiment>
Hereinafter, a crystallization system 10A8 according to an eighth modification of the crystallization system 10A according to the first embodiment will be described with reference to FIG. 11.
The crystallizer 4h of the eighth modification is different from the crystallizer 4f of the sixth modification in that the stirring blade Wf is a stirring blade Wh. In the following explanation, only the differences from the stirring blade Wf will be explained, and the explanation of the overlapping parts will be omitted.
As shown in FIG. 11, the stirring blade Wh has a wider distance between the outer circumferential surface 20o of the columnar part 20 and the perforated plate 18P than the stirring blade Wf of the eighth modification. Furthermore, an extension tube 12 is provided that extends further radially outward from a liquid supply section 50b that opens radially outward in the stirring blade Wf, and the tip of the extension tube 12 is the liquid supply section 50b.
According to such a stirring blade Wh, since the distance between the outer circumferential surface 20o of the columnar part 20 and the inner circumferential surface of the perforated plate 18P can be widened, the first The reaction liquid L1, the second reaction liquid L2, and a mixed liquid thereof become easier to flow in. Therefore, circulation of the reaction solution can be promoted, and uniform and fine particles can be produced. Further, the second reaction liquid L2 supplied from the liquid supply part 50b is delivered to the inner and outer periphery of the stirring blade Wg having the highest shearing force, that is, within a close distance, for example, within 2 mm, from the inner and outer periphery of the perforated plate 18P. can be supplied.
　このような晶析装置４ｈを含む第８の変形例に係る晶析システム１０Ａ８によれば、晶析装置４ｈにおける反応生成物の粒子径、粒度分布、真球度などの粒子品質に影響を与える剪断力、第１の反応液Ｌ１の循環量、スラリの滞留時間を個別に調整することができ、より一層、粒子品質の制御性能を向上することができる。 According to the crystallization system 10A8 according to the eighth modification including such a crystallizer 4h, the particle quality such as the particle size, particle size distribution, and sphericity of the reaction product in the crystallizer 4h is affected. The shearing force, the circulation amount of the first reaction liquid L1, and the residence time of the slurry can be adjusted individually, and the control performance of particle quality can be further improved.
　上記の変形例のうち、給液部５ｂが下方に開口している、第１実施形態に係る晶析装置４の撹拌翼Ｗｃ、第１の変形例に係る晶析装置４ａの撹拌翼Ｗ、及び、第４の変形例に係る晶析装置４ｄの撹拌翼Ｗｄでは、第１の反応液Ｌ１と第２の反応液Ｌ２とを、より均一に混合することができる。 Among the above modifications, the stirring blade Wc of the crystallizer 4 according to the first embodiment, the stirring blade W of the crystallizer 4a according to the first modification, in which the liquid supply part 5b is open downward, Further, in the stirring blade Wd of the crystallizer 4d according to the fourth modification, the first reaction liquid L1 and the second reaction liquid L2 can be mixed more uniformly.
＜晶析方法＞
　なお、上記実施形態と変形例に記載される晶析システムを使用することで粒子を生成することを、晶析方法として見なすことができる。 <Crystallization method>
Note that generating particles by using the crystallization system described in the above embodiments and modifications can be regarded as a crystallization method.
　例えば、第１実施形態の晶析システム１０Ａは、複数の原料溶液を混合して前記複数の原料溶液の中の複数の原料に由来する粒子を晶析装置４で成長させる晶析ステップと、晶析装置４の排出口６から排出される粒子を含むスラリＤ１を、蛇行形状をなす屈曲部Ｐｐを有する循環管路Ｐｏを流動させることで晶析装置４の導入口５ａまで循環させる循環ステップと、を含む晶析方法と見なすことができる。このような晶析方法によれば、第１実施形態の晶析装置システム１０Ａと同様の効果を得ることができる。 For example, the crystallization system 10A of the first embodiment includes a crystallization step in which a plurality of raw material solutions are mixed and particles derived from a plurality of raw materials in the plurality of raw material solutions are grown in the crystallizer 4; a circulation step in which the slurry D1 containing particles discharged from the discharge port 6 of the crystallizer 4 is circulated to the inlet 5a of the crystallizer 4 by flowing the circulation pipe Po having a meandering bent portion Pp; It can be considered as a crystallization method including . According to such a crystallization method, effects similar to those of the crystallizer system 10A of the first embodiment can be obtained.
