JP5768162B1 - Horizontal inner cylinder rotation type crystallized product slurry extractor - Google Patents

Abstract

Provided is an inner cylinder rotating type mixer capable of forming a stable injection vortex in a reaction tank as compared with a conventional apparatus and obtaining a stable continuous crystallization action when a crystallization material is precipitated. To do. An inner cylinder rotor of a stirring and mixing unit has a conical tip that protrudes to the side without a bearing mechanism at the other end of a cantilever structure, and reacts on the central axis of a front cover that covers the conical tip. Inner cylinder rotation type that can set up the main injection port for injecting the crystallization material solution into the tank and injecting the crystallization material solution from the main injection port to the conical apex of the inner cylinder rotor to form the injection vortex Stirring mixer. [Selection] Figure 2

Description

The present invention relates to a crystallized product slurry extractor of a horizontal inner cylinder rotation type that enables crystallization of a good specific crystal form mainly in the pharmaceutical manufacturing field and the electronic material manufacturing field .

Further, the inner cylinder rotating type stirring mixer improved in the present invention is a horizontal inner cylinder rotating capable of producing a crystallized product slurry of a specific crystal form product of, for example, an active pharmaceutical ingredient or an electronic material with high efficiency and high yield. A type of crystallized product slurry extractor is provided.

As an apparatus that enables crystallization of a specific crystal form, there is an inner cylinder rotating type stirring mixer that applies Taylors-flow. An inner cylinder rotating type mixer is provided with a hollow outer cylinder fixed on the same axis and an inner cylinder rotor that rotates while maintaining a constant distance from the inner wall of the outer cylinder, and a liquid is provided between the two long concentric cylinders. While injecting, the inner cylinder rotor is rotated and the target component is continuously crystallized (crystallized) from the liquid by cooling or heating using the temperature dependence of the solubility of the injected solution, and the chemical separation operation is performed. It is a device to do.

Thus, as a specific conventional example of the continuous crystallization apparatus according to the present invention, there is JP 2013-539176 A (hereinafter referred to as Patent Document 1).
The configuration of the apparatus described in Patent Document 1 includes a cylinder (10) as a non-rotating body having a reaction chamber (11) therein, and a stirring motor (20) disposed on one side of the cylinder (10). And a stirring rod that is connected to the motor shaft (21) of the stirring motor (20) and is built in the reaction chamber (11) but is separated from the wall of the reaction chamber (11). (30) having a continuous reactor,
1) a flange portion (12) formed on one side of the cylinder (10);
2) one or more reactant injection ports (13) formed on the flange portion so as to communicate with the reaction chamber (11) and into which reactants are injected;
3) a reaction result discharge port (14) formed on the other side of the cylinder (10) so as to communicate with the reaction chamber (11) and discharge the reaction result;
4) A number of excess ports (15) formed to communicate with the reaction chamber (11) between the reactant injection port (13) and the reaction product discharge port (14) of the cylinder (10). ,
5) a temperature adjusting unit (40) disposed between the outer peripheral surface and the inner peripheral surface of the cylinder (10);
6) A particle crushing section (50) provided on the flow path of the reactant injection port (13) for crushing particles of the reactant to be sucked through the reactant injection port;
7) A flow rate sensor (60) that is provided in at least one of the reactant injection port (13), the reaction product discharge port (14), and the surplus port (15) to sense the flow rate of the reactant. When,
8) a flow rate controller (70) for controlling the flow rate of the reactant flowing in via the reactant injection port (13) according to the flow rate sensing data returned by the flow rate sensor (60);
With
9) The temperature adjusting unit (40) includes an annular refrigerant chamber (41) and a refrigerant (42) filled in the refrigerant chamber;
An all-in-one type continuous reactor for producing a positive electrode active material of a lithium secondary battery.
(This description refers to claim 1 of Patent Document 1 and summarizes the structure of the invention in an itemized list. For reference numerals, refer to FIGS. 1 to 4 of Reference Document 1.)

Thus, the invention of Patent Document 1 provides a continuous crystallizer similar to the invention of the conventional apparatus, that is, JP 2011-83768 A (hereinafter referred to as Patent Document 2). In the invention of Patent Document 1, a series of operations for obtaining a specific crystal product of an electronic material in which the temperature adjusting unit 5), the particle size adjusting unit 6), and the flow rate controlling unit 7) are integrated. The present invention provides a continuous reactor that can be carried out in one reaction apparatus and a crystal separation apparatus including the same.

