A residual liquid neutralization kettle and its application in the preparation of 2,4-dichloro-5-fluorobenzoyl chloride

Abstract

The present invention relates to the technical field related to residual liquid treatment, and in particular to a residual liquid neutralization kettle and application thereof in the preparation of 2,4-dichloro-5-fluorobenzoyl chloride. The residual liquid neutralization kettle comprises a kettle body and a variable volume structure arranged in the kettle body; the variable volume structure divides the inner part of the kettle body into a reaction zone and a mixing zone distributed up and down, and comprises a disc body that is sealingly slidably arranged in the kettle body and has a volume depth, and a cover plate that is sealingly slidably arranged in the disc body; by arranging a disc body and a cover plate that can move relative to each other in the kettle body, the kettle body is separated into a reaction zone and a mixing zone distributed up and down, and this design has significant advantages in residual liquid treatment: when residual liquid is added to the kettle body and submerged in the cover plate, as the reaction proceeds, the pressure in the reaction zone gradually increases, and the cover plate slides on the disc body to realize automatic expansion of the reaction zone, which effectively avoids damage to the kettle body caused by excessive pressure in the reaction zone, thereby ensuring the safety and stability of the equipment.

Description

Technical Field

[0001] The present invention relates to the technical field related to residual liquid treatment, in particular to a residual liquid neutralization kettle and application thereof in the preparation of 2,4-dichloro-5-fluorobenzoyl chloride. Background Art

[0002] Amidst the booming chemical industry, the fine chemical sector is experiencing rapid development. The production of 2,4-dichloro-5-fluorobenzoyl chloride is undoubtedly a highly representative example. With the continued rise in global demand for fluorinated fine chemicals, these compounds are finding significant application in a wide range of fields, including pharmaceuticals, pesticides, and materials. However, their production process is not always smooth sailing, particularly with the handling of distillation residues, a persistent challenge for companies.

[0003] Thus, the residual liquid neutralization kettle came into being. By introducing the residual liquid neutralization kettle, enterprises can convert the distillation residual liquid, which was originally regarded as a burden, into a reusable resource. Since the neutralization reaction is an exothermic reaction, it is easy to cause the pressure in the kettle to be too high, which has an adverse effect on the kettle body. For this reason, some kettle bodies are equipped with corresponding pressure relief valves. When the pressure in the kettle is too high, the pressure relief valve opens to reduce the pressure. However, in the actual implementation, after the residual liquid and the neutralizing liquid are added, the neutralization reaction between the residual liquid and the neutralizing liquid in the kettle is relatively intense, and the heat release rate is relatively fast, which can easily cause the pressure in the kettle to be too high instantly. After the pressure relief valve is opened, it takes a certain amount of time for the pressure relief process to occur, making it difficult to provide timely and comprehensive protection for the kettle body. Summary of the Invention

[0004] The object of the present invention is to provide a residual liquid neutralization kettle and its application in the preparation of 2,4-dichloro-5-fluorobenzoyl chloride, so as to solve the problems raised in the above background technology.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] A residual liquid neutralization kettle, comprising a kettle body and a variable volume structure arranged in the kettle body;

[0007] The variable volume structure divides the inner portion of the kettle into a reaction zone and a mixing zone distributed vertically. The structure includes a deep-filled disc that is sealingly slidably disposed within the kettle, and a cover plate that is sealingly slidably disposed within the disc. A variable chamber is formed between the disc and the bottom wall of the cover plate.

[0008] A channel is formed between the disc and the cover plate so that the residual liquid added to the kettle can cover the cover plate, and the added neutralizing liquid can react with the residual liquid in the reaction zone, thereby promoting relative movement between the cover plate and the disc, reducing the variable chamber, and cooperating with the atomizing mechanism provided at the bottom of the disc;

[0009] The disc can be driven to rise by multiple lifting mechanisms provided on the kettle body, so that the reaction liquid in the reaction zone is discharged into the mixing zone in an atomized form through the channel and the atomization mechanism. At the same time, the flow disturbance mechanism provided in the kettle body is triggered to form turbulence in the mixing zone.

[0010] As a further solution of the present invention: the disk body and the cover plate are connected by multiple groups of elastic support structures, a plurality of first through holes are provided at the eccentric portion of the disk body, a plurality of second through holes are provided at the eccentric portion of the cover plate, and a corrugated tube is connected between each of the plurality of first through holes and the plurality of second through holes to form the channel.