　さらに、第１実施形態の晶析システム１０Ａは、晶析システム１０Ａにおいて、循環管路Ｐｏの内径が一定である晶析方法と見なすことができる。このような晶析方法によれば、第１実施形態の晶析システム１０Ａと同様の効果を得ることができる。 Further, the crystallization system 10A of the first embodiment can be considered as a crystallization method in which the inner diameter of the circulation pipe Po is constant. According to such a crystallization method, effects similar to those of the crystallization system 10A of the first embodiment can be obtained.
　さらに、第２実施形態の晶析システム１０Ｂは、晶析システム１０Ａにおいて、屈曲部Ｐｐが複数設けられている晶析方法と見なすことができる。このような晶析方法によれば、第２実施形態の晶析システム１０Ｂと同様の効果を得ることができる。 Furthermore, the crystallization system 10B of the second embodiment can be considered as a crystallization method in which a plurality of bent portions Pp are provided in the crystallization system 10A. According to such a crystallization method, effects similar to those of the crystallization system 10B of the second embodiment can be obtained.
　さらに、第３実施形態の晶析システム１０Ｃは、晶析システム１０Ａにおいて、屈曲部Ｐｐの少なくとも一部が温度調節槽の中に設けられている晶析方法と見なすことができる。このような晶析方法によれば、第３実施形態の晶析システム１０Ｃと同様の効果を得ることができる。 Furthermore, the crystallization system 10C of the third embodiment can be considered as a crystallization method in which at least a portion of the bent portion Pp is provided in the temperature control tank in the crystallization system 10A. According to such a crystallization method, effects similar to those of the crystallization system 10C of the third embodiment can be obtained.
　さらに、第１実施形態の晶析システム１０Ａは、屈曲部Ｐｐが、分離可能な、複数の直管部と複数の曲管部Ｃと、から構成されている晶析方法と見なすことができる。このような晶析方法によれば、第１実施形態の晶析システム１０Ａと同様の効果を得ることができる。 Further, the crystallization system 10A of the first embodiment can be regarded as a crystallization method in which the bent portion Pp is composed of a plurality of separable straight pipe portions and a plurality of bent pipe portions C. According to such a crystallization method, effects similar to those of the crystallization system 10A of the first embodiment can be obtained.
　さらに、第１実施形態の晶析システム１０Ａの第１の変形例に係る晶析システム１０Ａ１は、晶析システム１０Ａにおいて、晶析装置４ａが、径方向に貫通する複数の孔ｈを備えるとともに中心軸Ｏ１回りに回転する撹拌翼Ｗと、この撹拌翼Ｗを同心状に内部に収容する有底円筒状の反応槽１と、この反応槽１の内部に第１の反応液Ｌ１を供給する導入口５ａと、撹拌翼Ｗに設けられるとともに第２の反応液Ｌ２を反応槽１の内部に供給可能な給液部５ｂと、を備え、第１の反応液Ｌ１を導入口５ａから反応槽１に供給する第１給液ステップと、第２の反応液Ｌ２を給液部５ｂから反応槽１に供給する第２給液ステップと、を備える晶析方法と見なすことができる。このような晶析方法によれば、第１実施形態の晶析システム１０Ａの第１の変形例に係る晶析システム１０Ａ１と同様の効果を得ることができる。 Furthermore, in the crystallization system 10A1 according to the first modification of the crystallization system 10A of the first embodiment, in the crystallization system 10A, the crystallizer 4a is provided with a plurality of holes h penetrating in the radial direction, and a central A stirring blade W rotating around an axis O1, a cylindrical reaction tank 1 with a bottom that concentrically accommodates the stirring blade W, and an introduction for supplying a first reaction liquid L1 into the reaction tank 1. The first reaction liquid L1 is supplied from the inlet 5a to the reaction tank 1. This can be regarded as a crystallization method comprising a first liquid supply step of supplying the second reaction liquid L2 to the reaction tank 1 from the liquid supply part 5b. According to such a crystallization method, effects similar to those of the crystallization system 10A1 according to the first modification of the crystallization system 10A of the first embodiment can be obtained.
