Residual liquid neutralization kettle and application thereof in preparation of 2, 4-dichloro-5-fluorobenzoyl chloride

Abstract

The invention relates to the related technical field of raffinate treatment, in particular to a raffinate neutralization kettle and application thereof in preparation of 2, 4-dichloro-5-fluorobenzoyl chloride, the raffinate neutralization kettle comprises a kettle body and a variable volume structure arranged in the kettle body; the volume-variable structure divides the interior of the kettle body into a reaction area and a mixing area which are distributed up and down, and comprises a disc body which is arranged in the kettle body in a sealing and sliding manner and has a containing depth and a cover plate which is arranged in the disc body in a sealing and sliding manner; the disc body and the cover plate which can move relatively are arranged in the kettle body, and the kettle body is divided into the reaction area and the mixing area which are distributed up and down, so that the design has the remarkable advantages during residual liquid treatment: after residual liquid is added into the kettle body and submerges the cover plate, along with the reaction, the pressure intensity of the reaction area is gradually increased, and the cover plate slides on the disc body, so that the automatic expansion of the reaction area is realized; therefore, the damage to the kettle body caused by overlarge pressure in the reaction area is effectively avoided, and the safety and the stability of equipment are ensured.

Description

Technical Field

[0001] The 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] As the chemical industry is booming, the field of fine chemicals is changing with each passing day. The production of 2,4-dichloro-5-fluorobenzoyl chloride is undoubtedly a very representative case. As the global demand for fluorine-containing fine chemicals continues to rise, this type of compound has shined in many fields such as medicine, pesticides and materials. However, its production process is not smooth sailing, especially the treatment of distillation residues, which has always been a problem that has plagued enterprises.

[0003] Therefore, 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. In this regard, 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 specific 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 violent, 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 period of time for the pressure relief process to be released, and it is difficult to provide comprehensive protection for the kettle body in time. 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: A residual liquid neutralization kettle, comprising a kettle body and a variable volume structure arranged in the kettle body; The variable volume structure divides the inner part of the kettle into a reaction zone and a mixing zone distributed up and down, and comprises a disc body with a volume depth and a cover plate sealed and slidably arranged in the kettle body, and a variable chamber is formed between the disc body and the bottom wall of the cover plate; A channel is formed between the disk 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 to cause the cover plate and the disk to move relative to each other, the variable chamber is reduced, and the channel cooperates with the atomization mechanism provided at the bottom of the disk; The disk body can be driven to rise by multiple groups of lifting mechanisms arranged on the kettle body, so that the reaction liquid in the reaction area is discharged into the mixing area in an atomized form through the channel and the atomizing mechanism. At the same time, the turbulence mechanism arranged in the kettle body is triggered to form a turbulent flow in the mixing area.

[0006] 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 position of the disk body, and a plurality of second through holes are provided at the eccentric position of the cover plate. A bellows is connected between each of the plurality of first through holes and each of the plurality of second through holes to form the channel.

[0007] As a further solution of the present invention: a first inlet and a second inlet are provided at the upper part of the kettle body, and the first inlet and the second inlet are respectively used to add residual liquid and neutralizing liquid into the kettle body.

[0008] 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 hermetically and slidably connected to the disk body. The end of the connecting column away from the cover plate is connected to the atomizing mechanism. A cylindrical spring is also sleeved on the outer periphery of the connecting column. The cylindrical spring is located in the variable chamber and is respectively connected to the bottom wall of the disk body and the cover plate at both ends.

[0009] As a further solution of the present invention: the atomizing mechanism includes a plurality of atomizing nozzles hermetically and slidably arranged at the bottom of the disk body and adapted to the first through holes. Each of the plurality of atomizing nozzles is respectively connected to a plurality of the connecting columns through a set of transmission structures. When the variable chamber shrinks, the connecting column can drive the atomizing nozzle to move along the radial direction of the disk body through the transmission structure until the atomizing nozzle coincides with the first through hole.