[0011] As a further solution of the present invention, a first inlet and a second inlet are provided on the upper portion of the kettle body, and the first inlet and the second inlet are used for adding residual liquid and neutralizing liquid into the kettle body respectively.

[0012] As a further solution of the present invention: the elastic support structure includes a connecting column fixed to the bottom of the cover plate and sealed and slidably connected to the disk body, the end of the connecting column away from the cover plate is connected to the atomization mechanism, and the outer periphery of the connecting column is also sleeved with a cylindrical spring, the cylindrical spring is located in the variable chamber, and the two ends are respectively connected to the bottom wall of the disk body and the cover plate.

[0013] As a further solution of the present invention: the atomization mechanism includes a plurality of atomizing nozzles that are sealed and slidably arranged at the bottom of the disk body and adapted to the first through hole. The plurality of atomizing nozzles are respectively connected to the plurality of connecting columns through a group of transmission structures. When the variable chamber shrinks, the connecting columns can drive the atomizing nozzles to move radially along the disk body through the transmission structure until the atomizing nozzles coincide with the first through hole.

[0014] As a further solution of the present invention: the transmission structure includes two guide rails fixed to the bottom of the disk body and a movable seat slidably engaged between the two guide rails, the atomizing nozzle is installed on the movable seat, and a guide column is also fixed to the bottom of the disk body. A follower ring is slidably sleeved on the guide column, and the follower ring is fixed to the connecting column through a connecting arm, and a connecting rod is provided between the follower ring and the movable seat, the head end of the connecting rod is hinged to the follower ring, and the tail end is hinged to the movable seat.

[0015] As a further solution of the present invention: a mixing mechanism is also provided in the kettle body, and the mixing mechanism includes a driving motor installed on the top of the kettle body and a central vertical shaft connected to the output end of the driving motor and extending into the mixing zone, and the central vertical shaft is fixedly connected to a plurality of stirring blades located in the mixing zone, and the central vertical shaft sequentially passes through the cover plate and the disk body, and is sealed and slidably connected to the cover plate and the disk body.

[0016] As a further solution of the present invention: the spoiler mechanism includes a protrusion fixed on the inner wall of the kettle body, a rotating shaft rotatably mounted on the protrusion, and an arc-shaped spoiler fixed on the rotating shaft, the bottom of the plate body is fixedly connected to a ring body through a fixing frame, and the ring body is slidably fitted on the rotating shaft;

[0017] Among them, a convex column perpendicular to the rotating shaft is fixed on the ring body, and the convex column extends into a groove body provided on the outer wall of the rotating shaft and is slidingly connected to the rotating shaft. The groove body includes a first groove and a second groove connected to each other, the first groove is arranged in a spiral shape, and the second groove is arranged along the axial direction of the rotating shaft.

[0018] As a further solution of the present invention: the lifting mechanism includes a cylinder installed on the top of the kettle body and a riser slidingly arranged on the kettle body and fixedly connected to the movable end of the cylinder through an arc-shaped arm. The riser is fixed to the disc body and is also sealed and slidably connected to the cover plate.

[0019] The invention discloses an application of the residual liquid neutralization kettle in the preparation of 2,4-dichloro-5-fluorobenzoyl chloride.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] The present invention provides a relatively movable disc and cover plate in the kettle body to separate the kettle body into a reaction zone and a mixing zone distributed above and below. When the residual liquid is added to the kettle body and submerges the cover plate, as the reaction proceeds, the pressure in the reaction zone gradually increases, and the cover plate slides on the disc body to achieve automatic expansion of the reaction zone, effectively avoiding damage to the kettle body caused by excessive pressure in the reaction zone.

[0022] The capacity of the variable chamber formed between the disc and the cover gradually decreases as the reaction progresses, allowing the reaction zone to expand. When the neutralization reaction is intense and the pressure change is instantaneous, comprehensive protection of the kettle is achieved, ensuring the safety and stability of the equipment.

[0023] At the same time, by utilizing the high-pressure environment, the reaction liquid in the reaction zone is discharged into the mixing zone to generate atomization impact, which is conducive to the full fusion of the reaction liquid and the turbulence in the mixing zone, further improving the sufficiency and efficiency of the reaction, ensuring the uniform progress of the reaction, and improving the quality and yield of the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a structural schematic diagram of an embodiment of a residual liquid neutralization kettle.