　さらに、第１実施形態の晶析システム１０Ａの第１の変形例に係る晶析システム１０Ａ１は、晶析システム１０Ａ１において、撹拌翼Ｗが、円筒状の円筒部２と、円筒部２の内周面に外縁部が固定される円盤状の円盤部８と、円盤部８の平面視の中心から中心軸Ｏ１に沿って上方に延びる回転軸３と、をさらに備え、円盤部８と回転軸Ｏ１との内部を第２の反応液Ｌ２が流通可能であり、第２給液ステップでは円盤部８の外縁部から下方に向けて第２の反応液Ｌ２を供給する晶析方法と見なすことができる。このような晶析方法によれば、第１実施形態の晶析システム１０Ａの第１の変形例に係る晶析システム１０Ａ１と同様の効果を得ることができる。 Furthermore, in the crystallization system 10A1 according to the first modification of the crystallization system 10A of the first embodiment, the stirring blade W is connected to the cylindrical portion 2 and the inner periphery of the cylindrical portion 2. It further includes a disc-shaped disc part 8 whose outer edge is fixed to a surface, and a rotating shaft 3 extending upward from the center of the disc part 8 in plan view along the central axis O1, and the disc part 8 and the rotating shaft O1 The second reaction liquid L2 can flow through the inside of the disk, and the second liquid supply step can be considered as a crystallization method in which the second reaction liquid L2 is supplied downward from the outer edge of the disk part 8. . According to such a crystallization method, effects similar to those of the crystallization system 10A1 according to the first modification of the crystallization system 10A of the first embodiment can be obtained.
　さらに、第１実施形態の晶析システム１０Ａの第２の変形例に係る晶析システム１０Ａ２は、第１実施形態の晶析システム１０Ａの第１の変形例に係る晶析システム１０Ａ１において、撹拌翼Ｗは、円筒状の円筒部２と、円筒部２の内周面２ｉに外縁部が固定される円盤状の円盤部８と、円盤部８の平面視の中心から中心軸に沿って上方に延びる回転軸Ｏ１と、をさらに備え、円盤部８と回転軸Ｏ１との内部を第２の反応液Ｌ２が流通可能であり、第２給液ステップでは円盤部８の外縁部から円筒部２を貫通して径方向外側に向けて第２の反応液Ｌ２を供給する晶析方法と見なすことができる。このような晶析方法によれば、第１実施形態の晶析システム１０Ａの第２の変形例に係る晶析システム１０Ａ２と同様の効果を得ることができる。 Furthermore, the crystallization system 10A2 according to the second modification of the crystallization system 10A of the first embodiment has a stirring blade in the crystallization system 10A1 according to the first modification of the crystallization system 10A of the first embodiment. W includes a cylindrical cylindrical part 2, a disc-shaped disc part 8 whose outer edge is fixed to the inner circumferential surface 2i of the cylindrical part 2, and a part W extending upward along the central axis from the center of the disc part 8 in a plan view. The second reaction liquid L2 can flow through the interior of the disc part 8 and the rotating shaft O1, and in the second liquid supply step, the cylindrical part 2 is supplied from the outer edge of the disc part 8. This can be considered as a crystallization method in which the second reaction liquid L2 is supplied radially outward through the hole. According to such a crystallization method, the same effects as the crystallization system 10A2 according to the second modification of the crystallization system 10A of the first embodiment can be obtained.