[0010] 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 fitted between the two guide rails. The atomizing nozzle is installed on the movable seat. A guide post is also fixed to the bottom of the disk body. A follower ring is slidably sleeved on the guide post. The follower ring is fixed to the connecting column through a connecting arm. 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.

[0011] As a further solution of the present invention: A mixing mechanism is further provided in the kettle body. The mixing mechanism includes a driving motor installed at 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 area. The central vertical shaft is fixedly connected with a plurality of stirring blades located in the mixing area. The central vertical shaft sequentially penetrates through the cover plate and the disc body, and is in sealed sliding connection with the cover plate and the disc body.

[0012] As a further solution of the present invention: The flow disturbing mechanism includes a protruding block fixed on the inner wall of the kettle body, a rotating shaft rotatably installed on the protruding block, and a flow disturbing plate fixed on the rotating shaft and arranged in an arc shape. The bottom of the disc body is fixedly connected with an annular body through a fixing frame, and the annular body is slidably sleeved with the rotating shaft; Wherein, a convex column perpendicular to the rotating shaft is fixed on the annular body. The convex column extends into a groove on the outer wall of the rotating shaft and is slidably connected with the rotating shaft. The groove includes a connected first groove and a second groove. The first groove is arranged in a spiral shape, and the second groove is arranged along the axial direction of the rotating shaft.

[0013] As a further solution of the present invention: The lifting mechanism includes a cylinder installed at the top of the kettle body and a vertical pipe slidably arranged on the kettle body and fixedly connected to the movable end of the cylinder through an arc-shaped arm. The vertical pipe is fixed to the disc body and is also in sealed sliding connection with the cover plate.

[0014] An application of the residual liquid neutralization kettle in the preparation of 2,4-dichloro-5-fluorobenzoyl chloride.

[0015] Compared with the prior art, the beneficial effects of the present invention are: In this application, by arranging a relatively movable disc body and a cover plate in the kettle body, the kettle body is divided into a reaction area and a mixing area distributed up and down. When the residual liquid is added to the kettle body and covers the cover plate, as the reaction progresses, the pressure in the reaction area gradually increases, and the cover plate slides on the disc body to realize the automatic expansion of the reaction area, effectively avoiding the damage to the kettle body caused by excessive pressure in the reaction area; The capacity of the variable chamber formed between the disc body and the cover plate gradually decreases according to the reaction process, enabling the expansion of the reaction area. In the case where the neutralization reaction is relatively intense and the pressure change is instantaneous, the comprehensive protection of the kettle body is realized, ensuring the safety and stability of the equipment; At the same time, by utilizing the high-pressure environment, the reaction liquid in the reaction area generates atomization impact when discharging into the mixing area, which is beneficial to the full fusion of the reaction liquid and the turbulence in the mixing area, 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. Description of the Drawings

[0016] Figure 1It is a schematic structural diagram of an embodiment of a residual liquid neutralization kettle.

[0017] Figure 2 It is a schematic structural diagram of another angle of an embodiment of a residual liquid neutralization kettle.

[0018] Figure 3 It is a schematic structural diagram of yet another angle of an embodiment of a residual liquid neutralization kettle.

[0019] Figure 4 It is a schematic internal structure diagram of the kettle body in an embodiment of a residual liquid neutralization kettle.

[0020] Figure 5 It is an exploded view of the internal structure of the kettle body in an embodiment of a residual liquid neutralization kettle.

[0021] Figure 6 It is a schematic structural diagram of the flow guiding mechanism in an embodiment of a residual liquid neutralization kettle.

[0022] Figure 7 It is a schematic structural diagram of the variable volume structure in an embodiment of a residual liquid neutralization kettle.

[0023] Figure 8 It is an exploded view of the variable volume structure in an embodiment of a residual liquid neutralization kettle.

[0024] Figure 9 It is Figure 8 A schematic structural diagram of another angle.