[0025] Figure 2 It is a structural schematic diagram of another angle of an embodiment of the residual liquid neutralization kettle.

[0026] Figure 3 It is a structural schematic diagram of another angle of an embodiment of the residual liquid neutralization kettle.

[0027] Figure 4 This is a schematic diagram of the internal structure of the kettle body in one embodiment of the residual liquid neutralization kettle.

[0028] Figure 5 This is an exploded view of the internal structure of the residual liquid neutralization kettle in one embodiment.

[0029] Figure 6 It is a structural schematic diagram of the flow guide mechanism in one embodiment of the residual liquid neutralization kettle.

[0030] Figure 7 It is a structural schematic diagram of the variable volume structure in one embodiment of the residual liquid neutralization kettle.

[0031] Figure 8 This is an exploded view of the variable volume structure in one embodiment of the residual liquid neutralization kettle.

[0032] Figure 9 for Figure 8 Schematic diagram of the structure from another angle.

[0033] In the figure: 1. kettle body; 2. drive motor; 3. central vertical shaft; 4. stirring blade; 5. spoiler; 6. disc body; 601. first through hole; 602. limiting protrusion; 7. cover plate; 701. second through hole; 8. bellows; 9. connecting column; 10. cylindrical spring; 11. connecting arm; 12. follower ring; 13. guide column; 14. guide rail; 15. movable seat; 16. connecting rod; 17. atomizing nozzle; 18. protrusion block; 19. rotating shaft; 1901. first groove; 1902. second groove; 20. fixing frame; 21. ring body; 22. protrusion; 23. cylinder; 24. arc arm; 25. vertical pipe; 2501. first air hole; 2502. second air hole; 26. first inlet; 27. second inlet; 28. solenoid valve. DETAILED DESCRIPTION

[0034] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0035] In addition, when an element in the present invention is referred to as being "fixed to" or "disposed on" another element, it may be directly on the other element or there may be an intermediate element. When an element is referred to as being "connected to" another element, it may be directly connected to the other element or there may be an intermediate element. The terms "vertical," "horizontal," "left," "right," and similar expressions used herein are for illustrative purposes only and do not represent the only implementation method.

[0036] See also Figures 1-9 In an embodiment of the present invention, a residual liquid neutralization kettle comprises a kettle body 1 and a variable volume structure provided in the kettle body 1;

[0037] The variable volume structure divides the interior of the kettle body 1 into a reaction zone and a mixing zone distributed vertically. The variable volume structure includes a disc 6 with a volume depth and a cover plate 7 that is sealed and slidably disposed in the kettle body 1. A variable chamber is formed between the disc 6 and the bottom wall of the cover plate 7.

[0038] A channel is formed between the disc 6 and the cover plate 7 so that the residual liquid added to the kettle 1 can cover the cover plate 7, and the added neutralizing liquid can react with the residual liquid in the reaction zone, thereby promoting relative movement between the cover plate 7 and the disc 6, reducing the variable chamber, and cooperating with the atomizing mechanism provided at the bottom of the disc 6;

[0039] The disc 6 can be driven to rise by multiple lifting mechanisms provided on the kettle body 1, so that the reaction liquid in the reaction zone is discharged into the mixing zone in an atomized form through the channel and the atomization mechanism. At the same time, the flow disturbance mechanism provided in the kettle body 1 is triggered to form turbulence in the mixing zone.

[0040] It should be noted that the neutralizing solution is an alkaline solution, such as sodium hydroxide solution. The specific type is not specifically limited in this application and can be selected according to actual needs.

[0041] When using the neutralization kettle to treat residual liquid, the residual liquid is added to the kettle body 1 until the residual liquid covers the cover plate 7, and then the neutralizing liquid is added to the kettle body 1. Then, the neutralizing liquid and the residual liquid will undergo a neutralization reaction in the reaction zone of the kettle body 1;

[0042] The neutralization reaction is an exothermic reaction. The temperature of the system will rise during the reaction process. During the neutralization reaction, a large amount of heat will be released, which may cause the pressure in the reaction zone to rise. Then, the cover plate 7 will move relative to the disk body 6. Specifically, the cover plate 7 moves toward the bottom wall of the disk body 6, the capacity of the variable chamber decreases, and the space of the reaction zone increases. Therefore, the effect of automatic expansion according to the degree of reaction is achieved, which can effectively avoid the local pressure inside the kettle body 1 being too high during the treatment process, thereby causing damage to the kettle body 1.

