Wet crystallization system and method for microcrystal

Abstract

A wet crystallization system for a microcrystal, comprising at least one dispersion unit (100), a solvent tank (200) for providing a poor solvent to the dispersion unit (100), and a saturated solution tank (300) for providing a saturated solution to the dispersion unit (100), the poor solvent being delivered into the dispersion unit (100) by means of a delivery structure, the saturated solution tank (300) being connected to a feeding pipe (120) of the dispersion unit (100), and the feeding pipe (120) passing through the delivery structure and extending to a position close to a dispersion module of the dispersion unit (100), such that the saturated solution starts to be mixed with the poor solvent at the position. The wet crystallization system for a microcrystal changes the feeding mode of the saturated solution from three-way mixing feeding into feeding pipe (120) and three-way mixing feeding, so as to change the mixing area of the saturated solution and the poor solvent to the area closer to the dispersion module, thus improving the uniformity of microcrystals generated in a crystallization process. Further provided is a corresponding method.

Description

Wet microcrystal crystallization system and method Technical Field

[0001] The present invention relates to a crystallization system and method, and in particular to a wet crystallization system and method. Background Art

[0002] Currently, there are two main methods for preparing sterile microcrystals on the market. One is wet crushing, which involves placing the raw materials in water to form a suspension, and then using a high-pressure homogenizer or ball mill to crush the raw materials in water.

[0003] The other is wet crystallization, which first places the raw material in an alcohol solvent to dissolve it to form a saturated solution; then the saturated solution is added to a poor solvent such as water. Since the solvent of the saturated solution is miscible with water, when the saturated solution is added to water, the concentration of the alcohol solvent is rapidly reduced, thereby reducing the saturated solubility of the raw material, causing the raw material to precipitate and reform into crystals.

[0004] In the prior art, as shown in FIG6 , the alcohol solvent from tank T01 is added to the aqueous solution in tank T02 from the top of tank T02 at a set flow rate. During this process, the agitator at the bottom of tank T02 is used to continuously stir and disperse the solution, rapidly reducing the concentration of the saturated solution so that crystals precipitate at a certain concentration, thereby achieving the requirement of controlling the particle size of the precipitated crystals.

[0005] However, such a crystallization system has certain problems. For example, as production scales up, the volume of tank T02 increases, resulting in a higher initial liquid level and a longer travel distance from the saturated solution to the bottom mixer. Due to the rapid precipitation reaction, the saturated solution cannot be quickly dispersed into the water after scaled-up production. This can lead to excessively high local concentrations of the saturated solution, but the precipitation reaction will still occur. The high concentration of precipitation will result in larger crystal particles, which are inconsistent with the particle size of the precipitation during the pilot test, resulting in poor product particle size uniformity.

[0006] Summary of the Invention

[0007] An object of the present invention is to provide a wet microcrystal crystallization system with improved uniformity of precipitated particle size.

[0008] To this end, some embodiments of the present application provide a wet microcrystal crystallization system, which includes at least one dispersion unit, a solvent tank that provides a poor solvent to the dispersion unit, and a saturated solution that provides a saturated solution to the dispersion unit; wherein the poor solvent is fed into the dispersion unit through a distribution structure, the saturated solution tank is connected to a feed pipe of the dispersion unit, and the feed pipe passes through the distribution structure and extends to a position adjacent to the dispersion module of the dispersion unit so that the saturated solution begins to mix with the poor solvent at this position.

[0009] In some embodiments, the location of the dispersion module adjacent to the dispersion unit is within the dispersion unit or at an outlet location of the delivery structure adjacent to the dispersion unit.

[0010] In some embodiments, the feeding tube includes a long tubular body and a pre-dispersion hole disposed at a distal end of the long tubular body.

[0011] In some embodiments, the pre-dispersion holes are sized to form different forms of pre-dispersed saturated solutions.

[0012] In some embodiments, the pre-dispersed saturated solution includes a saturated solution jet or a sprayed saturated solution.

[0013] In some embodiments, the dispersion unit includes a dispersion chamber and the dispersion module disposed in the dispersion chamber.

[0014] In some embodiments, the dispersion unit includes a first dispersion chamber, a first dispersion module arranged in the first dispersion chamber, a second dispersion chamber, and a second dispersion module arranged in the second dispersion chamber; the first dispersion chamber and the second dispersion chamber are connected by a channel; the first dispersion module and the second dispersion module are coupled by a reversing mechanism so that the first dispersion module rotates in a first direction, and the second dispersion module rotates in a second direction opposite to the first direction.