And in invention of the said patent document 1, in the continuous reactor which has the temperature control part 5), the particle size adjustment part 6), and the flow volume control part 7), it discharges | emits via a reaction result product discharge port (14). A positive electrode active material separator (300) such as a centrifugal separator or a dehydrator for separating the positive electrode active material and the filtrate from the reacted thriller-like material, or the positive electrode active material separator (300) A particle size analyzer for analyzing the particle size distribution and size of the cathode active material connected to the dryer and drying the cathode active material, or connected to the dryer (400) and dried. Discloses an invention relating to an all-in-one type continuous reactor equipped with a reactor and a crystal separation device equipped with the same.

However, in the conventional inner cylinder type stirring mixer used in the inventions of Patent Document 1 and Patent Document 2 described above, since it is a complex reaction apparatus, it has stable performance and good specific crystal form. It was not an easy-to-use inner cylinder type stirring mixer that enables crystallization of

Special table 2013-539176 gazette JP 2011-83768 A

The present invention is capable of forming a stable injection vortex in a reaction tank in a continuous crystallization apparatus using a stirring mixer of an inner cylinder rotation type as compared with the conventional apparatus, and stable in precipitation of the crystallization material. The present invention provides an inner cylinder rotating type stirring mixer capable of obtaining a continuous crystallization action.

The present invention also relates to a continuous crystallization apparatus using an inner cylinder rotating type agitation mixer, in which the shape of the reaction tank formed by the fixed hollow outer cylinder and the inner cylinder rotor is improved, and the crystallization liquid is contained in the reaction tank. By eliminating the pool portion, a reaction with a constant residence time is made possible at all times, and an inner cylinder rotating type stirring mixer is provided in which a crystallized product slurry of the same quality can be obtained continuously.

Furthermore, the present invention provides a new mechanism for the rotation support mechanism of the apparatus, the shape of the inner cylinder rotor, the installation of the front cover of the inner cylinder rotor, etc. By adopting the present invention, there is provided an inner cylinder rotating type agitation mixer that can easily clean a fixed hollow outer cylinder, an inner cylinder rotor, and a reaction tank that form an agitation and mixing section.

The present invention provides a stirring and mixing unit having a reaction tank in which a gap between a fixed hollow outer cylinder and a rotatable inner cylinder rotor formed on a coaxial central axis is horizontally installed. The drive motor side for the inner cylinder rotor is attached to the gantry with a cantilever structure, and the inner cylinder rotor of the stirring and mixing unit has a conical tip that protrudes to the side without the bearing mechanism at the other end of the cantilever structure The fixed hollow outer cylinder that forms the outer cylinder portion of the inner cylinder rotor having the conical tip portion is provided with a front cover that covers the conical tip portion of the inner cylinder rotor, on the central axis of the front cover. Is provided with a main inlet for injecting a crystallizing material solution into the reaction tank, and the main inlet is provided to face the conical apex of the conical tip of the inner cylinder rotor. , The flow at the apex of the conical shape of the inner cylinder rotor It is formed from a main inlet Tokaba crystallization析材cost solution injection to inject vortex, after which the crystallization析材cost solution of the horizontal inner cylinder rotating injected moved continuously in the reaction vessel crystallization product A slurry extractor is provided.

Further, in the present invention, the crystallization material solution is injected into the conical apex portion of the inner cylinder rotor from the main injection port of the front cover to form an injection vortex, and then the crystallization material While the vortex flow of the solution is continuously moved in the reaction tank toward the drive motor for the inner cylinder rotor, the crystallization is promoted, and the crystallized material solution whose crystallization is promoted is the end of the reaction tank. There is provided a crystallized product slurry extractor of a horizontal inner cylinder rotating type in which there is no crystallization accumulation through a crystallized material extraction port provided on the rotary side wall surface provided in the section. Is.

Further, in the present invention, the front cover installed at the distal end portion of the fixed hollow outer cylinder for covering the conical distal end portion of the inner cylinder rotor and forming the distal outer cylinder portion of the inner cylinder rotor is provided on the inner cylinder rotor. A horizontal inner cylinder rotation type crystallized product that is detachably attached to the outer cylinder end, and the inside of the fixed hollow outer cylinder forming the stirring and mixing unit, the inner cylinder rotor, and the reaction tank are cleaned by removing the front cover. A slurry extractor is provided.

