Rapid cooling device for benzyl hydroxamic acid crystallization

Abstract

This invention discloses a rapid cooling device for the crystallization of benzohydroxyxamic acid, specifically relating to the field of chemical synthesis equipment technology. It includes a centrifuge cylinder body with a crystallization assembly mounted on it. The crystallization assembly includes an inner liner cylinder positioned at the top of the centrifuge cylinder body. This invention significantly increases the crystal adhesion area by using multiple layers of rough-surfaced crystal-adhering disks combined with spiral elastic ribs. Furthermore, both the crystal-adhering disks and the elastic ribs are hollow structures, allowing for the introduction of cooling media to achieve active cooling and enhance crystal precipitation. This solves the core defect of existing devices that are difficult for crystals to adhere to. By employing a heat exchange chamber between the separator cylinder and the inner liner cylinder, and an internal cooling channel, a dual cooling design is achieved. The cooling media can comprehensively cover the crystallization area. Combined with the centrifugal diffusion effect brought about by the rotation of the sieve cylinder, the reaction liquid is rapidly reduced to the target temperature, forming a stable supersaturation and ensuring regular crystal morphology and achieving the required purity.

Description

Technical Field

[0001] This invention relates to the field of chemical synthesis equipment technology, and more specifically, to a rapid cooling device for the crystallization of benzohydroxyxamic acid. Background Technology

[0002] Benzyl hydroxamic acid is an organic compound belonging to the hydroxamic acid derivatives. Crystallization is a key process for the purification and separation of benzoyl hydroxamic acid (usually obtained by crystallizing its reaction solution after concentration). "Rapid cooling" is a commonly used operation in industrial production. Its core purpose is to optimize the yield, purity, morphology and process efficiency of the crystallized product. Rapid cooling can quickly lower the solution temperature to a low temperature range, causing a sharp drop in solubility and instantaneously forming a high degree of supersaturation, which promotes the rapid precipitation of a large amount of solute in crystal form.

[0003] Among them, the patent with announcement number CN208032564U discloses an apparatus for producing benzohydroxyxamic acid, including a tank body and a tank cover. The tank body is provided with a jacket, and the tank cover is provided with a stirring motor. The stirring motor is connected to a stirring shaft that extends into the tank body. The stirring shaft is provided with stirring blades. The stirring motor on the tank cover is provided with two material addition ports on both sides. The upper part of one side of the tank body is provided with a steam inlet that connects to the jacket, and the opposite side is provided with a steam outlet that connects to the jacket. The upper part of one side of the tank body is provided with several cooling pipes that penetrate the jacket and extend into the tank body. The cooling pipes penetrate the jacket from the upper part of the other side of the tank body and extend out of the tank body.

[0004] When in use, this structure, with its simultaneous heating jacket and cooling pipes, allows for separate heating or cooling of the tank, enabling effective temperature adjustment according to the reaction progress. This rapid adjustment ensures stable final product quality. However, the lack of a dedicated crystal-coating structure during crystallization makes it difficult for benzohydroxyxamic acid crystals to adhere and precipitate efficiently. Insufficient contact between the reaction liquid and the cooling structure results in low raw material crystallization efficiency, failing to meet the high-efficiency requirements for crystallization yield and purity in industrial production. Summary of the Invention

[0005] In order to overcome the above-mentioned defects of the prior art, the present invention provides a rapid cooling device for benzyl hydroxamic acid crystallization, which aims to solve the problems mentioned in the background art.