　さらに、第１実施形態の晶析システム１０Ａ、及び第１実施形態の晶析システム１０Ａの第３の変形例に係る晶析システム１０Ａ３は、第１実施形態の晶析システム１０Ａの第１の変形例の晶析システム１０Ａ１の撹拌翼Ｗ、及び第１実施形態の晶析システム１０Ａの第２の変形例の晶析システム１０Ａ２の撹拌翼Ｗａにおいて、円盤部８より上側の円筒部２において、径方向に貫通する複数の孔ｈがない（閉塞されている）とともに、円筒部２の内周面に外縁部が固定される円盤状の第２円盤部１５が円筒部２の上端部に設けられている晶析方法と見なすことができる。このような晶析方法によれば、第１実施形態の晶析システム１０Ａ、及び第１実施形態の晶析システム１０Ａの第３の変形例に係る晶析システム１０Ａ３と同様の効果を得ることができる。 Furthermore, the crystallization system 10A of the first embodiment and the crystallization system 10A3 according to the third modification of the crystallization system 10A of the first embodiment are the first modification of the crystallization system 10A of the first embodiment. In the stirring blade W of the example crystallization system 10A1 and the stirring blade Wa of the crystallization system 10A2 of the second modification of the crystallization system 10A of the first embodiment, in the cylindrical part 2 above the disk part 8, the diameter A second disc part 15 is provided at the upper end of the cylindrical part 2, and the plurality of holes h penetrating in the direction are not (closed), and the outer edge part is fixed to the inner circumferential surface of the cylindrical part 2. It can be regarded as a crystallization method that According to such a crystallization method, it is possible to obtain the same effects as the crystallization system 10A of the first embodiment and the crystallization system 10A3 according to the third modification of the crystallization system 10A of the first embodiment. can.
　さらに、第１実施形態の晶析システム１０Ａの第４の変形例に係る晶析システム１０Ａ４は、第１実施形態の晶析システム１０Ａの第１の変形例の晶析システム１０Ａ１の撹拌翼Ｗにおいて、円盤部８が撹拌翼Ｗの上端部に設けられる晶析方法と見なすことができる。このような晶析方法によれば、第１実施形態の晶析システム１０Ａの第４の変形例に係る晶析システム１０Ａ４と同様の効果を得ることができる。 Further, in the crystallization system 10A4 according to the fourth modification of the crystallization system 10A of the first embodiment, in the stirring blade W of the crystallization system 10A1 of the first modification of the crystallization system 10A of the first embodiment, This can be considered as a crystallization method in which the disk portion 8 is provided at the upper end of the stirring blade W. According to such a crystallization method, the same effects as the crystallization system 10A4 according to the fourth modification of the crystallization system 10A of the first embodiment can be obtained.
　さらに、第１実施形態の晶析システム１０Ａの第５の変形例に係る晶析システム１０Ａ５は、第１実施形態の晶析システム１０Ａの第１の変形例に係る晶析システム１０Ａ１において、撹拌翼Ｗが、円柱状の円柱部２０と、円柱部２０の上端部に前記円柱部２０と同心状に設けられる円盤基部１８と、円盤基部１８の平面視の中心から中心軸Ｏ１に沿って上方に延びる回転軸３と、円柱部２０の径方向外側に円柱部２０と同心状に設けられる円筒状の多孔板１８Ｐと、を備え、多孔板１８Ｐは、円盤基部１８の外縁から下方に延びており、回転軸Ｏ１と円盤基部１８と円柱部２０との内部を第２の反応液Ｌ２が流通可能であり、第２給液ステップでは、円柱部２０の外周面２０ｏに上下方向に間隔を空けて設けられた複数の給液部５０ｂから径方向外側に向けて第２の反応液Ｌ２を供給する晶析方法と見なすことができる。このような晶析方法によれば、第１実施形態の晶析システム１０Ａの第５の変形例に係る晶析システム１０Ａ４と同様の効果を得ることができる。 Furthermore, the crystallization system 10A5 according to the fifth modification of the crystallization system 10A of the first embodiment has a stirring blade in the crystallization system 10A1 according to the first modification of the crystallization system 10A of the first embodiment. W extends upward along the central axis O1 from the center of the circular columnar part 20, the disk base 18 provided at the upper end of the circular column part 20 concentrically with the columnar part 20, and the disk base 18 in plan view. It includes an extending rotating shaft 3 and a cylindrical perforated plate 18P provided concentrically with the cylindrical part 20 on the outside in the radial direction of the cylindrical part 20, and the perforated plate 18P extends downward from the outer edge of the disc base 18. , the second reaction liquid L2 can flow through the interior of the rotating shaft O1, the disc base 18, and the cylindrical part 20, and in the second liquid supply step, the second reaction liquid L2 is formed on the outer circumferential surface 20o of the cylindrical part 20 at intervals in the vertical direction. This can be considered as a crystallization method in which the second reaction liquid L2 is supplied radially outward from a plurality of provided liquid supply parts 50b. According to such a crystallization method, effects similar to those of the crystallization system 10A4 according to the fifth modification of the crystallization system 10A of the first embodiment can be obtained.