The inner cylinder rotor forming the stirring and mixing unit according to the present invention removes the inner cylinder rotor from the rotation shaft in the rotation shaft meshing mechanism portion provided in the rotation shaft portion of the inner cylinder rotor after the front cover is removed. Crystallized product slurry extractor of horizontal inner cylinder rotation type that can take out the inner cylinder rotor from the fixed hollow outer cylinder and can be cleaned separately in the front cover, fixed hollow outer cylinder and inner cylinder rotor Is to provide.

The present invention relates to a continuous crystallization apparatus using an inner cylinder rotating type stirring mixer, wherein the stirring and mixing unit having a reaction tank formed by a gap between a fixed hollow outer cylinder and a rotatable inner cylinder rotor is provided on the drive motor side. The main inlet of the crystallization material solution into the inner cylinder rotor and the reaction tank can be installed on the other end of the cantilever structure on the side without the bearing mechanism. It is possible to configure the conical tip of the inner cylinder rotor at a position opposite to the main injection port of the crystallization material solution and inject the crystallization sample solution into the apex of the conical tip. An injection vortex can be formed at the tip of the conical shape of the inner cylinder rotor, and a stable continuous crystallization reaction can be efficiently obtained upon extraction of the crystallized product slurry.

Further, in the present invention, the crystallization material solution is formed into an injection vortex by injecting the crystallization material solution from the solution inlet of the front cover into the conical apex of the inner cylinder rotor, and then the crystallization material solution While the injected vortex flow continuously moves in the reaction tank toward the drive motor for the inner cylinder rotor, crystallization is promoted, and the crystallized material solution whose crystallization is promoted is the end of the reaction tank. In the rotating side wall surface provided on the rotating side wall surface, the crystallized material is extracted without any crystallization material extraction port provided at the time of the rotating side wall surface, so that the reactor always has a constant residence time. An inner-cylinder rotating type agitation mixer that continuously obtains a crystallized product slurry of the same quality can be provided.

Furthermore, the present invention covers the conical tip of the inner cylinder rotor, and the front cover installed at the tip of the fixed hollow outer cylinder to form the tip outer cylinder of the inner cylinder rotor is located outside the inner cylinder rotor. The inner cylinder rotor is configured to be detachably attached to the end of the cylinder portion, and the inner cylinder rotor is configured to be removable from a rotating shaft meshing mechanism portion provided in the rotating shaft core portion of the inner cylinder rotor after the front cover is removed. This makes it possible to provide a device that can easily clean the front cover, the fixed hollow outer cylinder, the inner cylinder rotor, and the reaction tank, and the inner cylinder rotating type stirring that is extremely efficient for each lot. A mixer is provided.

It is principal part sectional drawing explaining the inner cylinder rotation type stirring mixer of this invention. It is operation | movement explanatory drawing of the crystallization effect | action in this invention. It is cleaning operation explanatory drawing of this invention.

The present invention is a continuous crystallization apparatus using a stirring mixer of an inner cylinder rotation type, and can form a stable injection vortex in a reaction vessel as compared with a conventional apparatus, and a crystallization material, that is, a crystallization It is an object of the present invention to provide an inner cylinder rotating type stirring mixer capable of obtaining a stable continuous crystallization action when depositing a product slurry.

In addition, the present invention improves the shape of the tip of the inner cylinder rotor and the shape of the reaction tank formed by the fixed hollow outer cylinder and the inner cylinder rotor in a continuous crystallization apparatus using an inner cylinder rotating type mixer. In this way, a stable injection vortex can be sent into the reaction tank, and a mechanism that eliminates the crystallization liquid reservoir near the extraction port of the reaction tank is used to constantly react the reaction with a certain residence time. The present invention provides an inner cylinder rotating type stirring mixer that can be configured in a tank and can continuously obtain a crystallized product slurry of the same quality.

Furthermore, the present invention provides a continuous crystallization apparatus using an inner cylinder rotating type stirring mixer, wherein a cantilevered bearing mechanism is adopted as the rotation support mechanism of the apparatus, and the bearing mechanism is arranged at the other end of the cantilever mechanism. The new mechanism is configured so that the front end of the inner cylinder rotor is installed at the front end of the device, and the main inlet of the crystallization material solution can be installed at the center of the front cover. With this configuration, a stable injection vortex can be formed in the reaction tank by injecting the crystallization material solution from the main injection port into the conical tip provided at the tip of the inner cylinder rotor. In addition, the front cover is removed from the fixed hollow outer cylinder when the operation of the apparatus is stopped, so that the fixed hollow outer cylinder, the inner cylinder rotor, and the reaction tank forming the stirring and mixing unit can be easily cleaned. Provide a blender It is intended.