[0015] In some embodiments, the channel is a straight channel or a spiral channel, and the spiral direction of the spiral channel is the same as the first direction.

[0016] In some embodiments, the channel includes a connecting hole connected to the first dispersion chamber and a swirl section connected to the second dispersion chamber, and the swirl section is an arc-shaped channel with the same rotation direction as the second dispersion module.

[0017] In some embodiments, the dispersion unit includes a main body, which includes a feed port, a discharge port, and the first dispersion chamber and the second dispersion chamber arranged between the feed port and the discharge port, the channel connecting the first dispersion chamber and the second dispersion chamber, and a discharge buffer chamber arranged between the second dispersion chamber and the discharge port; wherein, the first dispersion module is installed in the first dispersion chamber, and the first dispersion module includes a first dispersion fan blade driven by a first rotating shaft; the second dispersion module is installed in the second dispersion chamber, and the second dispersion module includes a second dispersion fan blade driven by a second rotating shaft; wherein, the first rotating shaft and the second rotating shaft are coupled together through the reversing mechanism to realize the linkage between the first dispersion module and the second dispersion module; the second rotating shaft is driven by the motor through the transmission shaft.

[0018] In some embodiments, the dispersion module includes a dispersion chamber in which a dispersion module is disposed, and also includes a grinding chamber connected to the dispersion chamber in which a grinding module is disposed. The grinding module includes a grinding rotor, and the size of the grinding rotor is determined to form a gap channel around the grinding rotor.

[0019] In some embodiments, the gap size of the gap channel is set to 0.3-1 mm, preferably 0.4-0.7 mm, and more preferably 0.45-0.55 mm.

[0020] In some embodiments, a reversing mechanism is further included, and the dispersion module is coupled to the grinding module via the reversing mechanism.

[0021] In some embodiments, the grinding module further includes a gap adjustment block to adjust the axial position of the grinding rotor to adjust the gap size of the gap channel.

[0022] In some embodiments, the dispersion unit includes a main body, which includes a feed port, a discharge port, and the dispersion chamber and the grinding chamber arranged between the feed port and the discharge port, and a discharge buffer chamber arranged between the grinding chamber and the discharge port; wherein the dispersion module is installed in the dispersion chamber, and the dispersion module includes dispersion blades driven by a rotating shaft; the grinding module is arranged in the grinding chamber, and the grinding module includes a grinding rotor and a grinding shaft driving the grinding rotor; wherein the grinding shaft is driven by a motor through a transmission shaft.

[0023] In some embodiments, the dispersion unit includes a first dispersion unit and a second dispersion unit connected sequentially, wherein the dispersion module in the first dispersion unit is configured to rotate in a first direction, and the dispersion module in the second dispersion unit is configured to rotate in a second direction opposite to the first direction.

[0024] In some embodiments, a solvent tank provides a poor solvent to the dispersion unit through a poor solvent conduit, and a saturated solution tank provides a saturated solution to the dispersion unit through a saturated solution conduit; a first pump is provided on the poor solvent conduit, and a second pump is provided on the saturated solution conduit.

[0025] In some embodiments, the first pump and the second pump are metering pumps.

[0026] In some embodiments, the method further comprises a suspension buffer tank connected downstream of the dispersion unit via a microcrystal suspension conduit.

[0027] Another object of the present invention is to provide a wet-process microcrystal crystallization method with improved uniformity of precipitated particle size, the method comprising providing at least one dispersion unit; providing a distribution structure to provide a poor solvent to the dispersion unit; providing a feed pipe, the feed pipe passing through the distribution structure and extending to a position adjacent to the dispersion module of the dispersion unit, and providing a saturated solution through the feed pipe so that the saturated solution begins to mix with the poor solvent at this position.