[0006] The present invention provides the following technical solution: a rapid cooling device for the crystallization of benzohydroxyxamic acid, comprising a centrifuge cylinder body, wherein a crystallization component is provided on the centrifuge cylinder body;

[0007] The crystallization assembly includes an inner liner cylinder disposed at the top of the centrifuge cylinder body, a partition cylinder disposed in the middle of the inner liner cylinder, and a heat exchange cavity formed between the partition cylinder and the inner liner cylinder, a sieve cylinder disposed in the middle of the partition cylinder, a support ring disposed at the bottom of the inner cavity of the sieve cylinder, a reciprocating screw disposed in the middle of the support ring, and a hollow guide shroud that can be adjusted up and down is threaded to the outer side of the reciprocating screw, and an elastic sealing cover is provided on the top of the hollow guide shroud;

[0008] The hollow flow guide is hinged to the outside of several extension tubes, and each extension tube is provided with a mounting base at one end. A reinforcing tube is provided on the mounting base, and several crystal-adhesive disks are sleeved on the outside of the reinforcing tubes. Elastic ribs are provided between each pair of adjacent crystal-adhesive disks.

[0009] Optionally, in a possible implementation, a hinge seat is hinged to one side of the top of the inner liner, a cover plate is provided at the top of the hinge seat, the cover plate covers the top of the inner liner, a rotating shaft is rotatably connected to the cover plate, a clamping plate is fixedly provided at one end of the rotating shaft, a first motor for driving the rotating shaft to rotate is provided on the cover plate, and a slot is opened at the top of the reciprocating screw, and the clamping plate extends into the slot.

[0010] Optionally, in a possible implementation, a hydraulic rod is provided on one side of the inner liner, the bottom end of the hydraulic rod is hinged to the centrifuge body, the output end of the hydraulic rod extends to the bottom of the hinge seat and is rotatably connected to the hinge seat, a heat exchange tube is provided on the outside of the centrifuge body, a mounting plate is provided at one end of the heat exchange tube, the mounting plate is located at the bottom of the separator, a sealing ring is provided at the top of the sieve cylinder, the sealing ring abuts against the top of the inner cavity of the cover plate, a second motor is provided at the bottom of the mounting plate, a support ring is provided at the output end of the second motor, the support ring is located at the bottom of the separator, multiple crystal-adhering disks are stacked, and each pair of adjacent crystal-adhering disks are connected to the elastic ribs, the elastic ribs are spiral in shape, and both the elastic ribs and the crystal-adhering disks are hollow, multiple extension tubes and reinforcing tubes are inclined upwards, and the top of the support ring abuts against the bottom of the extension tube, so that the reciprocating screw rotates to drive the hollow guide shroud to move upwards to adjust the angle of the extension tube;

[0011] The technical effects and advantages of this invention are as follows:

[0012] 1. This invention significantly increases the crystal adhesion area by setting up a multi-layered rough surface crystal-adhesive disk and combining it with spiral elastic ribs; and both the crystal-adhesive disk and the elastic ribs are hollow structures, which can be circulated with cooling medium to achieve active cooling, enhance the crystal precipitation dynamics, solve the core defect of existing devices that are not easy to adhere to crystals, and significantly improve the crystallization reaction efficiency.

[0013] 2. This invention achieves a dual cooling design by using a heat exchange chamber between the separator and the inner liner, and internal cooling channels including a hollow guide shroud, extension tube, reinforcing tube, crystal-adhering disk, and elastic ribs. The cooling medium can cover the crystallization area in all directions. Combined with the centrifugal diffusion effect brought about by the rotation of the sieve cylinder, the reaction liquid is rapidly reduced to the target temperature, forming a stable supersaturation, ensuring that the crystal morphology is regular and the purity meets the standards.

[0014] 3. This invention uses a reciprocating screw to drive the hollow guide hood up and down, which can adjust the tilt angle between the extension tube and the crystal-adhering disk. It can dynamically adjust the spatial distribution of the crystal-adhering structure according to the amount of reaction liquid and the crystallization stage, avoiding crystallization dead zones and further improving the utilization rate of raw materials. At the same time, the crystal-adhering disk and the reinforcing tube are detachably connected, and the crystal-adhered components can be directly removed after crystallization without complicated separation steps. The sieve hole design of the sieve cylinder can also achieve preliminary separation of the reaction liquid and crystals, reducing subsequent processing costs.