Thus, in the present invention, the stirring and mixing unit having a reaction tank in which a gap between a fixed hollow outer cylinder disposed on a coaxial central axis and a rotatable inner cylinder rotor is formed is horizontally installed. The drive motor side for the inner cylinder rotor of the stirring and mixing unit is attached to the gantry in a cantilever structure, and the inner cylinder rotor of the stirring and mixing unit is a conical tip that protrudes to the side without the bearing mechanism at the other end of the cantilever structure A front cover that covers the conical tip of the inner cylinder rotor is provided on the fixed hollow outer cylinder forming the outer cylinder of the inner cylinder rotor having the conical tip. A main inlet for injecting the crystallizing material solution into the reaction vessel is installed on the central axis, and the main inlet faces the conical apex of the conical tip of the inner cylinder rotor. A cone-shaped apex of the inner cylinder rotor An inner cylinder rotating type stirring mixer in which a crystallization material solution is injected from the main inlet of the front cover to form an injection vortex, and then the crystallization material solution is continuously injected and moved into the reaction vessel. It is preferable that

Further, in the present invention, the crystallization material solution is injected into the conical apex portion of the inner cylinder rotor from the main injection port of the front cover to form an injection vortex, and then the crystallization material While the vortex flow of the solution is continuously moved in the reaction tank toward the drive motor for the inner cylinder rotor, the crystallization is promoted, and the crystallized material solution whose crystallization is promoted is the end of the reaction tank. It is preferable that the rotating side wall surface provided in the section is extracted without any crystallization pool through the crystallization material extraction port provided at the rotating side wall surface.

Further, in the present invention, the front cover installed at the distal end portion of the fixed hollow outer cylinder for covering the conical distal end portion of the inner cylinder rotor and forming the distal outer cylinder portion of the inner cylinder rotor is provided on the inner cylinder rotor. It is preferable that the inside of the fixed hollow outer cylinder that forms the stirring and mixing unit, the inner cylinder rotor, and the reaction tank be cleaned by removing the front cover.

The inner cylinder rotor forming the stirring and mixing unit according to the present invention removes the inner cylinder rotor from the rotation shaft in the rotation shaft meshing mechanism portion provided in the rotation shaft portion of the inner cylinder rotor after the front cover is removed. Provided is an inner-cylinder rotating type agitator that can take out the inner-cylinder rotor from a fixed hollow outer cylinder and can be cleaned separately for the front cover, fixed hollow outer cylinder, and inner cylinder rotor. It is.

Thus, the present invention provides a stirring and mixing unit having a reaction tank in which a gap is formed between a fixed hollow outer cylinder and a rotatable inner cylinder rotor in a continuous crystallization apparatus using an inner cylinder rotating type stirring mixer. Is attached to the base in a cantilever structure on the drive motor side, so that the main inlet of the crystallization material solution to the inner cylinder rotor and the reaction vessel is installed on the other end of the cantilever structure on the side without the bearing mechanism. Therefore, the conical tip of the inner cylinder rotor is formed at a position facing the main inlet of the crystallization material solution, and the crystallization sample solution is injected into the apex of the conical tip. Therefore, an injection vortex can be formed at the tip of the conical shape of the inner cylinder rotor, and a stable continuous crystallization reaction can be efficiently obtained upon extraction of the crystallization slurry.

Further, in the present invention, the crystallization material solution is formed into an injection vortex by injecting the crystallization material solution from the solution inlet of the front cover into the conical apex of the inner cylinder rotor, and then the crystallization material solution While the injected vortex flow continuously moves in the reaction tank toward the drive motor for the inner cylinder rotor, crystallization is promoted, and the crystallized material solution whose crystallization is promoted is the end of the reaction tank. In the rotating side wall surface provided on the rotating side wall surface, the crystallized material is extracted without any crystallization material extraction port provided at the time of the rotating side wall surface, so that the reactor always has a constant residence time. An inner-cylinder rotating type agitation mixer that continuously obtains a crystallized product slurry of the same quality can be provided.