[0028] The beneficial effects of this solution include: in some embodiments, the wet microcrystal crystallization system and method of the present application changes the feeding mode of the saturated solution, from a three-way mixed feed to a feed pipe and a three-way mixed feed, and the mixed zone of the saturated solution in the poor solvent is changed to an area closer to the dispersion module, so as to enhance the uniformity of the microcrystals produced by the crystallization process and improve the dispersion effect after crystallization. In some embodiments, the structural setting of the pre-dispersion hole of the feed pipe allows the saturated solution to enter the dispersion module in a pre-dispersion manner and mix with the poor solvent therein, and then be further dispersed by the dispersion module to ensure the particle size of the microcrystals. In some embodiments, the use of two sets of upper and lower dispersion modules that rotate in opposite directions helps to better solve the agglomeration problem of the microcrystals produced by crystallization, thereby increasing the uniformity of the particle size of the precipitated microcrystals. In some embodiments, the use of a dispersion module and a grinding module set up above helps to better solve the agglomeration problem of the microcrystals produced by crystallization, thereby increasing the uniformity of the particle size of the precipitated microcrystals. In some embodiments, the wet microcrystal crystallization system of the present application has two-stage dispersion units, and the first-stage dispersion unit rotates in the opposite direction to the first dispersion unit. Such a setting helps to better solve the agglomeration problem of microcrystals produced by crystallization, thereby increasing the uniformity of the particle size of the precipitated microcrystals. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Other features, objects and advantages of the present invention will become more apparent upon reading the detailed description of non-limiting embodiments made with reference to the following drawings:

[0030] FIG1 is a schematic structural diagram of a wet-process microcrystal crystallization system according to a first embodiment of the present invention;

[0031] FIG2A is a schematic structural diagram of an introduction component according to an embodiment of the present invention;

[0032] FIG2B is a schematic side view of a saturated solution pre-dispersion conduit structure according to an embodiment of the present invention;

[0033] FIG2C is a bottom view schematically showing the structure of a saturated solution pre-dispersion conduit according to an embodiment of the present invention;

[0034] FIG2D is a schematic structural diagram of a dispersion unit of a wet-process microcrystal crystallization system according to the first embodiment of the present invention;

[0035] FIG3A is a schematic structural diagram of a dispersion unit of a wet-process micro-crystal crystallization system according to a second embodiment of the present invention;

[0036] FIG3B is a schematic side view of a configuration of a channel of a dispersion unit of a wet-process microcrystal crystallization system according to a second embodiment of the present invention;

[0037] FIG3C is a schematic side view of another configuration of the channel of the dispersion unit of the wet microcrystal crystallization system according to the second embodiment of the present invention;

[0038] FIG3D is a bottom view schematically showing another configuration of the channel of the dispersion unit of the wet-process microcrystal crystallization system according to the second embodiment of the present invention;

[0039] FIG4 is a schematic structural diagram of a dispersion unit of a wet-process microcrystal crystallization system according to a third embodiment of the present invention;

[0040] FIG5 is a schematic structural diagram of a wet-process microcrystal crystallization system according to a second embodiment of the present invention;

[0041] FIG6 is a structural diagram of a driving device of the prior art in the background art of the present invention; DETAILED DESCRIPTION

[0042] The present invention is further described in detail below with reference to the accompanying drawings.

[0043] The specific structural and functional details disclosed herein are merely representative and are for the purpose of describing exemplary embodiments of the present application. However, the present application may be implemented in many alternative forms and should not be construed as being limited to the embodiments set forth herein.

[0044] It should be understood that although the terms "first," "second," and the like may be used herein to describe various elements, these elements should not be limited by these terms. These terms are used solely to distinguish one element from another. For example, a first element may be referred to as a second element, and similarly, a second element may be referred to as a first element, without departing from the scope of the exemplary embodiments. The term "and / or" as used herein includes any and all combinations of one or more of the listed associated items.

[0045] The terms used herein are intended only to describe specific embodiments and are not intended to limit exemplary embodiments. Unless the context clearly indicates otherwise, the singular forms "a", "an", "an item" used herein are also intended to include the plural. It should also be understood that the terms "comprise" and / or "include" used herein specify the presence of stated features, integers, steps, operations, units and / or components, and do not exclude the presence or addition of one or more other features, integers, steps, operations, units, components and / or combinations thereof.

[0046] Those skilled in the art will readily appreciate other embodiments of the present invention after considering the specification and practicing the invention disclosed herein. This application is intended to cover any variations, uses, or adaptations of the present invention that follow the general principles of the invention and include common knowledge or customary techniques in the art not disclosed herein.