[0043] When the reaction in the reaction zone is completed (at this time, the residual liquid and the neutralizing liquid in the reaction zone may not react fully), the lifting mechanism works to drive the disc 6 and the cover plate 7 to rise in the kettle body 1, the space in the mixing zone increases, and the space in the reaction zone decreases. Since the pressure in the reaction zone is relatively high after the reaction, the reaction liquid in the reaction zone can be discharged into the mixing zone through the channel with a certain impact force for mixing, thereby ensuring the adequacy of the reaction. At the same time, the flow disturbance mechanism is triggered to form turbulence in the mixing zone.

[0044] Specifically, turbulence has strong turbulence and irregularity, which can make the acid and base reactants more fully and evenly mixed in the mixing zone, greatly increase the contact area and collision opportunities between the reactants, and thus significantly increase the reaction rate;

[0045] In the turbulent state, the flow of the fluid is more complex and random, which reduces the diffusion distance and time between reactants, reduces the diffusion limitation, enables the reaction to proceed faster, and effectively avoids the local acid-base excess caused by insufficient stirring or uneven fluid flow.

[0046] The present application provides an innovative kettle body design, which cleverly divides the interior of the kettle body 1 into a reaction zone and a mixing zone distributed upper and lower by arranging a disk body 6 and a cover plate 7 that can move relative to each other inside the kettle body 1. This design shows significant advantages in processing residual liquid: when the residual liquid is added to the kettle body 1 and does not exceed the cover plate 7, as the reaction proceeds, the pressure in the reaction zone gradually increases. At this time, the cover plate 7 slides on the disk body 6 to achieve automatic expansion of the reaction zone. This process not only effectively avoids damage to the kettle body 1 caused by excessive pressure in the reaction zone, ensuring the safety and stability of the equipment, but also makes full use of the high-pressure environment, so that the reaction liquid in the reaction zone has a certain atomization impact effect when discharged into the mixing zone. This atomization impact is conducive to the full integration of the reaction liquid and the turbulence in the mixing zone, further improving the sufficiency and efficiency of the reaction, ensuring the uniform progress of the reaction, and improving the quality and yield of the product.

[0047] Please refer again Figure 8 and Figure 9 The disk body 6 and the cover plate 7 are connected by multiple groups of elastic support structures. A plurality of first through holes 601 are provided at the eccentric portion of the disk body 6, and a plurality of second through holes 701 are provided at the eccentric portion of the cover plate 7. A bellows 8 is connected between each of the plurality of first through holes 601 and the plurality of second through holes 701 to form the channel.

[0048] Furthermore, the provision of the bellows 8 can effectively form a channel between the disc 6 and the cover plate 7 without affecting the relative movement between the cover plate 7 and the disc 6. As a highly flexible and retractable pipe, the bellows 8 has a unique corrugated structure that gives it the ability to flexibly expand and contract and bend when subjected to force. In this design, the bellows 8 is cleverly installed between the disc 6 and the cover plate 7. When the cover plate 7 slides or displaces relative to the disc 6, the bellows 8 can expand and contract and deform accordingly, thereby always keeping the channel between the disc 6 and the cover plate 7 unobstructed. This design not only makes full use of the elastic deformation capacity of the bellows 8, ensuring that during the reaction process, as the reaction zone expands or contracts, the relative movement between the cover plate 7 and the disc 6 can proceed smoothly, but also effectively utilizes the sealing performance of the bellows 8, preventing the reaction liquid from leaking in the channel and ensuring the stability of the reaction system.

[0049] A first inlet 26 and a second inlet 27 are provided on the upper portion of the kettle body 1 . The first inlet 26 and the second inlet 27 are used to add residual liquid and neutralizing liquid into the kettle body 1 , respectively.