　さらに、第１実施形態の晶析システム１０Ａの第６の変形例に係る晶析システム１０Ａ６は、第１実施形態の晶析システム１０Ａの第１の変形例に係る晶析システム１０Ａ１において、撹拌翼Ｗが、円柱状の円柱部２０と、円柱部２０の平面視の中心から中心軸Ｏ１に沿って上方に延びる回転軸３と、円柱部２０の径方向外側に円柱部２０と同心状に設けられる円筒状の多孔板１８Ｐと、を備え、多孔板１８Ｐは、円柱部２０の外周面２０ｏから径方向外側に延びる接続棒１１に固定されており、回転軸Ｏ１と円柱部２０との内部を第２の反応液Ｌ２が流通可能であり、第２給液ステップでは、円柱部２０の外周面２０ｏに上下方向に間隔を空けて設けられた複数の給液部５０ｂから径方向外側に向けて第２の反応液Ｌ２を供給する晶析方法と見なすことができる。このような晶析方法によれば、第１実施形態の晶析システム１０Ａの第６の変形例に係る晶析システム１０Ａ６と同様の効果を得ることができる。 Furthermore, the crystallization system 10A6 according to the sixth modification of the crystallization system 10A of the first embodiment has a stirring blade in the crystallization system 10A1 according to the first modification of the crystallization system 10A of the first embodiment. W is provided concentrically with the columnar section 20 on the radially outer side of the columnar section 20, and the rotating shaft 3 extending upward from the center of the columnar section 20 in plan view along the central axis O1. The perforated plate 18P is fixed to a connecting rod 11 extending radially outward from the outer circumferential surface 20o of the cylindrical part 20, and the perforated plate 18P is fixed to a connecting rod 11 extending radially outward from the outer peripheral surface 20o of the cylindrical part 20. The second reaction liquid L2 can flow, and in the second liquid supply step, the second reaction liquid L2 is distributed radially outward from a plurality of liquid supply parts 50b provided on the outer circumferential surface 20o of the columnar part 20 at intervals in the vertical direction. This can be considered as a crystallization method for supplying the second reaction solution L2. According to such a crystallization method, the same effects as the crystallization system 10A6 according to the sixth modification of the crystallization system 10A of the first embodiment can be obtained.
　さらに、第１実施形態の晶析システム１０Ａの第７の変形例に係る晶析システム１０Ａ７は、第１実施形態の晶析システム１０Ａの第５の変形例に係る晶析システム１０Ａ５、又は第１実施形態の晶析システム１０Ａの第６の変形例に係る晶析システム１０Ａ６において、複数の給液部５０ｂから径方向外側に向かって延びる延長管１２が設けられ、第２給液ステップでは、延長管１２の先端から第２の反応液Ｌ２を供給する晶析方法と見なすことができる。このような晶析方法によれば、第１実施形態の晶析システム１０Ａの第７の変形例に係る晶析システム１０Ａ７及び第８の変形例に係る晶析システム１０Ａ８と同様の効果を得ることができる。 Furthermore, the crystallization system 10A7 according to the seventh modification of the crystallization system 10A of the first embodiment is the crystallization system 10A5 according to the fifth modification of the crystallization system 10A of the first embodiment, or the first In a crystallization system 10A6 according to a sixth modification of the crystallization system 10A of the embodiment, extension pipes 12 extending radially outward from the plurality of liquid supply parts 50b are provided, and in the second liquid supply step, the extension pipes 12 are This can be considered as a crystallization method in which the second reaction liquid L2 is supplied from the tip of the tube 12. According to such a crystallization method, effects similar to those of the crystallization system 10A7 according to the seventh modification of the crystallization system 10A of the first embodiment and the crystallization system 10A8 according to the eighth modification can be obtained. I can do it.