[0047] Microcrystals here refer to

[0048] [Example 1: Primary dispersion unit + pre-dispersion pipe extended to dispersion module]

[0049] As shown in Figures 1 to 2C, the wet microcrystal crystallization system in the first embodiment provided by the present invention includes a dispersion unit 100, a suspension buffer tank 400 connected to the downstream of the dispersion unit 100 via a microcrystal suspension conduit 401, a solvent tank 200 that provides a poor solvent to the dispersion unit 100 via a poor solvent conduit 201, and a saturated solution tank 300 that provides a saturated solution to the dispersion unit 100 via a saturated solution conduit 301. A first pump 202 may also be provided on the poor solvent conduit 201, and a second pump 302 may also be provided on the saturated solution conduit 301.

[0050] As shown in Figure 2D, the dispersion unit 100 may include a dispersion chamber 101 and a dispersion module 104 in the dispersion chamber, and the dispersion module 104 includes a rotating shaft 141 and a rotatable dispersion fan 142 driven by the rotating shaft, and the dispersion blade 141 can disperse the mixed solution of the poor solvent and the saturated solution in the dispersion chamber 101 to enhance the crystallization effect of microcrystals. The introduction of the poor solvent and the saturated solution is achieved by a distribution structure, such as a three-way structure 110, the outlet 113 of the three-way structure connects the inlet of the dispersion unit 100, the first inlet 111 of the three-way structure is provided with a feed pipe 120 for introducing a saturated solution, the feed pipe 120 is directly connected to the saturated solution conduit 301, and the second inlet 112 of the three-way structure is connected to the poor solvent. The structure of the feed pipe 120 can include a cover plate 122 for sealingly fitting on the first inlet 111 of the three-way structure and a long tube portion 121 that can extend through the length of the cavity 114 of the entire three-way structure to reach the outlet 113 of the three-way structure.

[0051] The length of the long tube portion 121 is set to be as close to the dispersion module 104 as possible, for example, extending at least to the vicinity of the outlet of the three-way structure, for example, extending out of the outlet 113 of the three-way structure into the dispersion unit 100, for example, reaching the feed port of the body of the dispersion unit, or for example, passing through the feed port of the body of the dispersion unit into the dispersion chamber 101 to be close to the dispersion module 104.

[0052] In some embodiments, the long tube portion 121 is concentric with the cavity 114 of the three-way structure.

[0053] The feeding method of the saturated solution is changed from three-way mixed feeding to feeding pipe and three-way mixed feeding, and the mixing area of ​​the saturated solution and the poor solvent is changed from the inside of the cavity of the three-way to the area closer to the dispersion module 104, so as to avoid the saturated solution concentration in the three-way being too high and crystallization occurring too early. By making the saturated solution enter the dispersion cavity more dispersedly, the uniformity of the microcrystals produced in the crystallization process can be enhanced, and the consistency of the particles after crystallization can be improved.

[0054] It should be understood that the distribution structure in this application does not necessarily have to be a three-way structure. It can also be of other structural forms, as long as the feed pipe carrying the saturated solution directly delivers the saturated solution to a position of the dispersion module adjacent to the dispersion unit. This position can be within a position of the dispersion unit or at the outlet position of the distribution structure adjacent to the dispersion unit. [Improvement: Pre-dispersion of the pre-dispersion pipe]

[0055] In some embodiments, an array of holes is provided at the distal end 1210 of the long tube portion 121 of the feeding tube 120 on the side of the outlet 113 of the three-way structure as pre-dispersion holes 12101 .

[0056] The distal end 1210 of the long tube portion 121 may be cylindrical, hemispherical, conical, or truncated-conical in shape. The array arrangement of the pre-distribution holes 1210 at the distal end 1210 is not limited and may, for example, be distributed throughout the distal end 1210, the bottom and / or the entire distal end of the distal end 1210, and a certain length of the upwardly extending long tube portion.

[0057] The diameter of the pre-dispersion hole 12101 can be set according to the size requirements of the crystallization. For example, if a larger diameter crystallization is required, a larger pre-dispersion hole 12101 can be set to achieve jet or spray feeding of the saturated solvent; if a smaller diameter crystallization is required, a smaller pre-dispersion hole 12101 can be set to control the saturated solvent to a feeding form with a higher dispersion degree. The above methods are collectively referred to as pre-dispersion methods.

[0058] The structural setting of the pre-dispersion hole of the feeding tube 120 allows the saturated solution to enter the dispersion module in a pre-dispersion manner and mix with the poor solvent therein, and then be further dispersed by the dispersion module 104 to ensure the particle size of the microcrystals.