[0050] When the reaction liquid is added into the kettle body 1 through the first inlet 26 and the second inlet 27, the liquid falls onto the cover plate 7 and then flows into the mixing zone through the second through hole 701, the bellows 8 and the first through hole 601;

[0051] The first inlet 26 and the second inlet 27 are arranged at the upper part of the kettle body 1. The purpose is that the residual liquid added to the kettle and the neutralizing liquid can undergo a neutralization reaction in the reaction zone, thereby effectively causing the disc body 6 and the cover plate 7 to move relative to each other, so that after the disc body 6 and the cover plate 7 rise, the high-pressure environment generated by the reaction can be utilized to make the reaction liquid in the reaction zone have a certain atomization impact effect when it is discharged into the mixing zone. This atomization impact is conducive to the full fusion of the reaction liquid and the turbulence in the mixing zone, further improving the adequacy of the reaction.

[0052] Please refer again Figure 8 and Figure 9The elastic support structure includes a connecting column 9 fixed to the bottom of the cover plate 7 and sealed and slidably connected to the disk body 6. The end of the connecting column 9 away from the cover plate 7 is connected to the atomization mechanism. The outer periphery of the connecting column 9 is also sleeved with a cylindrical spring 10. The cylindrical spring 10 is located in the variable chamber, and its two ends are respectively connected to the bottom wall of the disk body 6 and the cover plate 7.

[0053] As the neutralization reaction proceeds in the reaction zone, since the neutralization reaction is an exothermic reaction, the temperature of the system will increase during the reaction process. During the neutralization reaction, a large amount of heat will be released, which may cause the pressure in the reaction zone to increase. Accordingly, the cover plate 7 will gradually move downward relative to the disk body 6 under the action of pressure, the connecting column 9 will slide downward, the cylindrical spring 10 will gradually be compressed, and the space of the reaction zone will increase. In this way, the effect of automatic expansion according to the degree of reaction is achieved, which can effectively avoid the local pressure inside the kettle body 1 being too high during the treatment process and causing damage to the kettle body 1, thereby realizing the self-protection function of the kettle body 1.

[0054] Please refer again Figure 7 and Figure 9 The atomizing mechanism includes a plurality of atomizing nozzles 17 that are sealed and slidably arranged at the bottom of the disc body 6 and adapted to the first through hole 601. The plurality of atomizing nozzles 17 are respectively connected to the plurality of connecting columns 9 through a set of transmission structures. When the variable chamber shrinks, the connecting column 9 can drive the atomizing nozzle 17 to move radially along the disc body 6 through the transmission structure until the atomizing nozzle 17 coincides with the first through hole 601.

[0055] It should be noted that a plurality of limiting protrusions 602 are formed on the upper edge of the disk body 6. The limiting protrusions 602 are used to limit the cover plate 7 to prevent the cover plate 7 from being separated from the disk body 6, thereby ensuring the effective maintenance of the variable chamber and preventing the reactants from entering the variable chamber.

[0056] The transmission structure includes two guide rails 14 fixed to the bottom of the disk body 6 and a movable seat 15 slidably engaged between the two guide rails 14. The atomizing nozzle 17 is installed on the movable seat 15. A guide column 13 is also fixed to the bottom of the disk body 6. A follower ring 12 is slidably sleeved on the guide column 13. The follower ring 12 is fixed to the connecting column 9 through a connecting arm 11, and a connecting rod 16 is provided between the follower ring 12 and the movable seat 15. The head end of the connecting rod 16 is hinged to the follower ring 12, and the tail end is hinged to the movable seat 15.

[0057] As the reaction proceeds, the cover plate 7 moves toward the bottom wall of the disc 6 due to the high-pressure environment in the reaction zone. The connecting post 9 drives the follower ring 12 to slide away from the disc 6 on the guide post 13 through the connecting arm 11. Correspondingly, the follower ring 12 pulls the movable seat 15 to slide along the guide rail 14 through the connecting rod 16. The movable seat 15 drives the atomizing nozzle 17 to move radially along the disc 6 toward the first through hole 601. Finally, the atomizing nozzle 17 coincides with the first through hole 601.

[0058] Therefore, when the lifting mechanism drives the disc 6 and the cover plate 7 to rise, the reaction liquid in the reaction zone can be discharged into the mixing zone through the channel and the atomizing nozzle 17 by virtue of the high pressure state in the reaction zone. The reaction liquid in the reaction zone has a certain atomization impact effect when it is discharged into the mixing zone.