[0025] In the figure: 1. Kettle body; 2. Driving motor; 3. Central vertical shaft; 4. Stirring blade; 5. Turbulence plate; 6. Disk body; 601. First through hole; 602. Limit projection; 7. Cover plate; 701. Second through hole; 8. Bellows; 9. Connecting column; 10. Columnar spring; 11. Connecting arm; 12. Follow-up ring; 13. Guide post; 14. Guide rail; 15. Movable seat; 16. Connecting rod; 17. Atomizing nozzle; 18. Protruding block; 19. Rotating shaft; 1901. First groove; 1902. Second groove; 20. Fixed frame; 21. Ring body; 22. Convex column; 23. Cylinder; 24. Arc-shaped arm; 25. Vertical pipe; 2501. First air hole; 2502. Second air hole; 26. First inlet; 27. Second inlet; 28. Solenoid valve. Detailed implementation manners

[0026] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts belong to the scope of protection of the present invention.

[0027] In addition, the components in the present invention are referred to as "fixed to" or "disposed on" another component, and it can be directly on another component or there can also be an intermediate component. When a component is considered to be "connected to" another component, it can be directly connected to another component or there may be an intermediate component at the same time. The terms "vertical", "horizontal", "left", "right" and similar expressions used herein are only for illustrative purposes and do not represent the only implementation.

[0028] Please refer to Figures 1-9 , in an embodiment of the present invention, a residual liquid neutralization kettle includes a kettle body 1 and a variable volume structure disposed in the kettle body 1; The variable volume structure divides the inside of the kettle body 1 into a reaction zone and a mixing zone which are distributed up and down. It includes a disk body 6 that is hermetically and slidably disposed in the kettle body 1 and has a depth, and a cover plate 7 that is hermetically and slidably disposed in the disk body 6. A variable chamber is formed between the bottom wall of the disk body 6 and the cover plate 7; Wherein, a channel is formed between the disk body 6 and the cover plate 7 so that the residual liquid added into the kettle body 1 can submerge the cover plate 7, and the added neutralizing liquid can carry out a neutralization reaction with the residual liquid in the reaction zone, prompting relative movement between the cover plate 7 and the disk body 6, and the variable chamber decreases. The channel cooperates with an atomization mechanism disposed at the bottom of the disk body 6; The disk body 6 can be driven to rise by multiple sets of lifting mechanisms disposed 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, a turbulence mechanism disposed in the kettle body 1 is triggered to form a turbulent flow in the mixing zone.

[0029] It should be added that the above-mentioned neutralizing liquid is an alkaline liquid, such as sodium hydroxide solution, etc. For its specific type, the present application does not make a specific limitation and can be selected according to actual needs; When using this neutralization kettle to treat residual liquid, the residual liquid is added into the kettle body 1 until the residual liquid submerges the cover plate 7. Subsequently, the neutralizing liquid is added into the kettle body 1. Then, the neutralizing liquid will carry out a neutralization reaction with the residual liquid in the reaction zone of the kettle body 1; The neutralization reaction is an exothermic reaction, and the temperature of the system will rise during the reaction process. A large amount of heat will be released during the neutralization reaction, which may cause the pressure in the reaction zone to rise. Furthermore, the cover plate 7 will have relative movement with the disk body 6. Specifically, the cover plate 7 moves towards 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 automatically expanding the volume according to the reaction degree is achieved, and it can effectively avoid damage to the kettle body 1 caused by excessive local pressure inside the kettle body 1 during the treatment process; After the reaction in the reaction zone ends (at this time, there may be an insufficient reaction between the residual liquid and the neutralizing liquid in the reaction zone), the lifting mechanism operates to drive the disk body 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 then be discharged into the mixing zone through the channel with a certain impact force for mixing, ensuring the sufficiency of the reaction. At the same time, the turbulence generating mechanism is triggered, which can cause a turbulent flow to form in the mixing zone; Specifically, turbulent flow has strong turbulence and irregularity, which can make the acid-base reactants be more fully and evenly mixed in the mixing zone. The contact area and collision chance between the reactants are greatly increased, thus significantly improving the reaction rate; In the state of turbulent flow, the fluid flow is more complex and random, reducing the diffusion distance and time between the reactants, reducing the diffusion limitation, enabling the reaction to proceed faster, and effectively avoiding the phenomenon of local acid-base excess caused by insufficient stirring or uneven fluid flow.