Furthermore, the present invention covers the conical tip of the inner cylinder rotor, and the front cover installed at the tip of the fixed hollow outer cylinder to form the tip outer cylinder of the inner cylinder rotor is located outside the inner cylinder rotor. The inner cylinder rotor is configured to be detachably attached to the end of the cylinder portion, and the inner cylinder rotor is configured to be removable from a rotating shaft meshing mechanism portion provided in the rotating shaft core portion of the inner cylinder rotor after the front cover is removed. This makes it possible to provide a device that can easily clean the front cover, the fixed hollow outer cylinder, the inner cylinder rotor, and the reaction tank, and the inner cylinder rotating type stirring that is extremely efficient for each lot. A mixer is provided.

FIG. 1 is a cross-sectional view of an essential part for explaining a first embodiment of the present invention. In FIG. 1, reference numeral 1 denotes a mounting table of the apparatus, and a horizontal and height-adjustable substrate 2 is installed on the mounting table 1, and the apparatus frame 3 and a housing incorporating a driving device and a control device are mounted on the substrate 2. 4 is installed, and a drive motor 6 is installed on the gantry 3 via a flange portion 5. The rotation of the drive motor 6 is supported in a cantilever structure by a transmission rotating shaft 7 and bearing portions 8a and 8b. Further, the rotation shaft 9 is connected to the rotary shaft 9, and the rotation of the drive motor 6 can be transmitted to the rotary side wall plate 11 and the inner cylinder rotor 12 provided in the stirring and mixing unit 10 at the tip portion.

Note that heat release openings 13 a, 13 b, 13 c... For the drive motor are provided in the vicinity of the drive motor 6 of the casing 4, and 14 a and 14 b are rotations fixed to the flange portion 5. The shaft cover cylinder 14 b is a rotating shaft cover cylinder 14 b having a cantilever structure support portion 15 incorporating the bearing portions 8 a and 8 b of the rotation shaft 9, and an air seal attached to the cantilever structure support portion 15. By installing the mechanism 16, sealing between the stirring and mixing unit 10 and the cantilever structure support unit 15 is achieved.

Thus, the members forming the stirring and mixing unit 10 include a fixed hollow outer cylinder 18 fixed to the rotary shaft cover cylinder 14b with bolts 17a, 17b, 17c, etc., and the fixed hollow outer cylinder. The rotatable inner cylinder rotor 12 that is inserted into the reaction tank 19 and constitutes the gap of the reaction tank 19, and the other end side of the cantilever structure integrated with the inner cylinder rotor 12, that is, the bearing portion 8a. , 8b, and a front cover 21 serving as a member covering the conical tip 20 provided at the tip of the inner cylinder rotor 12, the front cover 21 being fixed It attaches to the front-end | tip part of the hollow outer cylinder 18 so that attachment or detachment is possible with attachment bolt 22a, 22b, 22c ....

In addition, the stirring and mixing unit 10 horizontally includes a reaction tank 19 having a reaction tank 19 formed with a gap between a fixed hollow outer cylinder 18 disposed on the coaxial central axis C and a rotatable inner cylinder rotor 12. In the installed state, the front cover 21 is installed. On the central axis C of the front cover 21, a main inlet 24a for injecting the crystallization material solution 23a into the reaction tank 19 is installed, and the fixed hollow The outer cylinder 18 is provided with a sub inlet 24 b so that the crystallization material solution 23 b can be introduced into the reaction tank 19.

Further, the fixed hollow outer cylinder 18 is provided with a crystallization material extraction port 26 at the end of the reaction vessel 19 at the rotating side wall surface 25 of the rotating side wall plate 11. The opening 26 has a configuration in which the crystallized product slurry 27 is efficiently extracted without so-called crystallization pools, by being formed in the rotary side wall surface 25 of the rotary side wall plate 11.
Reference numeral 28 denotes a hot water or refrigerant inlet provided in the fixed hollow outer cylinder 18, and 29 denotes a hot water or refrigerant outlet provided in the fixed hollow outer cylinder 18, which is introduced through the hot water or refrigerant inlet 28. The heated water or refrigerant enters the chamber 30 provided in the fixed hollow outer cylinder 18 and heats or cools the inside of the reaction tank 19 formed by the inner wall of the fixed hollow outer cylinder 18 so that the crystallization material in the reaction tank 19 is heated. It has a structure that promotes crystallization.