[0059] The present application sets an atomizing nozzle 17 at the bottom of the disk 6 to discharge the reaction liquid in the reaction zone into the mixing zone in the form of atomization. The atomized reaction liquid forms tiny droplets, which greatly increases the contact area between the reaction liquid and the residual liquid in the mixing zone, thereby effectively ensuring that the neutralization liquid that has not fully reacted in the reaction zone is fused with the residual liquid in the mixing zone, thereby improving the sufficiency of the reaction. At the same time, atomization helps to evenly distribute the reaction liquid in the mixing zone, promotes sufficient mixing between the reactants, and avoids local excess or uneven reaction. In addition, the atomized reaction liquid can further enhance the heat and mass transfer efficiency in the collision with the residual liquid in the mixing zone, which is beneficial to the rapid transfer of heat and the uniform progress of the reaction, thereby shortening the reaction time and improving the purity and yield of the product.

[0060] As can be seen from the above, the purpose of setting the atomizing nozzle 17 in the present application is to enable the reaction liquid to be discharged into the mixing zone in the form of atomized impact, thereby improving the sufficiency of mixing. Before the reaction starts, the atomizing nozzle 17 and the first through hole 601 are in a staggered state. When the reaction starts, under the action of high pressure, the cover plate 7 and the disc 6 slide relative to each other, and the atomizing nozzle 17 will coincide with the first through hole 601. The atomizing nozzle 17 in the present application is movably arranged, rather than being directly fixed at the first through hole 601, for the following purposes:

[0061] If the atomizing nozzle 17 is directly fixed to the first through hole 601, when the residual liquid is added to the kettle through the first inlet 26, the surface tension of the residual liquid will cause the residual liquid to form spheres or drops in the small holes of the atomizing nozzle 17, making it difficult to pass through smoothly. Specifically, when the residual liquid enters the small holes of the atomizing nozzle 17, due to the effect of surface tension, a mutual attraction will be generated between the liquid molecules, causing the liquid to gather into spheres or drops in the small holes instead of forming a continuous liquid flow. This phenomenon will hinder the smooth flow of the residual liquid, resulting in the residual liquid being unable to be smoothly ejected from the atomizing nozzle 17 and enter the mixing zone. Furthermore, since the residual liquid cannot pass through the atomizing nozzle 17 smoothly, it may form a blockage inside the nozzle, or even be completely unable to flow to the mixing zone. In this case, the efficiency of adding the residual liquid will be affected.

[0062] Please refer again Figure 4 and Figure 5 A mixing mechanism is also provided in the kettle body 1, and the mixing mechanism includes a driving motor 2 installed on the top of the kettle body 1 and a central vertical shaft 3 connected to the output end of the driving motor 2 and extending into the mixing zone, and the central vertical shaft 3 is fixedly connected to a plurality of stirring blades 4 located in the mixing zone, and the central vertical shaft 3 sequentially passes through the cover plate 7 and the disk body 6, and is sealed and slidably connected to the cover plate 7 and the disk body 6.

[0063] Specifically, the central vertical shaft 3 passes through the cover plate 7 and the disk body 6 in sequence. To this end, the center of each of the cover plate 7 and the disk body 6 is provided with a hole (not numbered in the figure) for the central vertical shaft 3 to pass through.

[0064] During the treatment of the residual liquid, the drive motor 2 works and drives the multiple stirring blades 4 to rotate in the mixing zone through the central vertical shaft 3. The stirring blades 4 stir the reaction liquid in the kettle, so that the residual liquid in the mixing zone forms a vortex. When the disturbing mechanism is triggered, the vortex will be broken, so that turbulence can be formed in the kettle. Therefore, the reaction liquid discharged into the mixing zone through the atomizing nozzle 17 can be fully merged with the residual liquid to ensure the adequacy of the reaction.

[0065] Please refer again Figure 5 and Figure 6 The spoiler mechanism includes a protruding block 18 fixed on the inner wall of the kettle body 1, a rotating shaft 19 rotatably mounted on the protruding block 18, and a spoiler 5 fixed to the rotating shaft 19 in an arc shape. The bottom of the disc body 6 is fixedly connected to a ring body 21 through a fixing frame 20, and the ring body 21 is slidably fitted with the rotating shaft 19;

[0066] Among them, a boss 22 perpendicular to the rotating shaft 19 is fixed on the ring body 21, and the boss 22 extends into a groove body provided on the outer wall of the rotating shaft 19 and is slidingly connected to the rotating shaft 19. The groove body includes a first groove 1901 and a second groove 1902 connected to each other. The first groove 1901 is arranged in a spiral shape, and the second groove 1902 is arranged along the axial direction of the rotating shaft 19.