[0030] This application provides an innovative design of the kettle body. By arranging a relatively movable disk body 6 and a cover plate 7 inside the kettle body 1, the interior of the kettle body 1 is ingeniously divided into an upper and lower distributed reaction zone and a mixing zone. This design shows significant advantages when dealing with the residual liquid: when the residual liquid is added to the kettle body 1 and covers the cover plate 7, as the reaction progresses, the pressure in the reaction zone gradually increases. At this time, the cover plate 7 slides on the disk body 6 to realize the automatic expansion of the reaction zone. This process not only effectively avoids the 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, enabling the reaction liquid in the reaction zone to have a certain atomization impact effect when being discharged into the mixing zone. This atomization impact is conducive to the full fusion of the reaction liquid and the turbulent flow in the mixing zone, further enhancing the sufficiency and efficiency of the reaction, ensuring the uniform progress of the reaction, and improving the quality and yield of the product.

[0031] Please refer to again Figure 8 And Figure 9 , the disk body 6 and the cover plate 7 are connected by multiple groups of elastic support structures. Multiple first through holes 601 are provided at the eccentric position of the disk body 6, and multiple second through holes 701 are provided at the eccentric position of the cover plate 7. Bellows 8 are connected between the multiple first through holes 601 and the multiple second through holes 701 in pairs to form the channel.

[0032] Furthermore, the arrangement of the bellows 8 can effectively form a channel between the disc body 6 and the cover plate 7 without affecting the relative movement between the cover plate 7 and the disc body 6. The bellows 8 is a highly flexible and retractable pipe, and its unique corrugated structure gives it the characteristics of flexible expansion and contraction when subjected to force. In this design, the bellows 8 is cleverly installed between the disc body 6 and the cover plate 7. When the cover plate 7 slides or displaces relative to the disc body 6, the bellows 8 can expand and deform accordingly, thereby always keeping the channel between the disc body 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 body 6 can proceed smoothly, but also the sealing performance of the bellows 8 is effectively exerted, preventing the leakage of the reaction liquid in the channel and ensuring the stability of the reaction system.

[0033] The upper portion of the kettle body 1 is provided with a first inlet 26 and a second inlet 27 , and the first inlet 26 and the second inlet 27 are used to add residual liquid and neutralizing liquid into the kettle body 1 , respectively.

[0034] 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; 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 and the neutralizing liquid added to the kettle can undergo a neutralization reaction in the reaction zone, so that the disk body 6 and the cover plate 7 can effectively move relative to each other, so that after the disk 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.

[0035] Please refer again Figure 8 and Figure 9 The 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 the two ends are respectively connected to the bottom wall of the disk body 6 and the cover plate 7.

[0036] 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. A large amount of heat will be released during the neutralization reaction, which may cause the pressure in the reaction zone to increase. Correspondingly, 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, and the columnar spring 10 will be gradually compressed. The space of the reaction zone increases. In this way, the effect of automatic expansion according to the reaction degree is achieved, which can effectively prevent local pressure in the kettle body 1 from being too high during the treatment process and damaging the kettle body 1, and realizing the self-protection function of the kettle body 1.

[0037] Please refer to again Figure 7 And Figure 9 , the atomization mechanism includes a plurality of atomizing nozzles 17 that are hermetically and slidably arranged at the bottom of the disk body 6 and adapted to the first through hole 601. Each of the plurality of atomizing nozzles 17 is connected to a plurality of the connecting columns 9 through a set of transmission structures respectively. When the variable chamber shrinks, the connecting column 9 can drive the atomizing nozzle 17 to move radially along the disk body 6 through the transmission structure until the atomizing nozzle 17 coincides with the first through hole 601.

