Cooling crystallization device

Abstract

The utility model provides a cooling crystallization device which comprises a distillation kettle with a jacket on the outer wall and a crystallization kettle, the bottom of the distillation kettle is communicated with the crystallization kettle through a guide pipe, a motor is mounted at the top of the crystallization kettle, a discharge pipe is arranged at the bottom of the crystallization kettle, a vertical pipe inserted from the top of the crystallization kettle is fixed on an output shaft of the motor, and a stirring rod is fixed on the vertical pipe in the crystallization kettle. A cold water pipe with one end communicated with the jacket is horizontally inserted into the crystallization kettle, the lower end of the vertical pipe is rotatably communicated with the cold water pipe, the upper end of the vertical pipe is sleeved and rotatably connected with a sleeve communicated with the water outlet pipe I, and the upper end of the jacket of the crystallization kettle is communicated with the water outlet pipe II. According to the cooling crystallization device, the inside and outside of a solution in the crystallization kettle can be uniformly and continuously cooled through the jacket and the vertical pipe, the cooling crystallization efficiency is improved, and separated crystals are prevented from being dissolved again in the stirring process. Meanwhile, when the cold source circulates in the pipe, the motor is not influenced to drive the vertical pipe to rotate so as to drive the stirring rod to stir the solution in the crystallization kettle.

Description

Technical Field

[0001] This application relates to a cooling crystallization technique in the preparation of dimethomorph, and more particularly to a cooling crystallization apparatus. Background Technology

[0002] In the preparation of dimethomorph, the solution is acid-washed and water-washed, then distilled in a distillation kettle to remove part of the solvent. The remaining solution after distillation is discharged into a crystallization kettle for cooling and crystallization. Then, it is filtered, pressed into a filter cake, washed, and dried to obtain dimethomorph.

[0003] Existing cooling crystallization devices cool the solution from the outside in by injecting a cold source into the jacket after it is filled. This uneven cooling results in the solution near the inner wall of the vessel cooling and crystallizing earlier than the solution in the center. The crystals accumulated on the inner wall affect heat transfer and reduce crystallization efficiency. Furthermore, in existing cooling crystallization devices, the crystals on the inner wall dissolve again during stirring as they move towards the center of the solution due to the higher temperature at the center. Utility Model Content

[0004] This application provides a cooling crystallization device to solve the problem of uneven cooling of the solution inside and outside the vessel in existing cooling crystallization devices.

[0005] This application provides a cooling crystallization device, including a distillation vessel with a jacket on the outer wall and a crystallization vessel. The bottom of the distillation vessel is connected to the crystallization vessel through a feed pipe. A motor is installed on the top of the crystallization vessel, and a discharge pipe is provided at the bottom. A vertical pipe inserted from the top of the crystallization vessel is fixed on the output shaft of the motor. A stirring rod is fixed on the vertical pipe inside the crystallization vessel. A cold water pipe with one end connected to its jacket is horizontally inserted inside the crystallization vessel. The lower end of the vertical pipe is rotatably connected to the cold water pipe, and the upper end is fitted with and rotatably connected to a sleeve connected to a water outlet pipe. The upper end of the jacket of the crystallization vessel is connected to a water outlet pipe.

[0006] Optionally, the stirring rod fixed on the vertical pipe is a stirring branch pipe that is circulated and connected to the vertical pipe.

[0007] Optionally, a paddle wheel for pushing liquid in a vertical direction is fitted and fixed on the vertical pipe.

[0008] Optionally, the first water outlet pipe and the second water outlet pipe are connected to the jacket on the distillation vessel, and a heater is installed at the lower end of the jacket of the distillation vessel.

[0009] The cooling crystallization device provided in this application has a cold water pipe connected to both the jacket and the vertical pipe serving as a rotating shaft on the crystallization vessel. This allows for uniform and continuous cooling of the solution inside and outside the crystallization vessel, improving the efficiency of cooling crystallization and preventing the precipitated crystals from redissolving during stirring. Simultaneously, the lower end of the vertical pipe is rotatably connected to the cold water pipe, and the upper end is rotatably connected to the outlet pipe via a sleeve. This ensures that the flow of cold water from the pipe does not affect the motor driving the vertical pipe to rotate and stir the solution inside the crystallization vessel. Attached Figure Description

[0010] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0011] Figure 1 This is a front view of a cooling crystallization apparatus provided in an embodiment of this application;

[0012] Figure 2 A cooling crystallization apparatus provided in one embodiment of this application Figure 1 Top view;

[0013] Figure 3 A cooling crystallization apparatus provided in one embodiment of this application Figure 1 A sectional view;

[0014] Figure 4 This is a cross-sectional view of the crystallization vessel of a cooling crystallization apparatus provided in an embodiment of this application.

[0015] Explanation of reference numerals in the attached figures:

[0016] 1. Distillation vessel; 2. Crystallization vessel; 3. Feed pipe; 4. Heater; 5. Exhaust pipe; 6. Motor; 7. Vertical pipe; 8. Cold water pipe; 9. Sleeve; 10. Water outlet pipe 1; 11. Water outlet pipe 2; 12. Stirring branch pipe; 13. Paddle wheel; 14. Discharge pipe. Detailed Implementation

[0017] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions in the embodiments of this application are described clearly and completely below. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. Based on the embodiments in this application, all other embodiments obtained by those skilled in the art without creative effort are also within the scope of protection of this application.