[0059] [Example 2: Dispersion Unit of Double Dispersion Module]

[0060] The dispersion unit 100 in the above embodiment can be a dispersion module structure with a single dispersion blade set in a traditional single dispersion chamber, as shown in Figure 2D, a double dispersion blade, or a triple dispersion blade. Or it can be a dispersion module with an improved structure. For example, as shown in Figure 3A, the dispersion unit 100 can be a dispersion unit of a double dispersion module, which includes a body 101, the body includes a feed port 1011, a discharge port 1016, and a first dispersion chamber 1012 and a second dispersion chamber 1014 arranged between the feed port 1011 and the discharge port 1016, a channel 1013 connecting the first dispersion chamber and the second dispersion chamber, and a discharge buffer chamber 1015 arranged between the second dispersion chamber 1014 and the discharge port 1016. A first dispersion module 104 is installed in the first dispersion chamber, and the first dispersion module includes first dispersion blades driven by a first rotating shaft 1041; a second dispersion module 105 is installed in the second dispersion chamber, and the second dispersion module includes second dispersion blades driven by a second rotating shaft 1051. The first rotating shaft 1041 and the second rotating shaft 1051 are coupled together via a reversing mechanism 106 to achieve linkage between the first dispersion module and the second dispersion module. For example, the second rotating shaft 1051 is driven by the motor 103 via the transmission shaft 102. In this way, the second rotating shaft can drive the second dispersion blades to rotate in the second direction, and by coupling with the reversing mechanism, the first rotating shaft can drive the first dispersion blades to rotate in a first direction opposite to the second direction. Alternatively, the second rotating shaft can drive the second dispersion blades to rotate in the second direction, and by coupling with the reversing mechanism, the first rotating shaft can drive the first dispersion blades to rotate in the second direction, but at the same or different speed as the second rotating shaft.

[0061] The reversing mechanism 106 may be a mechanical coupler, such as a gear pair; or an electromagnetic coupler.

[0062] The channel 1013 may be a straight connecting channel as shown in FIG3A . Alternatively, the channel 1013 may be a spiral channel formed in the same direction as the rotation direction of the first dispersing blades, as shown in FIG3B .

[0063] Alternatively, as shown in Figures 3C and 3D, the channel 1013 may be a combination of a connecting hole 10131 connecting the first dispersion chamber and a swirl section 10132 connecting the second dispersion chamber 1014. In this design, the suspension in the swirl section is accelerated by the rotation of the second dispersion module, thereby generating a siphon effect on the suspension in the connecting hole 10131, drawing the suspension in the first dispersion chamber 1012 through the connecting hole into the second dispersion chamber 1014. In an improved embodiment, the rotation speed of the second dispersion module can be controlled to adjust the degree of the siphon effect, for example, by adjusting the rotation speed of the second dispersion module to be higher than that of the first dispersion module.

[0064] It should be understood that although the first dispersion module and the second dispersion module given in the above embodiment are in a vertical positional relationship, other variations of this embodiment may also have a positional relationship such as left-right setting or inclined setting, as long as the first dispersion module and the second dispersion module have an upstream and downstream processing relationship.

[0065] The use of two sets of upper and lower dispersion modules that rotate in opposite directions helps to better solve the agglomeration problem of microcrystals produced by crystallization, thereby increasing the uniformity of the particle size of the precipitated microcrystals.

[0066] As shown in Figure 3, the feed port 1011 of the body is coupled to a three-way structure 120, which can be the same as the three-way structure in the previous embodiment. In this embodiment, the feed pipe can be arranged in the same manner as the feed pipe in the previous embodiment, for example, it can also extend to the first dispersion unit.

[0067] [Example 3: Dispersion unit of dispersion module + grinding module]

[0068] As shown in FIG4 , the wet microcrystal crystallization system in this embodiment adopts another dispersion unit 100, which is a dispersion, grinding, mixing and dispersion unit, and includes a main body 101, which includes a feed inlet 1011, a discharge port 1016, a first dispersion chamber 1012 arranged between the feed inlet 1011 and the discharge port 1016, a grinding chamber 1017, and a discharge buffer chamber 1015 arranged between the grinding chamber 1017 and the discharge port 1016. A first dispersion module 104 is installed in the first dispersion chamber, and the first dispersion module includes a first dispersion fan driven by a first rotating shaft 1041. A grinding module is provided in the grinding chamber 1017, and the grinding module includes a grinding rotor 107 and a grinding rotating shaft 1071 that drives the grinding rotor 107. The grinding rotating shaft 1071 is further driven by a motor 103 through a transmission shaft 102.