[0038] It should be added that a plurality of limiting protrusions 602 are further 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 separating from the disk body 6, ensure the effective maintenance of the variable chamber, and prevent reactants from entering the variable chamber.

[0039] The transmission structure includes two guide rails 14 fixed to the bottom of the disk body 6 and a movable seat 15 slidably fitted between the two guide rails 14. The atomizing nozzle 17 is installed on the movable seat 15. A guide post 13 is also fixed to the bottom of the disk body 6. A follower ring 12 is slidably sleeved on the guide post 13. The follower ring 12 is fixed to the connecting column 9 through a connecting arm 11. 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.

[0040] As the reaction proceeds, when the cover plate 7 moves toward the bottom wall of the disk body 6 due to the high-pressure environment in the reaction zone, the connecting column 9 will drive the follower ring 12 to slide away from the disk body 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, and the movable seat 15 drives the atomizing nozzle 17 to move radially close to the first through hole 601 along the disk body 6. Finally, the atomizing nozzle 17 coincides with the first through hole 601; Thus, when the lifting mechanism drives the disc body 6 and the cover plate 7 to rise, by virtue of the high-pressure state in the reaction zone, the reaction liquid in the reaction zone can be discharged into the mixing zone through the channel and the atomizing nozzle 17, and the reaction liquid in the reaction zone has a certain atomizing impact effect when being discharged into the mixing zone; In this application, by arranging the atomizing nozzle 17 at the bottom of the disc body 6, the reaction liquid in the reaction zone is discharged into the mixing zone in an atomized form. The atomized reaction liquid forms tiny droplets, greatly increasing the contact area between the reaction liquid and the residual liquid in the mixing zone, thereby effectively ensuring the fusion of the neutralizing liquid that has not been fully reacted in the reaction zone and the residual liquid in the mixing zone, improving the sufficiency of the reaction. At the same time, atomization helps the reaction liquid to be evenly distributed in the mixing zone, promotes the full mixing between reactants, and avoids the situation of local excess or uneven reaction. In addition, during the collision of the atomized reaction liquid with the residual liquid in the mixing zone, the heat transfer and mass transfer efficiency can be further enhanced, which is conducive 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.

[0041] As can be seen from the above, the purpose of setting the atomizing nozzle 17 in this application is to enable the reaction liquid to be discharged into the mixing zone in the form of atomizing impact, so as to improve the sufficiency of mixing in turn. When the reaction has not started, 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, when the cover plate 7 and the disc body 6 undergo relative sliding, the atomizing nozzle 17 will coincide with the first through hole 601. The atomizing nozzle 17 in this application is movably arranged instead of being directly fixed at the first through hole 601, and the purpose is as follows: If the atomizing nozzle 17 is directly fixed at the first through hole 601, when adding the residual liquid into the kettle through the first inlet 26, the surface tension of the residual liquid will cause the residual liquid to form a spherical or droplet shape in the small holes of the atomizing nozzle 17 and it is difficult to pass through smoothly. Specifically, when the residual liquid enters the small holes of the atomizing nozzle 17, due to the action of surface tension, an attractive force will be generated between liquid molecules, causing the liquid to aggregate into a spherical or droplet shape 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 inability of the residual liquid to be sprayed out of the atomizing nozzle 17 smoothly and enter the mixing zone. Further, since the residual liquid cannot pass through the atomizing nozzle 17 smoothly, it may form a blockage inside the nozzle and even completely unable to flow to the mixing zone. In this case, the adding efficiency of the residual liquid will be affected.