　以上、この発明の実施形態とその変形例について図面を参照して詳述してきたが、具体的な構成はこの実施形態とその変形例に限られず、請求項に定義されるこの発明の範囲の設計等や実施形態と変形例の相互の組み合わせも含まれる。 The embodiments of this invention and their modifications have been described above in detail with reference to the drawings, but the specific configuration is not limited to this embodiment and its modifications, and is within the scope of the invention as defined in the claims. It also includes designs, etc., and mutual combinations of embodiments and modifications.
　例えば、上記実施形態では、第１の反応液Ｌ１と第２の反応液Ｌ２との２種類の反応液を混合させて生成物を得たが、３種類以上の反応液を混合させても良い。 For example, in the above embodiment, the product was obtained by mixing two types of reaction liquids, the first reaction liquid L1 and the second reaction liquid L2, but three or more types of reaction liquids may be mixed. .
　本発明の晶析システムおよび晶析方法によれば、滞留槽を必須とせずに、晶析装置で結晶化された微粒子を滞留させることができる。 According to the crystallization system and crystallization method of the present invention, fine particles crystallized in a crystallizer can be retained without requiring a retention tank.
　１　反応槽
　２　円筒部
　３　回転軸
　４　晶析装置
　５ａ　導入口
　５ｂ　給液部
　６　排出口
　８　円盤部
　９、ｈ　孔
　１０Ａ、１０Ｂ、１０Ｃ、１０Ａ１、１０Ａ２、１０Ａ３、１０Ａ４、１０Ａ５、１０Ａ６、１０Ａ７、１０Ａ８　晶析システム
　２２、２３、２４　配管
　３０　循環ポンプ
　３１　第２循環ポンプ
　Ｐｏ　循環管路
　Ｐｐ　屈曲部
　Ｐｏ１、Ｐｏ２、Ｐｏ３、Ｐｏ４、Ｐｏ５、Ｐｏ６　直管部
　Ｃ、Ｃ１、Ｃ２、Ｃ３、Ｃ４、Ｃ５　  曲管部
　Ｗ、Ｗａ、Ｗｂ、Ｗｃ、Ｗｄ、Ｗｅ、Ｗｆ、Ｗｇ、Ｗｈ　撹拌翼 1 Reaction tank 2 Cylindrical part 3 Rotating shaft 4 Crystallizer 5a Inlet 5b Liquid supply part 6 Outlet 8 Disk part 9, h Hole 10A, 10B, 10C, 10A1, 10A2, 10A3, 10A4, 10A5, 10A6, 10A7, 10A8 Crystallization system 22, 23, 24 Piping 30 Circulation pump 31 Second circulation pump Po Circulation pipe Pp Bent part Po1, Po2, Po3, Po4, Po5, Po6 Straight pipe part C, C 1 , C 2 , C 3 , C 4 , C 5 curved pipe section W, Wa, Wb, Wc, Wd, We, Wf, Wg, Wh Stirring blade

Claims (10)

  1. 　複数の原料溶液を混合して前記複数の原料溶液の中の複数の原料に由来する粒子を生成させる晶析装置と、
    　前記晶析装置の排出口から排出される前記粒子を含むスラリを流動させ前記晶析装置の導入口から前記晶析装置内に前記スラリを循環させる循環管路と、
    　前記スラリを前記晶析装置と前記循環管路との間で循環させる循環ポンプと、を備え、
    　前記循環管路は、蛇行形状をなす屈曲部を有する晶析システム。     a crystallizer that mixes a plurality of raw material solutions to generate particles derived from a plurality of raw materials in the plurality of raw material solutions;
    a circulation pipe that flows the slurry containing the particles discharged from the discharge port of the crystallizer and circulates the slurry into the crystallizer from the inlet of the crystallizer;
    a circulation pump that circulates the slurry between the crystallizer and the circulation pipe,
    In the crystallization system, the circulation pipe has a meandering bent portion.
  2. 　前記循環管路の内径が一定である請求項１に記載の晶析システム。 The crystallization system according to claim 1, wherein the inner diameter of the circulation pipe is constant.