[0069] The grinding chamber may have a configuration corresponding to that of the grinding rotor, for example, the same configuration, so that a gap channel, for example, a gap channel approximately in the shape of a truncated cone, is formed between the grinding chamber and the grinding rotor 107, for the microcrystal suspension dispersed by the first dispersion module to pass through the gap channel and then be ground by the grinding rotor to reduce the agglomeration of the microcrystals.

[0070] The gap channel of the grinding chamber 1017 between the main body 101 and the grinding rotor 107 is set to a gap of 0.3-1 mm, preferably a gap of 0.4-0.7 mm, and more preferably a gap of 0.45-0.55 mm; since the gap is very small, the agglomerated crystals can be fully broken up to avoid the occurrence of large agglomeration.

[0071] In this embodiment, the grinding rotor 107 may be provided with a gap adjustment block to adjust the axial position of the grinding rotor 107 on the grinding shaft 1071, thereby adjusting the gap size of the gap channel. This allows microcrystals that meet the particle size requirements to pass smoothly, while particles that do not meet the particle size requirements, such as particles formed by agglomerated microcrystals, continue to experience a certain shear force within the gap channel, thereby being ground to a smaller particle size.

[0072] In some variations of this embodiment, the first rotating shaft 1041 and the grinding rotating shaft 1071 are coupled together via a reversing mechanism 106 to achieve linkage between the first dispersion module and the grinding module. For example, the grinding rotating shaft 1071 is driven by the motor 103 via the transmission shaft 102. In this way, the grinding rotating shaft can drive the grinding rotor to rotate in the second direction, and by virtue of the coupling with the reversing mechanism, the first rotating shaft can drive the first dispersion blade to rotate in the first direction opposite to the second direction. Alternatively, the grinding rotating shaft 1071 can drive the grinding rotor 107 to rotate in the second direction, and by virtue of the coupling with the reversing mechanism, the first rotating shaft can drive the first dispersion blade to rotate in the second direction as well, but at the same or different speed as the grinding rotating shaft.

[0073] The reversing mechanism 106 may be a mechanical coupler, such as a gear pair; or an electromagnetic coupler.

[0074] It should be understood that although the first dispersion module and the grinding module given in the above embodiment are in a vertical positional relationship, other variations of this embodiment may also have a positional relationship such as left-right setting or inclined setting, as long as the first dispersion module and the grinding module have an upstream and downstream processing relationship.

[0075] The use of the dispersing module and the grinding module arranged upstream and downstream helps to better solve the agglomeration problem of the microcrystals produced by crystallization, thereby increasing the uniformity of the particle size of the precipitated microcrystals.

[0076] [Example 4: Secondary dispersion unit + pre-dispersion pipe extended to dispersion module]

[0077] As an improvement to the above embodiment, as shown in FIG5 , a two-stage dispersion unit can be provided for the wet microcrystal crystallization system, that is, the wet microcrystal crystallization system includes a first dispersion unit 100A, a second dispersion unit 100B connected downstream of the first dispersion unit 100A, a suspension buffer tank 400 connected downstream of the second dispersion unit 100B via a microcrystal suspension conduit 401, a solvent tank 200 that supplies a poor solvent to the first dispersion unit 100A via a poor solvent conduit 201, and a saturated solution tank 300 that supplies a saturated solution to the first dispersion unit 100A via a saturated solution conduit 301. A first pump 202 can also be provided on the poor solvent conduit 201, and a second pump 302 can also be provided on the saturated solution conduit 301.

[0078] Similarly, the first dispersion unit 100A may include a first dispersion module, the first dispersion module including a first dispersion chamber and a rotatable first dispersion blade, and the first dispersion blade can disperse the mixture of the poor solvent and the saturated solution in the first dispersion chamber to enhance the crystallization effect of the microcrystals. The introduction of the poor solvent and the saturated solution is achieved by a three-way structure 110, the outlet 113 of the three-way structure is connected to the inlet of the dispersion unit 100, the first inlet 111 of the three-way structure is connected to the saturated solution, and the second inlet 112 of the three-way structure is connected to the poor solvent. A feed pipe 120 is provided in the three-way structure, and the structure of the feed pipe 120 as shown in Figures 2B and 2C may include a cover plate 122 for sealingly fitting on the first inlet 111 of the three-way structure and a long tube portion 121 that can extend through the length of the cavity 114 of the entire three-way structure. The second dispersion unit 100B has the same structure as the first dispersion unit, except that the feed inlet does not need to be connected to the three-way structure, but is directly connected to the first discharge port of the first dispersion unit 100A. The second discharge port of the second dispersing unit 100B is connected to the suspension buffer tank 400, or directly connected to equipment in subsequent processes, such as a filtering device.