[0067] During the reaction process, the spoiler 5 is concentric with the kettle body 1. At this time, under the stirring action of the multiple stirring blades 4, the reaction liquid in the mixing zone can effectively form a vortex. When the lifting mechanism drives the disc body 6 to rise, the fixing frame 20 and the ring body 21 rise together with the disc body 6. Correspondingly, the boss 22 rises along the axial direction of the rotating shaft 19. During the previous process, the boss 22 slides with the rotating shaft 19 through the first groove 1901, causing the rotating shaft 19 to rotate. As a result, the spoiler 5 deflects toward the center direction of the kettle body 1, and the spoiler 5 intervenes in the vortex. After the boss 22 enters the second groove 1902, the spoiler 5 maintains the intervention angle, so that a vortex is formed in the mixing zone, thereby improving the sufficient mixing of the reactants and ensuring the sufficiency and efficiency of the reaction.

[0068] Please refer again Figure 1 、 Figure 2 as well as Figure 4 The lifting mechanism includes a cylinder 23 installed on the top of the kettle body 1 and a riser 25 slidably arranged on the kettle body 1 and fixedly connected to the movable end of the cylinder 23 through an arc arm 24. The riser 25 is fixed to the disc body 6 and is also sealed and slidably connected to the cover plate 7.

[0069] It should be emphasized that in order to ensure that the cover plate 7 can slide smoothly toward the bottom wall of the disk body 6 under the action of the increased pressure in the reaction zone, thereby achieving the purpose of expanding the reaction zone, a first air hole 2501 and a second air hole 2502 are respectively provided at the upper end and the lower end of the standpipe 25. When the cover plate 7 slides toward the bottom wall of the disk body 6, the air in the variable chamber will be discharged to the outside through the second air hole 2502, the standpipe 25 and the first air hole 2501. It should be noted that when the compression of the cylindrical spring 10 reaches the maximum, the height of the cover plate 7 is not lower than the second air hole 2502 to prevent the reaction liquid from entering the standpipe 25 through the second air hole 2502.

[0070] During operation, the movable end of the cylinder 23 extends, and the vertical pipe 25 is driven to rise through the arc-shaped arm 24, so that the vertical pipe 25 can drive the plate 6 to rise;

[0071] It should be noted that in order to effectively utilize the high pressure state in the reaction zone and discharge the reaction liquid in the reaction zone into the mixing zone in the form of atomized impact to achieve the purpose of sufficient mixing, the extension speed of the movable end of the cylinder 23 must be fast enough, that is, the cylinder 23 can drive the disc 6 to rise at a faster speed.

[0072] It should be added that, since the interior of the kettle body 1 is the place where the acidic residual liquid and the alkaline neutralizing liquid undergo neutralization reaction, the material selection of the components located inside the kettle body 1 is crucial. First of all, the material needs to have good corrosion resistance to cope with the alternating effects of acidic and alkaline environments. 316L stainless steel is an ideal material. It contains high levels of chromium, nickel and molybdenum, and can form a dense oxide film that effectively resists acid and alkali erosion. In addition, 316L stainless steel also has good high-temperature stability, can maintain structural stability during the reaction process, and is not prone to deformation or damage. In terms of safety, 316L stainless steel is non-toxic and chemically stable, and will not react adversely with reactants or products, ensuring the safety of the reaction process and the purity of the product.

[0073] Secondly, a solenoid valve 28 is provided on the top of the kettle body 1. As the reaction proceeds, the overall pressure inside the kettle body 1 will gradually increase. In order to avoid excessive pressure, the solenoid valve 28 can be opened to release the pressure to ensure the safety of equipment and personnel.

[0074] As another embodiment of the present invention, a use of the residual liquid neutralization kettle in the preparation of 2,4-dichloro-5-fluorobenzoyl chloride is also proposed.

[0075] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims, not the foregoing description, and all variations within the meaning and range of equivalents of the claims are intended to be included therein. Any reference sign in a claim should not be construed as limiting the claim to which it relates.