[0042] Please refer to again Figure 4 And Figure 5, a mixing mechanism is further provided in the kettle body 1. The mixing mechanism includes a driving motor 2 installed at 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 area. A plurality of stirring blades 4 located in the mixing area are fixedly connected to the central vertical shaft 3. The central vertical shaft 3 sequentially penetrates through the cover plate 7 and the disc body 6 and is in sealed sliding connection with the cover plate 7 and the disc body 6.

[0043] Specifically, the central vertical shaft 3 sequentially penetrates through the cover plate 7 and the disc body 6. For this purpose, holes (not labeled in the figure) for the central vertical shaft 3 to pass through are provided at the centers of both the cover plate 7 and the disc body 6. During the process of treating the residual liquid, the driving motor 2 operates, and drives a plurality of the stirring blades 4 to rotate in the mixing area through the central vertical shaft 3. The stirring blades 4 play a role in stirring the reaction liquid in the kettle, and can form a vortex of the residual liquid in the mixing area. When the flow 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 area through the atomizing nozzle 17 can be fully fused with the residual liquid, ensuring the sufficiency of the reaction.

[0044] Please refer to again Figure 5 And Figure 6 , the flow disturbing mechanism includes a protruding block 18 fixed on the inner wall of the kettle body 1, a rotating shaft 19 rotatably installed on the protruding block 18, and a flow disturbing plate 5 fixed on the rotating shaft 19 and arranged in an arc shape. The bottom of the disc body 6 is fixedly connected with a ring body 21 through a fixing frame 20, and the ring body 21 is slidably sleeved with the rotating shaft 19. Wherein, a convex column 22 perpendicular to the rotating shaft 19 is fixed on the ring body 21. The convex column 22 extends into a groove provided on the outer wall of the rotating shaft 19 and is slidably connected with the rotating shaft 19. The groove includes a connected first groove 1901 and a second groove 1902. 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.

[0045] During the reaction process, the spoiler 5 is concentric with the kettle body 1. At this time, under the agitation of the plurality of 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 convex column 22 rises along the axial direction of the rotating shaft 19. In the previous process, the convex column 22 is in sliding fit with the rotating shaft 19 through the first groove 1901, so that the rotating shaft 19 rotates. Then, the spoiler 5 swings towards the center direction of the kettle body 1, and the spoiler 5 intervenes in the vortex. After the convex column 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 sufficiency of the mixing of the reactants and ensuring the sufficiency and efficiency of the reaction.

[0046] Please refer to again Figure 1 、 Figure 2 and Figure 4 , the lifting mechanism includes a cylinder 23 installed at 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-shaped arm 24. The riser 25 is fixed to the disc body 6 and is also in sealed sliding connection with the cover plate 7.

[0047] It should be emphasized that in order to ensure that the cover plate 7 can smoothly slide towards the bottom wall of the disc body 6 under the action of the increased pressure in the reaction zone, so as to achieve 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 riser 25. When the cover plate 7 slides towards the bottom wall of the disc body 6, the air in the variable chamber will be discharged to the outside through the second air hole 2502, the riser 25 and the first air hole 2501. It should be noted that when the compression amount 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 riser 25 through the second air hole 2501.

[0048] During operation, when the movable end of the cylinder 23 extends, the riser 25 can be driven to rise through the arc-shaped arm 24. Then, the riser 25 can drive the disc body 6 to rise; It should be noted that in order to effectively utilize the high-pressure state in the reaction zone and realize the discharge of 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 needs to be fast enough, that is, the cylinder 23 can drive the disc body 6 to rise at a relatively fast speed.

[0049] It should be noted that since the inside of the kettle body 1 is a place where the acidic residual liquid and the alkaline neutralizing liquid carry out a neutralization reaction, therefore, 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 action of acidic and alkaline environments. 316L stainless steel is an ideal material. It contains relatively high chromium, nickel and molybdenum components, which can form a dense oxide film and effectively resist the erosion of acids and alkalis. In addition, 316L stainless steel also has good high-temperature stability, can maintain the stability of the structure during the reaction, and is not prone to deformation or damage. In terms of safety, 316L stainless steel is non-toxic and chemically stable, and will not have adverse reactions with reactants or products, ensuring the safety of the reaction process and the purity of the products.