Thus, FIG. 2 is a schematic diagram for explaining the operation of the crystallization action in the present invention. In FIG. 2, 10 is a stirring and mixing unit, 11 is a rotating side wall plate, 9 is a rotating shaft, 12 is an inner cylinder rotor, 18 is a fixed hollow outer cylinder, 19 is a reaction tank, and 20 is a tip of the reaction tank 19. The conical tip portion 20 is a front cover 21 that is detachably fixed to the fixed hollow outer cylinder 18.

Further, in the state where the stirring and mixing unit 10 having the reaction tank 19 in which a gap between the fixed hollow outer cylinder 18 disposed on the coaxial central axis C and the rotatable inner cylinder rotor 12 is formed is horizontally installed, the front A cover 21 is installed, and a main injection port 24 a for injecting the crystallization material solution 23 a into the reaction tank 19 is installed on the central axis C of the front cover 21. The crystallizing material solution 23b can be introduced into the reaction tank 19, and the fixed hollow outer cylinder 18 is connected to the rotating side wall surface of the rotating side wall plate 11 at the end of the reaction tank 19. 25, a crystallized material extraction port 26 is provided, and the crystallized material extraction port 26 is formed at the rotary side wall surface 25 of the rotary side wall plate 11 so that there is no crystallization pool. Efficiently extract crystallized slurry 27 It has a configuration that.

Further, the crystallization material solution 23a injected into the reaction tank 19 from the main injection port 24a can be injected toward the conical apex 31 of the conical tip 20 and can form a stable injection vortex. When the crystallizing material solution 23b for mixing is injected from the injection port 24b, a large spiral flow generated in the reaction tank 19 and a small flow having a periodicity to rotate are generated, and a continuous crystallization reaction is performed. It can be obtained efficiently.

Thus, the structural features of Example 1 are:
1) The inner cylinder rotor 12 and the reaction tank 19 are attached to the gantry 3 including the drive motor 6 and a control device (not shown) by a cantilever structure support portion 15.
2) The inner cylinder rotor 12 and the reaction tank 19 are provided at the other end of the cantilever structure support portion 15 so as to protrude to the side without the bearing portions 8a and 8b.
3) The main injection port 24a of the crystallization material solution 23a to the inner cylinder rotor 12 and the reaction tank 19 is installed at the center of the front cover 21 at the other end of the cantilever structure support unit 15, and the front cover 21 The crystallizing material solution 23a can be injected from the central portion toward the conical apex 31 of the conical tip 20 of the inner cylinder rotor 12.
4) A crystallization material extraction port 26 is provided at the end of the inner cylinder rotor 12 and the reaction tank 19 at the rotating side wall surface 25 of the rotating side wall plate 11. These are formed on the rotary side wall surface 25 of the rotary side wall plate 11.
It is said.

Thus, the first embodiment of the present invention has a stirring and mixing section 10 having a reaction tank 19 in which a gap is formed between a fixed hollow outer cylinder 18 and a rotatable inner cylinder rotor 12 arranged on a coaxial central axis C. Is attached to the gantry 3 in a cantilever structure, and the inner cylinder rotor 12 of the stirring and mixing unit 10 supports the cantilever structure. The fixed hollow outer cylinder 18 that has a conical tip 20 protruding to the side without the bearing mechanism at the other end of the portion 15 and forms the outer cylinder of the inner cylinder rotor 12 having the conical tip 20 Is provided with a front cover 21 covering the conical tip 20 of the inner cylinder rotor 12, and a main inlet 24a for injecting a crystallization material solution 23a into the reaction tank 19 on the central axis C of the front cover 21. Install the main inlet 2 a is provided opposite to the conical apex 31 of the conical tip 20 of the inner cylinder rotor 12, and the main inlet 24a of the front cover 21 is provided at the conical apex 31 of the inner rotor 12. The crystallization material solution 23a is injected from the crystallization material solution 23a to form an injection vortex, and then the crystallization material solution 23a is continuously injected into the reaction tank 19 by a horizontal inner cylinder rotating type crystallization product slurry extractor. It is to provide.