[0076] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A residual liquid neutralization kettle, comprising a kettle body and a variable volume structure provided in the kettle body; It is characterized by: The variable volume structure divides the inner portion of the kettle into a reaction zone and a mixing zone distributed vertically. The structure includes a deep-filled disc that is sealingly slidably disposed within the kettle, and a cover plate that is sealingly slidably disposed within the disc. A variable chamber is formed between the disc and the bottom wall of the cover plate. A channel is formed between the disc and the cover plate so that the residual liquid added to the kettle can cover the cover plate, and the added neutralizing liquid can react with the residual liquid in the reaction zone, thereby promoting relative movement between the cover plate and the disc, reducing the variable chamber, and cooperating with the atomizing mechanism provided at the bottom of the disc; The disc can be driven to rise by multiple lifting mechanisms provided on the kettle body, so that the reaction liquid in the reaction zone is discharged into the mixing zone in the form of atomization through the channel and the atomization mechanism. At the same time, the flow disturbance mechanism provided in the kettle body is triggered to form turbulent flow in the mixing zone. The disc body and the cover plate are connected via multiple sets of elastic support structures. A plurality of first through holes are provided at an eccentric portion of the disc body, and a plurality of second through holes are provided at an eccentric portion of the cover plate. A bellows is connected between each of the plurality of first through holes and the plurality of second through holes to form the channel. The elastic support structure includes a connecting column fixed to the bottom of the cover plate and sealingly and slidingly connected to the disk body. The end of the connecting column away from the cover plate is connected to the atomization mechanism. The outer periphery of the connecting column is further provided with a cylindrical spring. The cylindrical spring is located in the variable chamber, and its two ends are respectively connected to the bottom wall of the disk body and the cover plate; The atomizing mechanism includes a plurality of atomizing nozzles that are sealingly and slidingly arranged at the bottom of the disk body and adapted to the first through-holes. The plurality of atomizing nozzles are respectively connected to a plurality of connecting columns through a set of transmission structures. When the variable chamber shrinks, the connecting columns can drive the atomizing nozzles to move radially along the disk body through the transmission structure until the atomizing nozzles coincide with the first through-holes.

2. A residual liquid neutralization kettle according to claim 1, characterized in that, The upper portion of the kettle body is provided with a first inlet and a second inlet, and the first inlet and the second inlet are used for adding residual liquid and neutralizing liquid into the kettle body respectively.

3. A residual liquid neutralization kettle according to claim 1, characterized in that, The transmission structure includes two guide rails fixed to the bottom of the disk body and a movable seat slidably engaged between the two guide rails. The atomizing nozzle is installed on the movable seat. A guide column is also fixed to the bottom of the disk body. A follower ring is slidably sleeved on the guide column. The follower ring is fixed to the connecting column through a connecting arm, and a connecting rod is provided between the follower ring and the movable seat. The head end of the connecting rod is hinged to the follower ring, and the tail end is hinged to the movable seat.

4. A residual liquid neutralization kettle according to claim 1, characterized in that, A mixing mechanism is also provided in the kettle body, and the mixing mechanism includes a driving motor installed on the top of the kettle body and a central vertical shaft connected to the output end of the driving motor and extending into the mixing zone, and the central vertical shaft is fixedly connected to a plurality of stirring blades located in the mixing zone, and the central vertical shaft sequentially passes through the cover plate and the disk body, and is sealed and slidably connected to the cover plate and the disk body.

5. A residual liquid neutralization kettle according to claim 1, characterized in that, The spoiler mechanism includes a protrusion fixed on the upper wall of the kettle body, a rotating shaft rotatably mounted on the protrusion, and an arc-shaped spoiler fixed on the rotating shaft. The bottom of the plate body is fixedly connected to a ring body through a fixing frame, and the ring body is slidably fitted with the rotating shaft. Among them, a convex column perpendicular to the rotating shaft is fixed on the ring body, and the convex column extends into a groove body provided on the outer wall of the rotating shaft and is slidingly connected to the rotating shaft. The groove body includes a first groove and a second groove connected to each other, the first groove is arranged in a spiral shape, and the second groove is arranged along the axial direction of the rotating shaft.

6. A residual liquid neutralization kettle according to claim 1, characterized in that, The lifting mechanism includes a cylinder installed on the top of the kettle body and a riser slidably arranged on the kettle body and fixedly connected to the movable end of the cylinder through an arc-shaped arm. The riser is fixed to the disc body and is also sealed and slidably connected to the cover plate.

7. Use of the residual liquid neutralization kettle according to any one of claims 1 to 6 in the preparation of 2,4-dichloro-5-fluorobenzoyl chloride.

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