[0079] The first dispersing module in the first dispersing unit 100A is configured to rotate in a first direction, while the second dispersing module in the second dispersing unit 100B is configured to rotate in a second direction opposite to the first direction. For example, the first direction may be clockwise, and the second direction may be counterclockwise, or vice versa. The two-stage dispersing unit configuration with counter-rotating units helps to better resolve the agglomeration problem of microcrystals produced by crystallization, thereby increasing the uniformity of the particle size of the precipitated microcrystals.

[0080] Similar to the above embodiment, the distal end 1210 of the long tube portion 121 of the feed tube 120 located on the side of the outlet 113 of the three-way structure is provided with arrayed holes as pre-dispersion holes 12101, thereby enhancing the uniformity of the microcrystals.

[0081] Similar to the above-mentioned embodiment, the first dispersing unit 100A can be a common dispersing unit, the above-mentioned double dispersing module dispersing unit, or one of the dispersing grinding and mixing dispersing units, and the second dispersing unit 100B can be a common dispersing unit, the above-mentioned double dispersing module dispersing unit, or one of the dispersing grinding and mixing dispersing units.

[0082] In the above embodiment, the first pump 202 for pumping the poor solvent conduit 201 and the second pump 302 for pumping the saturated solution can be metering pumps, so as to adjust the ratio of the saturated solution to the poor solvent as needed.

[0083] The saturated solution can be prepared by dissolving the raw materials in an alcohol solvent, such as methanol, ethanol, benzyl alcohol, ethylene glycol, etc. The poor solvent is, for example, water, especially distilled water or deionized water.

[0084] It will be understood that the present invention is not limited to the exact construction that has been described above and shown in the drawings, and that various modifications and changes may be made without departing from the scope thereof.

[0085] The foregoing description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be applied to other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not intended to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

[0086] Furthermore, while advantages associated with certain embodiments of the technology have been described in the context of those embodiments, other embodiments may also exhibit such advantages, and not all embodiments need necessarily exhibit such advantages to fall within the scope of the technology. Accordingly, the present disclosure and associated technology may include other embodiments not expressly shown or described herein. Accordingly, the present disclosure is limited solely by the following claims.

Claims

1. A wet microcrystalline crystallization system, characterized in that: It includes at least one dispersion unit, a solvent tank for supplying a poor solvent to the dispersion unit, and a saturated solution tank for supplying a saturated solution to the dispersion unit; wherein, the poor solvent is fed into the dispersion unit through a distribution structure, the saturated solution tank is connected to the feed pipe of the dispersion unit, and the feed pipe passes through the distribution structure and extends to a position adjacent to the dispersion module of the dispersion unit such that the saturated solution starts to mix with the poor solvent at this position.

2. The wet microcrystal crystallization system according to claim 1, wherein: The position adjacent to the dispersion module of the dispersion unit is within the dispersion unit or at the outlet position of the distribution structure adjacent to the dispersion unit.

3. The wet microcrystal crystallization system according to claim 1, characterized in that: The feed pipe includes a long pipe body and pre-dispersion holes provided at the distal end of the long pipe body.

4. The wet microcrystal crystallization system according to claim 3, characterized in that: The size of the pre-dispersion holes is determined to form pre-dispersed saturated solutions in different forms.

5. The wet microcrystal crystallization system according to claim 4, characterized in that: The pre-dispersed saturated solutions include saturated solution jets and sprayed saturated solutions.

6. The wet microcrystalline crystallization system according to claim 1, characterized in that: The dispersion unit includes a dispersion chamber and the dispersion module provided in the dispersion chamber.

7. The wet microcrystal crystallization system according to claim 1, wherein: The dispersion unit includes a first dispersion chamber, a first dispersion module provided in the first dispersion chamber, a second dispersion chamber, and a second dispersion module provided in the second dispersion chamber; The first dispersion chamber and the second dispersion chamber are connected by a channel; the first dispersion module and the second dispersion module are coupled by a commutation mechanism such that the first dispersion module rotates in a first direction, while the second dispersion module rotates in a second direction opposite to the first direction.