[0050] Secondly, an electromagnetic valve 28 is also provided at the top of the kettle body 1. As the reaction progresses, the overall pressure inside the kettle body 1 will gradually rise. In order to avoid excessive pressure, the electromagnetic valve 28 can be opened to relieve pressure and ensure the safety of the equipment and personnel.

[0051] As another embodiment of the present invention, an application of the residual liquid neutralization kettle in the preparation of 2,4-dichloro-5-fluorobenzoyl chloride is also proposed.

[0052] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and without departing from the spirit or basic characteristics of the present invention, the present invention can be implemented in other specific forms. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included in the present invention. Any reference signs in the claims should not be regarded as limiting the claims involved.

[0053] In addition, it should be understood that although this specification is described according to embodiments, not every embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments 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 arranged in the kettle body; characterized in that: 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 includes 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, and a variable chamber is formed between the disc body and the bottom wall of the cover plate; wherein a channel is formed between the disc body and the cover plate, so that the residual liquid added to the kettle body can cover the cover plate, and the added neutralizing liquid can react with the residual liquid in the reaction zone, thereby causing the cover plate and the disc body to move relative to each other, the variable chamber is reduced, and the channel cooperates with the atomizing mechanism arranged at the bottom of the disc body; the disc body can be driven up by multiple groups of lifting mechanisms arranged 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 atomizing mechanism, and at the same time, the turbulence mechanism arranged in the kettle body is triggered to form turbulence in the mixing zone.

2. A residual liquid neutralization kettle according to claim 1, characterized in that: The disk body and the cover plate are connected via a plurality of sets of elastic support structures, a plurality of first through holes are provided at an eccentric portion of the disk body, a plurality of second through holes are provided at an eccentric portion of the cover plate, and a corrugated tube is connected between the plurality of first through holes and the plurality of second through holes in pairs to form the channel.

3. 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 to add residual liquid and neutralizing liquid into the kettle body respectively.

4. A residual liquid neutralization kettle according to claim 2, characterized in that: 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. A cylindrical spring is also sleeved on the outer periphery of the connecting column. 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.

5. A residual liquid neutralization kettle according to claim 4, characterized in that: The atomization mechanism includes a plurality of atomization nozzles which are sealingly and slidably arranged at the bottom of the disk body and adapted to the first through hole. The plurality of atomization nozzles are respectively connected to the plurality of connecting columns through a group of transmission structures. When the variable chamber is reduced, the connecting columns can drive the atomization nozzles to move radially along the disk body through the transmission structure until the atomization nozzles coincide with the first through hole.

6. A residual liquid neutralization kettle according to claim 5, 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, and 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.

7. 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 penetrates the cover plate and the disk body, and is sealingly and slidably connected to the cover plate and the disk body.

8. A residual liquid neutralization kettle according to claim 1, characterized in that: The spoiler mechanism includes a protruding block fixed on the inner wall of the kettle body, a rotating shaft rotatably installed on the protruding block, and a spoiler plate fixed on the rotating shaft in an arc shape. The bottom of the disc body is fixedly connected to a ring body through a fixing frame, and the ring body is slidably fitted with the rotating shaft; wherein, a convex column perpendicular to the rotating shaft is fixed on the ring body, the convex column extends into a groove body provided on the outer wall of the rotating shaft and is slidably connected to the rotating shaft, and the groove body includes a first groove and a second groove connected to each other, the first groove is spirally arranged, and the second groove is arranged along the axial direction of the rotating shaft.

9. A residual liquid neutralization kettle according to claim 1, characterized in that: The lifting mechanism comprises 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.

10. Use of the residual liquid neutralization kettle as claimed in any one of claims 1 to 9 in the preparation of 2,4-dichloro-5-fluorobenzoyl chloride.

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