[0018] like Figures 1-4As shown, one embodiment of this application provides a cooling crystallization device, including a distillation vessel 1 with a jacket on its outer wall and a crystallization vessel 2. The bottom of the distillation vessel 1 is connected to the crystallization vessel 2 via a feed pipe 3. A motor 6 is installed on the top of the crystallization vessel 2, and a discharge pipe 14 is provided at the bottom. A vertical pipe 7 inserted from the top of the crystallization vessel 2 is fixed on the output shaft of the motor 6, and a stirring rod is fixed on the vertical pipe 7 inside the crystallization vessel 2. A cold water pipe 8 is horizontally inserted into the crystallization vessel 2, with one end connected to its jacket. The lower end of the vertical pipe 7 is rotatably connected to the cold water pipe 8, and the upper end is fitted with and rotatably connected to a sleeve 9 connected to a water outlet pipe 10. The upper end of the jacket of the crystallization vessel 2 is connected to a water outlet pipe 11.

[0019] In use, the solution after partial solvent removal through distillation in distillation vessel 1 enters crystallization vessel 2 through feed pipe 3. Solvent vapor generated during distillation is discharged through exhaust pipe 5. Simultaneously, a cold source is injected into the jacket and vertical pipe 7 of crystallization vessel 2 through cold water pipe 8, cooling the solution inside and outside the crystallization vessel 2 at the same time, causing dimethomorpholine crystals to precipitate from the solution. A water outlet is provided at the vertical pipe 7 fitted by sleeve 9. The vertical pipe 7 is rotatably connected to sleeve 9, and the cold source after cooling is discharged through water outlet pipe 10 and water outlet pipe 11. During the cooling and crystallization process, the rotation of vertical pipe 7 driven by motor 6 does not affect the flow of cold source within vertical pipe 7, and also drives the fixed stirring rod on vertical pipe 7 to rotate, stirring the solution in crystallization vessel 2 and dispersing the crystal particles evenly. Crystal particles precipitated at the bottom of crystallization vessel 2 are discharged through discharge pipe 14.

[0020] In this embodiment, the cold water pipe 8 is connected to both the jacket on the crystallizing vessel 2 and the vertical pipe 7, which serves as the rotating shaft. This allows for uniform and continuous cooling of the solution inside and outside the crystallizing vessel 2, improving the efficiency of cooling crystallization and preventing the precipitated crystals from dissolving again during stirring. Simultaneously, the lower end of the vertical pipe 7 is rotatably connected to the cold water pipe 8, and the upper end is rotatably connected to the outlet pipe 10 via the sleeve 9. This ensures that the flow of cold water from the pipe does not affect the motor 6's ability to drive the vertical pipe 7 to rotate and stir the solution inside the crystallizing vessel 2.

[0021] In one possible implementation, the stirring rod fixed on the vertical pipe 7 is a stirring branch pipe 12 that is circulatedly connected to the vertical pipe 7.

[0022] The cold source entering the vertical pipe 7 can flow and circulate into the hollow stirring branch pipe 12, further expanding the contact cooling area and crystallization effect of the cold source.

[0023] In one possible implementation, a paddle wheel 13 for pushing liquid in a vertical direction is fitted and fixed on the vertical pipe 7.

[0024] The paddle wheel 13 is driven to rotate by the vertical tube 7, which can push the solution in the vertical direction, so that the solution in the vertical direction participates in the circulation, which is conducive to the uniform formation and precipitation of crystals.

[0025] In one possible implementation, the first water outlet pipe 10 and the second water outlet pipe 11 are connected to the jacket on the distillation vessel 1, and a heater 4 is installed at the lower end of the jacket on the distillation vessel 1.

[0026] After the cold source in the jacket and vertical pipe 7 of the crystallizing vessel 2 is used, it flows into the jacket of the distillation vessel 1 through the water outlet pipe 10 and the water outlet pipe 11. The solution in the distillation vessel 1 is then heated by the heater 4 at the lower end of the jacket and distilled.

[0027] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this application.

Claims

1. A cooling crystallization apparatus, comprising a distillation vessel (1) with a jacket on its outer wall and a crystallization vessel (2), wherein the bottom of the distillation vessel (1) is connected to the crystallization vessel (2) via a feed pipe (3), and a motor (6) is installed on the top of the crystallization vessel (2), and a discharge pipe (14) is provided at the bottom, characterized in that: A vertical pipe (7) inserted from the top of the crystallizer (2) is fixed on the output shaft of the motor (6). A stirring rod is fixed on the vertical pipe (7) inside the crystallizer (2). A cold water pipe (8) with one end connected to its jacket is horizontally inserted inside the crystallizer (2). The lower end of the vertical pipe (7) is rotatably connected to the cold water pipe (8). The upper end is fitted with and rotatably connected to a sleeve (9) connected to the first water outlet pipe (10). The upper end of the jacket of the crystallizer (2) is connected to the second water outlet pipe (11).

2. The cooling crystallization apparatus according to claim 1, characterized in that: The stirring rod fixed on the vertical pipe (7) is a stirring branch pipe (12) that is circulatedly connected to the vertical pipe (7).

3. The cooling crystallization apparatus according to claim 2, characterized in that: A paddle wheel (13) for pushing liquid in the vertical direction is fixedly fitted on the vertical pipe (7).

4. The cooling crystallization apparatus according to any one of claims 1-3, characterized in that: The first water outlet pipe (10) and the second water outlet pipe (11) are connected to the jacket on the distillation vessel (1), and a heater (4) is installed at the lower end of the jacket of the distillation vessel (1).

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