[0015] In summary, by setting up multi-layered rough-surfaced crystal-adhering disks and combining them with spiral elastic ribs, the crystal adhesion area is significantly increased. Furthermore, both the crystal-adhering disks and elastic ribs are hollow structures, allowing for the introduction of cooling media to achieve active cooling, thus enhancing the crystal precipitation dynamics. This solves the core defect of existing devices that make crystal adhesion difficult, resulting in a significant improvement in crystallization reaction efficiency. By employing a heat exchange chamber between the separator and the inner liner, and internal cooling channels including a hollow guide hood, extension tube, reinforcing tube, crystal-adhering disks, and elastic ribs, a dual cooling design is achieved. The cooling media can comprehensively cover the crystallization area. Combined with the centrifugal diffusion effect brought about by the rotation of the sieve cylinder, the reaction liquid is rapidly reduced to the target temperature, forming a stable supersaturation, ensuring regular crystal morphology and meeting purity standards. Attached Figure Description

[0016] To more clearly illustrate the technical solutions in this disclosure, the accompanying drawings used in some embodiments will be briefly described below. Obviously, the drawings described below are only drawings of some embodiments of this disclosure, and those skilled in the art can obtain other drawings based on these drawings. In addition, the drawings described below can be regarded as schematic diagrams and are not intended to limit the actual size of the product, the actual flow of the method, the actual timing of the signals, etc. involved in the embodiments of this disclosure.

[0017] Figure 1 This is a front view of the overall structure of the present invention.

[0018] Figure 2 This is a schematic diagram of the sieve cylinder, sealing ring, separator cylinder, support ring, second motor, and mounting plate of the present invention.

[0019] Figure 3 This is a schematic diagram of the first motor, rotating shaft, clamping plate, cover plate, hinge seat, and hydraulic rod of the present invention.

[0020] Figure 4 This is a schematic diagram of the centrifuge cylinder body, inner liner, and heat exchange tube of the present invention.

[0021] Figure 5 This is a schematic diagram of the support ring, hollow guide shield, elastic sealing cover, reciprocating screw, reinforcing tube and elastic rib of the present invention.

[0022] Figure 6 This is a schematic diagram showing the assembly of the support ring, hollow flow guide, elastic sealing cover, reinforcing tube, crystal bonding disk, and elastic ribs of the present invention.

[0023] Figure 7 For the present invention Figure 6 Exploded view.

[0024] Figure 8 This is a view of the separator cylinder, second motor, support ring, and mounting plate of the present invention installed inside the inner liner cylinder.

[0025] The attached figures are labeled as follows: 1. Centrifuge body; 2. Inner liner; 3. Separator; 4. Sieve; 5. Support ring; 6. Reciprocating screw; 7. Hollow guide shroud; 8. Elastic sealing cover; 9. Extension tube; 10. Mounting base; 11. Reinforcing tube; 12. Crystal bonding plate; 13. Elastic rib; 14. Hinge seat; 15. Cover plate; 16. Rotating shaft; 17. Clamping plate; 18. First motor; 19. Hydraulic rod; 20. Heat exchange tube; 21. Second motor; 22. Support ring; 23. Mounting plate; 24. Sealing ring. Detailed Implementation

[0026] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0027] This embodiment discloses a rapid cooling device for benzyl hydroxamic acid crystallization, which aims to solve the problem that the existing benzyl hydroxamic acid crystallization device is not easy to adhere to crystals, resulting in low efficiency of raw material crystallization reaction.

[0028] Specifically, as shown in the attached document Figure 1 As shown, the device includes a centrifuge body 1, on which a crystallization assembly for achieving efficient crystallization of benzohydroxyxamic acid is mounted. The core structure of the crystallization assembly includes an inner liner 2 disposed at the top of the centrifuge body 1, as shown in the attached diagram. Figure 4 As shown, the inner liner 2 is fixedly connected to the centrifuge body 1, and the outer side of the inner liner 2 is in contact with the inner wall of the centrifuge body 1, providing stable support for the internal structure.