  3. 　前記屈曲部が複数設けられている請求項１又は２に記載の晶析システム。 The crystallization system according to claim 1 or 2, wherein a plurality of the bent portions are provided.
  4. 　前記屈曲部の少なくとも一部が温度調節槽の中に設けられている請求項１から請求項３の何れか一項に記載の晶析システム。 The crystallization system according to any one of claims 1 to 3, wherein at least a portion of the bent portion is provided in a temperature control tank.
  5. 　前記屈曲部が、分離可能な、複数の直管部と複数の曲管部と、から構成されている請求項１から請求項４の何れか一項に記載の晶析システム。 The crystallization system according to any one of claims 1 to 4, wherein the bent part is composed of a plurality of separable straight pipe parts and a plurality of bent pipe parts.
  6. 　前記晶析装置は、径方向に貫通する複数の孔を備えるとともに中心軸の回りに回転可能な撹拌翼と、
    　前記撹拌翼を同心状に内部に収容可能な有底円筒状の反応槽と、
    　前記反応槽に設けられるとともに前記反応槽の内部に第１の反応液を供給可能な導入口と、
    　前記撹拌翼に設けられるとともに前記反応槽の内部に第２の反応液を供給可能な給液部と、
    　を備える請求項１から請求項５の何れか一項に記載の晶析システム。     The crystallizer includes a stirring blade that has a plurality of holes that penetrate in the radial direction and is rotatable around a central axis;
    a bottomed cylindrical reaction tank capable of concentrically accommodating the stirring blade;
    an inlet provided in the reaction tank and capable of supplying a first reaction liquid into the reaction tank;
    a liquid supply part that is provided on the stirring blade and is capable of supplying a second reaction liquid into the inside of the reaction tank;
    The crystallization system according to any one of claims 1 to 5, comprising:
  7. 　前記撹拌翼は、円筒状の円筒部と、前記円筒部の内周面に外縁部が固定される円盤状の円盤部と、前記円盤部の平面視の中心から前記中心軸に沿って上方に延びる回転軸と、を備え、
    　前記円盤部と前記回転軸との内部を前記第２の反応液が流通可能であり、
    　前記円盤部の前記外縁部に前記給液部が設けられている請求項６に記載の晶析システム。     The stirring blade includes a cylindrical cylindrical part, a disc-shaped disc part whose outer edge is fixed to an inner circumferential surface of the cylindrical part, and a disc part extending upwardly along the central axis from the center of the disc part in a plan view. comprising an extending rotation axis;
    The second reaction liquid can flow inside the disk portion and the rotating shaft,
    The crystallization system according to claim 6, wherein the liquid supply section is provided at the outer edge of the disk section.
  8. 　前記給液部は下方に向けて開口している請求項７に記載の晶析システム。 The crystallization system according to claim 7, wherein the liquid supply section opens downward.
  9. 　前記給液部は径方向外側に向けて開口し前記円筒部を貫通している請求項７に記載の晶析システム。 The crystallization system according to claim 7, wherein the liquid supply section opens radially outward and penetrates the cylindrical section.
  10. 　複数の原料溶液を混合して前記複数の原料溶液の中の複数の原料に由来する粒子を晶析装置で成長させる晶析ステップと、
    　前記晶析装置の排出口から排出される前記粒子を含むスラリを、蛇行形状をなす屈曲部を有する循環管路を流動させることで前記晶析装置の導入口まで循環させる循環ステップと、を含む晶析方法。     a crystallization step of mixing a plurality of raw material solutions and growing particles derived from a plurality of raw materials in the plurality of raw material solutions in a crystallizer;
    a circulation step of circulating the slurry containing the particles discharged from the discharge port of the crystallizer to the inlet of the crystallizer by flowing a circulation pipe having a meandering bent portion; Crystallization method.
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CN209865364U (en) * 2019-03-21 2019-12-31 杭州新龙化工有限公司 High-cooling crystallization device for preparing potassium nitrate
WO2022202489A1 (en) * 2021-03-26 2022-09-29 月島機械株式会社 Crystallization device, crystallization system, and crystallization method

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