8. The wet microcrystalline crystallization system according to claim 7, characterized in that: The channel is a straight channel or a spiral channel, and the spiral direction of the spiral channel is the same as the first direction.

9. The wet microcrystal crystallization system according to claim 7, characterized in that: The channel includes a communication hole connecting the first dispersion chamber and a swirl section connecting the second dispersion chamber, and the swirl section is an arc-shaped channel with the same rotation direction as the second dispersion module.

10. The wet microcrystal crystallization system according to claim 7, wherein: The dispersion unit includes a body, the body includes a feed port, a discharge port, and the first dispersion chamber, the second dispersion chamber provided between the feed port and the discharge port, the channel connecting the first dispersion chamber and the second dispersion chamber, and a discharge buffer chamber provided between the second dispersion chamber and the discharge port; wherein, the first dispersion module is installed in the first dispersion chamber, and the first dispersion module includes a first dispersion fan blade driven by a first rotating shaft; the second dispersion module is installed in the second dispersion chamber, and the second dispersion module includes a second dispersion fan blade driven by a second rotating shaft; wherein, the first rotating shaft and the second rotating shaft are coupled together through the commutation mechanism to realize the linkage of the first dispersion module and the second dispersion module; the second rotating shaft is driven by a motor through a transmission shaft.

11. The wet microcrystalline crystallization system according to claim 1, wherein: The dispersion module includes a dispersion chamber, a dispersion module is provided in the dispersion chamber, and also includes a grinding chamber communicated with the dispersion chamber, a grinding module is provided in the grinding chamber, and the grinding module includes a grinding rotor, and the size of the grinding rotor is determined to form a gap channel around the grinding rotor.

12. The wet microcrystalline crystallization system according to claim 11, characterized in that: The gap size of the gap channel is set to be 0.3 - 1 mm, preferably 0.4 - 0.7 mm, and more preferably 0.45 - 0.55 mm.

13. The wet microcrystalline crystallization system according to claim 11, characterized in that: It further includes a commutation mechanism, and the dispersion module is coupled to the grinding module through the commutation mechanism.

14. The wet microcrystalline crystallization system according to claim 1, characterized in that: The grinding module further includes a clearance adjustment block to adjust the axial position of the grinding rotor so as to adjust the clearance size of the clearance channel.

15. The wet microcrystal crystallization system according to claim 11, wherein: The dispersion unit includes a body, and the body includes a feed inlet, a discharge outlet, and the dispersion chamber, the grinding chamber provided between the feed inlet and the discharge outlet, and a discharge buffer chamber provided between the grinding chamber and the discharge; wherein, a dispersion module is installed in the dispersion chamber, and the dispersion module includes a dispersion fan blade driven by a rotating shaft; a grinding module is provided in the grinding chamber, and the grinding module includes a grinding rotor and a grinding rotating shaft for driving the grinding rotor; wherein, the grinding rotating shaft is driven by a motor through a transmission shaft.

16. The wet microcrystalline crystallization system according to claim 1, wherein: The dispersion unit includes a first dispersion unit and a second dispersion unit connected in sequence, wherein the dispersion module in the first dispersion unit is configured to rotate in a first direction, and the dispersion module in the second dispersion unit is configured to rotate in a second direction opposite to the first direction.

17. The wet microcrystalline crystallization system according to claim 1, characterized in that: A solvent tank for supplying a poor solvent to the dispersion unit through a poor solvent conduit, and a saturated solution tank for supplying a saturated solution to the dispersion unit through a saturated solution conduit; a first pump is further provided on the poor solvent conduit, and a second pump is further provided on the saturated solution conduit.

18. The wet microcrystalline crystallization system according to claim 17, characterized in that: The first pump and the second pump are metering pumps.

19. The wet microcrystalline crystallization system according to claim 17, wherein: It further includes a suspension buffer tank connected downstream of the dispersion unit through a microcrystal suspension conduit.

20. Wet microcrystalline crystallization method, characterized in that: It includes the following steps Provide at least one dispersion unit; Provide a distribution structure to supply a poor solvent to the dispersion unit; Provide a feed pipe, the feed pipe passes through the distribution structure and extends to a position adjacent to the dispersion module of the dispersion unit, and supply a saturated solution through the feed pipe so that the saturated solution starts to mix with the poor solvent at this position.

Images