[0029] As attached Figure 1 and attached Figure 5 As shown, a partition cylinder 3 is fixedly installed in the middle of the inner liner cylinder 2. The partition cylinder 3 and the inner liner cylinder 2 are arranged coaxially, forming an annular heat exchange chamber. This heat exchange chamber is used for the flow of cooling medium, providing a basic cooling environment for the crystallization process. A sieve cylinder 4 is installed in the middle of the partition cylinder 3. The cylinder wall of the sieve cylinder 4 is covered with fine sieve holes, allowing the benzohydroxyxamic acid reaction solution to pass through while preventing crystal particles from falling. A sealing ring 24 is installed at its top. Figure 2 As shown, the sealing ring 24 is made of high-temperature resistant elastic material, which can enhance the sealing performance of the device.

[0030] The bottom of the inner cavity of the screen cylinder 4 is provided with a support ring 5. The support ring 5 has a ring structure and a reciprocating screw 6 is vertically arranged in the middle. The outer side of the reciprocating screw 6 is threaded with a hollow guide shroud 7. The hollow guide shroud 7 can be adjusted up and down under the rotation drive of the reciprocating screw 6. The top of the hollow guide shroud 7 is covered with an elastic sealing cover 8. The elastic sealing cover 8 is made of silicone and has good elasticity. It can deform synchronously with the movement of the hollow guide shroud 7 to ensure the sealing of the internal space.

[0031] As attached Figure 5 Appendix Figure 6 and attached Figure 7 As shown, several extension tubes 9 are uniformly hinged circumferentially on the outer side of the hollow flow guide hood 7. Each extension tube 9 has a mounting base 10 fixedly installed at its end away from the hollow flow guide hood 7. A reinforcing tube 11 is detachably connected to the mounting base 10. Several crystal-adhesive discs 12 are sleeved along the length of the reinforcing tube 11. The crystal-adhesive discs 12 are disc-shaped with a roughened surface to enhance the adhesion of benzoyl hydroxyxamic acid crystals. Elastic ribs 13 are provided between each pair of adjacent crystal-adhesive discs 12. The elastic ribs 13 are spiral-shaped, and both the elastic ribs 13 and the crystal-adhesive discs 12 are hollow structures, interconnected internally. The lower part of the hollow flow guide hood 7 is connected to the heat exchange cavity formed between the inner liner 2 and the partition cylinder 3, allowing the hollow flow guide hood 7 to gather the cooling medium and transport it to the extension tubes 9 and reinforcing tubes 11. The cooling medium flows through these channels, achieving active cooling of the crystal-adhesive discs 12 and further improving crystal precipitation efficiency.

[0032] Multiple extension tubes 9 and reinforcing tubes 11 are all inclined upwards. In the initial state, the top of the support ring 5 abuts against the bottom of the extension tube 9, providing support for the extension tube 9. When the reciprocating screw 6 rotates and drives the hollow guide shroud 7 to move up and down, the angle between the extension tube 9 and the vertical direction is adjusted, thereby changing the distribution angle of the crystal-adhering disk 12 to adapt to the needs of different crystallization stages.

[0033] As attached Figure 3As shown, a hinge seat 14 is hinged to one side of the top of the inner liner 2. A cover plate 15 is fixedly installed at the top of the hinge seat 14. The size of the cover plate 15 matches the top opening of the inner liner 2, and it can completely cover the top of the inner liner 2. When the cover plate 15 is closed, the sealing ring 24 at the top of the screen cylinder 4 abuts against the top of the inner cavity of the cover plate 15, thereby sealing the internal space of the screen cylinder 4. A rotating shaft 16 is rotatably connected to the cover plate 15. The rotating shaft 16 is arranged radially along the cover plate 15, and a clamping plate 17 is fixedly installed at one end of it. A first motor 18 for driving the rotating shaft 16 to rotate is also fixedly installed on the cover plate 15. The output shaft of the first motor 18 is connected to the end of the rotating shaft 16 away from the clamping plate 17 through a coupling. Correspondingly, the top of the reciprocating screw 6 is provided with a slot that matches the clamping plate 17. When the cover plate 15 is closed, the clamping plate 17 can extend into the slot and drive the rotating shaft 16 to rotate through the first motor 18, thereby driving the reciprocating screw 6 to rotate synchronously.