In Example 1 of the present invention, the crystallization material solution 23a is injected from the main inlet 24a of the front cover 21 into the conical apex 31 of the inner cylinder rotor 12 to form an injection vortex, and then the crystal While the injection vortex of the crystallization material solution 23a continuously moves in the reaction tank 19 to the drive motor 6 side for the inner cylinder rotor, crystallization is promoted, and the crystallization material solution 23a in which the crystallization is promoted is promoted. The crystallized product slurry is extracted from the rotary side wall surface 25 of the rotary side wall plate 11 provided at the end in the reaction tank 19 through the crystallized material extraction port 26 provided at the rotary side wall surface 25. A crystallized product slurry extractor of a horizontal inner cylinder rotation type is provided.

In Example 1, a continuous crystallization apparatus using an inner cylinder rotating type stirring mixer includes a stirring and mixing unit having a reaction tank formed by a gap between a fixed hollow outer cylinder and a rotatable inner cylinder rotor. The main injection port of the crystallization material solution into the inner cylinder rotor and the reaction vessel should be installed on the other end of the cantilever structure on the side without the bearing mechanism by attaching it to the gantry with a cantilever structure on the drive motor side. Therefore, it is possible to configure the conical tip of the inner cylinder rotor at a position opposite to the main inlet of the crystallization material solution and inject the crystallization sample solution into the apex of the conical tip. The injection vortex can be formed at the conical tip of the inner cylinder rotor, and a stable continuous crystallization reaction can be efficiently obtained during the extraction of the crystallization slurry.

Further, in the present invention, the crystallization material solution is formed into an injection vortex by injecting the crystallization material solution from the solution inlet of the front cover into the conical apex of the inner cylinder rotor, and then the crystallization material solution While the injected vortex flow continuously moves in the reaction tank toward the drive motor for the inner cylinder rotor, crystallization is promoted, and the crystallized material solution whose crystallization is promoted is the end of the reaction tank. In the rotating side wall surface provided on the rotating side wall surface, the crystallized material is extracted without any crystallization material extraction port provided at the time of the rotating side wall surface, so that the reactor always has a constant residence time. An inner-cylinder rotating type agitation mixer that continuously obtains a crystallized product slurry of the same quality can be provided.

FIG. 3 is a cross-sectional view of a main part for explaining the second embodiment of the present invention. In FIG. 3, the same reference numerals as those in FIG. 1 denote the same components, 1 is a mounting table for the apparatus, and a horizontal and height-adjustable substrate 2 is installed on the mounting table 1. A gantry 3 and a housing 4 are installed, and a driving motor 6 is installed on the gantry 3 via a flange portion 5. The driving motor 6 is rotated by a transmission rotating shaft 7 and bearing portions 8a and 8b. It is connected to the rotating shaft 9 supported by the holding structure, and is configured so that the rotation of the drive motor 6 can be transmitted to the rotating side wall plate 11 and the inner cylinder rotor 12 provided in the stirring and mixing unit 10 at the tip part. Yes.

The members forming the stirring and mixing unit 10 are inserted into the fixed hollow outer cylinder 18 fixed to the rotary shaft cover cylinder 14b with bolts 17a, 17b, 17c. The rotatable inner cylinder rotor 12 that is attached and constitutes the gap portion of the reaction tank 19, and the other end side of the cantilever structure integrated with the inner cylinder rotor 12, that is, without the bearing portions 8a and 8b. A conical tip 20 projecting to the side and a front cover 21 serving as a member covering the conical tip 20 provided at the tip of the inner cylinder rotor 12, the front cover 21 being the fixed hollow outer cylinder 18. Are fixed detachably by mounting bolts 22a, 22b, 22c...

Thus, in the second embodiment of the present invention, as shown in FIG. 3, the operation of the apparatus is stopped, the mounting bolts 22a, 22b, 22c... Are removed, and the front cover 21 is fixed to the fixed hollow outer cylinder 18. It shows a more removed state.

Therefore, the front cover 21 installed at the tip of the fixed hollow outer cylinder 18 to cover the conical tip 20 of the inner cylinder rotor 12 and form the tip outer cylinder of the inner cylinder rotor 12 is a cantilever structure support. 15 can be easily removed on the other end side, that is, the side without the bearing portions 8a and 8b, and the inside of the fixed hollow outer cylinder 18 forming the stirring and mixing section 10, the inner cylinder rotor 12 and the reaction tank 19 The present invention provides a horizontal inner cylinder rotation type crystallized product slurry extractor that can be easily and easily cleaned .