[0034] A hydraulic rod 19 is provided on one side of the inner liner 2. The bottom end of the hydraulic rod 19 is hinged to the outer wall of the centrifuge body 1, and its output end extends to the bottom of the hinge seat 14 and is rotatably connected to the hinge seat 14. Through the extension and retraction of the hydraulic rod 19, the hinge seat 14 can be driven to rotate around the hinge point, thereby realizing the opening and closing operation of the cover plate 15.

[0035] As attached Figure 4 As shown, a heat exchange tube 20 is installed on the outside of the centrifuge body 1. The heat exchange tube 20 is a metal heat-conducting tube, one end of which passes through the side wall of the centrifuge body 1 and the inner liner 2, extends to the bottom of the separator 3 and is connected to a mounting plate 23, as shown in the attached figure. Figure 2 and 8 As shown, a second motor 21 is fixedly installed at the bottom of the mounting plate 23. The output end of the second motor 21 extends upward and is fixedly installed with a support ring 22. The support ring 22 is sleeved on the bottom of the outer side of the separator cylinder 3 and is fixedly connected to the separator cylinder 3. The second motor 21 can drive the separator cylinder 3 and the internal sieve cylinder 4 and other structures to rotate synchronously to achieve centrifugal effect.

[0036] The specific working principle is as follows: the hydraulic rod 19 is in the retracted state, the cover plate 15 is in the open state, and the operator injects the concentrated benzohydroxyoxime acid reaction solution into the sieve cylinder 4 until the surface of the reaction solution covers the top layer of the crystal-adhering disk 12.

[0037] The hydraulic rod 19 is extended, driving the hinge seat 14 to rotate, causing the cover plate 15 to close. At this time, the sealing ring 24 is in close contact with the cover plate 15 to achieve a seal. Then, the first motor 18 is started, driving the rotating shaft 16 to rotate, so that the clamping plate 17 is engaged in the groove at the top of the reciprocating screw 6 and rotates at the same time.

[0038] Cooling medium is introduced into heat exchange tube 20. The cooling medium enters the heat exchange cavity between partition cylinder 3 and inner liner cylinder 2 through mounting plate 23. At the same time, the cooling medium also enters the interior of reinforcing tube 11 and elastic rib 13 through hollow guide shroud 7 and extension pipe 9 to comprehensively cool the crystal-adhering disk 12. The cooled medium is discharged from the other end of the heat exchange cavity through the pipeline to form a circulating cooling system.

[0039] The second motor 21 is started, and the second motor 21 drives the separator cylinder 3 and the sieve cylinder 4 to rotate synchronously through the support ring 22. The reaction liquid in the sieve cylinder 4 diffuses to the surroundings under the action of centrifugal force and comes into full contact with the cooled crystal-adhering disk 12. Because the surface of the crystal-adhering disk 12 is rough and the temperature is low, benzohydroxyxamic acid quickly precipitates and adheres to its surface.

[0040] During the crystallization process, the reciprocating screw 6 can be rotated by the first motor 18, causing the hollow guide shroud 7 to move slowly up and down, which in turn drives the support ring 5 to move synchronously. This adjusts the tilt angle of the extension tube 9, changes the spatial position of the crystal-binding disk 12, and ensures that the reaction liquid is in full contact with all areas of the crystal-binding disk 12, avoiding crystallization dead zones. At the same time, the spiral elastic ribs 13 vibrate slightly during the rotation of the device, which can promote uniform crystal growth, and their hollow structure can further enhance the cooling effect.

[0041] After crystallization is completed, the second motor 21 and the cooling medium supply are turned off, and the hydraulic rod 19 is controlled to retract and open the cover plate 15. The reinforcing tube 11 and the crystal-adhering disk 12 with crystals on its surface are taken out to complete the crystal collection. The small amount of uncrystallized reaction liquid in the sieve cylinder 4 can flow into the heat exchange chamber through the sieve holes and be collected through the subsequent recovery pipeline.

[0042] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A rapid cooling device for benzyl hydroxamic acid crystallization, comprising a centrifuge tube body (1), characterized in that: A crystallization assembly is provided on the main body (1) of the centrifuge tube; The crystallization assembly includes an inner liner (2) disposed at the top of the centrifuge body (1), a separator (3) disposed in the middle of the inner liner (2), and a heat exchange chamber formed between the separator (3) and the inner liner (2). A sieve (4) is disposed in the middle of the separator (3), a support ring (5) is disposed at the bottom of the inner cavity of the sieve (4), a reciprocating screw (6) is disposed in the middle of the support ring (5), and a hollow guide shroud (7) that is adjustable up and down is threaded on the outer side of the reciprocating screw (6), and an elastic sealing cover (8) is provided on the top of the hollow guide shroud (7). The hollow flow guide (7) has several extension tubes (9) hinged to its outer side, and each extension tube (9) has a mounting base (10) at one end. The mounting base (10) has a reinforcing tube (11), and the reinforcing tube (11) has several crystal-adhesive disks (12) sleeved on its outer side. Elastic ribs (13) are respectively provided between each two adjacent crystal-adhesive disks (12).

2. The rapid cooling device for benzyl hydroxamic acid crystallization according to claim 1, characterized in that: A hinge seat (14) is hinged to one side of the top of the inner liner (2), and a cover plate (15) is provided at the top of the hinge seat (14), which covers the top of the inner liner (2).

3. The rapid cooling device for benzyl hydroxamic acid crystallization according to claim 2, characterized in that: A rotating shaft (16) is rotatably connected to the cover plate (15), and a clamping plate (17) is fixedly provided at one end of the rotating shaft (16). A first motor (18) for driving the rotating shaft (16) to rotate is provided on the cover plate (15).

4. The rapid cooling device for benzyl hydroxamic acid crystallization according to claim 3, characterized in that: The top end of the reciprocating lead screw (6) is provided with a slot, and the locking plate (17) extends into the slot.

5. The rapid cooling device for benzyl hydroxamic acid crystallization according to claim 2, characterized in that: A hydraulic rod (19) is provided on one side of the inner liner (2). The bottom end of the hydraulic rod (19) is hinged to the centrifuge body (1). The output end of the hydraulic rod (19) extends to the bottom of the hinge seat (14) and is rotatably connected to the hinge seat (14).

6. The rapid cooling device for benzyl hydroxamic acid crystallization according to claim 1, characterized in that: A heat exchange tube (20) is provided on the outside of the centrifuge body (1), and an installation plate (23) is provided at one end of the heat exchange tube (20). The installation plate (23) is located at the bottom of the separator (3).

7. The rapid cooling device for benzyl hydroxamic acid crystallization according to claim 6, characterized in that: The bottom of the mounting plate (23) is provided with a second motor (21), and the output end of the second motor (21) is provided with a support ring (22), which is located at the bottom of the separator (3).

8. The rapid cooling device for benzyl hydroxamic acid crystallization according to claim 2, characterized in that: A sealing ring (24) is provided at the top of the sieve cylinder (4), and the sealing ring (24) abuts against the top of the inner cavity of the cover plate (15).

9. The rapid cooling device for benzyl hydroxamic acid crystallization according to claim 1, characterized in that: Multiple bonding disks (12) are stacked, and each pair of adjacent bonding disks (12) are connected to an elastic rib (13). The elastic rib (13) is spiral in shape, and both the elastic rib (13) and the bonding disk (12) are hollow.

10. The rapid cooling device for benzyl hydroxamic acid crystallization according to claim 1, characterized in that: Multiple extension tubes (9) and reinforcing tubes (11) are inclined upwards, and the top of the support ring (5) abuts against the bottom of the extension tube (9) so that the reciprocating screw (6) rotates to drive the hollow guide shroud (7) to move up and down to adjust the angle of the extension tube (9).

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