As another example of the second embodiment, the inner cylinder rotor 12 forming the agitation and mixing unit 10 has a rotary shaft meshing mechanism unit 32 provided in the rotary shaft core of the inner cylinder rotor 12 after the front cover 21 is removed. By being configured to be removable, the inner cylinder rotor 12 can be removed from the reaction tank 19 and disassembled into the front cover 21, the fixed hollow outer cylinder 18, and the inner cylinder rotor 12, and can be individually cleaned. A crystallized product slurry extractor of a horizontal inner cylinder rotation type is provided.

DESCRIPTION OF SYMBOLS 1 Mounting base 2 Board | substrate 3 Mounting base 4 Housing | casing 5 Flange part 6 Drive motor 7 Transmission rotational shaft 8a, 8b Bearing part 9 Rotary shaft 10 Stirring mixing part 11 Rotary side wall board 12 Inner cylinder rotor 13a, 13b, 13c ... Heat release Opening 14a, 14b Rotating shaft cover cylinder 15 Cantilever structure support 16 Air seal mechanism 17a, 17b, 17c ... Bolt 18 Fixed hollow outer cylinder 19 Reaction tank 20 Conical tip 21 Front cover 22a, 22b, 22c .. Mounting bolt 23a Crystallization material solution 23b Crystallization material solution 24a Main injection port 24b Sub injection port 25 Rotating side wall surface 26 Crystallization material extraction port 27 Crystallized product slurry 28 Hot water or refrigerant inlet 29 Hot water or refrigerant Discharge port 30 chamber 31 conical apex 32 rotating shaft engagement mechanism C central axis

Claims (3)

In an inner cylinder rotating type stirring mixer that applies Taylor's flow as an apparatus that enables crystallization of a specific crystal form,
In a state where the stirring and mixing unit 10 having a reaction tank 19 formed by a gap between a fixed hollow outer cylinder 18 and a rotatable inner cylinder rotor 12 disposed on the central axis C of the horizontal coaxial axis is horizontally installed,
The drive motor 6 side for the inner cylinder rotor 12 of the stirring and mixing unit 10 is attached to the gantry 3 with a cantilever structure support unit 15;
The inner cylinder rotor 12 of the stirring and mixing unit 10 has a conical tip 20 that protrudes from the other end of the cantilever structure support 15 to the side without the bearings 8a and 8b.
The fixed hollow outer cylinder 18 forming the outer cylinder portion of the inner cylinder rotor 12 having the conical tip portion 20 is provided with a front cover 21 that covers the conical tip portion 20 of the inner cylinder rotor 12,
On the central axis C of the front cover 21, a main injection port 24a for injecting a crystallization material solution into the reaction tank 19 is installed,
The main inlet 24a is provided to face the conical apex 31 of the conical tip 20 of the inner cylinder rotor 12,
The crystallization material solution 23a is injected into the conical apex portion 31 of the inner cylinder rotor 12 from the main injection port 24a of the front cover 21 to form an injection vortex at the conical tip portion 20,
Thereafter, the vortex flow of the crystallization material solution 23a is continuously moved in the reaction tank 19 toward the drive motor 6 for the inner cylinder rotor 12, and crystallization is promoted.
The crystallized material solution 23 a in which the crystallization is promoted is a rotating side wall surface 25 provided at an end in the reaction tank 19 through a crystallizing material extraction port 26 provided on the rotating side wall surface 25. A horizontal inner cylinder rotation type crystallized product slurry extractor characterized by being extracted as a crystallized product slurry 27. A front cover 21 installed at the tip of the fixed hollow outer cylinder 18 to cover the conical tip 20 of the inner cylinder rotor 12 and form the tip outer cylinder of the inner cylinder rotor 12 is provided outside the inner cylinder rotor 12. It is detachably attached to the end of the tube,
The cleaning of the stirring and mixing unit 10 formed by the reaction tank 19 formed by the gap between the fixed hollow outer cylinder 18 and the inner cylinder rotor 12 is performed by removing the front cover 21. Horizontal inner cylinder rotation type crystallized product slurry extractor. The inner cylinder rotor 12 forming the reaction tank 19 can be removed from the rotating shaft meshing mechanism portion 32 provided in the rotating shaft core portion of the inner cylinder rotor 12 after the front cover 21 is removed,
The horizontal inner cylinder rotation type crystallization according to claim 1, wherein the front cover 21, the fixed hollow outer cylinder 18 and the inner cylinder rotor 12 can be separately cleaned. Slurry extractor.

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