Energy-saving reaction rectification integrated device and method for producing 2-hydrazino-4-methylbenzothiazole

Abstract

The present application belongs to the technical field of reaction kettle, especially to an energy-saving reaction rectification integrated device and method for 2-hydrazyl-4-methylbenzothiazole production, which solves the problems of sampling danger, difficult cleaning of coking in the tower, and low efficiency of rectification separation in the prior art. The device comprises a reaction kettle, a baffle plate fixed in the reaction kettle, a through hole provided in the baffle plate, and a coking scraping mechanism provided in the through hole. The mechanism comprises a cross member fixed in the through hole, a stand column, and a floating ring sleeved on the stand column. The rising steam impacts the turbine paddle to drive the floating ring to rotate and float up and down, thereby removing the coking. A sampling mechanism is provided on one side of the reaction kettle, which comprises a flow guide pipe and a sampling pipe. A piston plate and a closing plate controlled by a tension spring are provided in the sampling pipe. The flow guide pipe can be automatically closed or opened by rotating the sampling pipe, thereby realizing safe sampling. The present application solves the problems of coking shutdown cleaning and unsafe sampling operation, and guarantees the production continuity and personnel safety.

Description

Technical Field

[0001] This invention relates to the field of reaction vessel technology, and in particular to an energy-saving integrated reactive distillation apparatus and method for the production of 2-hydrazino-4-methylbenzothiazole. Background Technology

[0002] 2-Hydroxy-4-methylbenzothiazole is an important organic intermediate used in the synthesis of tricyclic azoles, which are widely used in agriculture as highly effective fungicides. Currently, the main industrial method for producing 2-hydrazino-4-methylbenzothiazole involves a nucleophilic substitution reaction between 4-methyl-2-aminobenzothiazole and hydrazine hydrate under high-temperature conditions. This reaction is carried out in a reactor, and the reaction temperature must be maintained within the range of 120 to 125°C. Ammonia gas is produced as a byproduct during the reaction.

[0003] Existing production technologies have several shortcomings in implementation. Traditional reactors typically employ a batch production method for such reactions, where raw materials are fed into the reactor all at once, heated to the reaction temperature and held for a period before subsequent operations such as cooling, discharging, and separation are performed after the reaction is complete. This method suffers from high energy consumption and low efficiency. After each reaction, the entire reaction system must be cooled before discharging, and reheating is required for the next production run, resulting in significant energy waste. The ammonia gas generated during the reaction is either directly emitted or simply absorbed, polluting the environment and wasting resources. The reaction system contains excess hydrazine hydrate and ethylene glycol solvent, which require complex separation and recovery processes for recycling after the reaction, further increasing production energy consumption and operating costs.

[0004] Reactive distillation, as a process intensification technique, couples chemical reactions with distillation separation within the same equipment. It continuously removes reaction products during distillation, disrupting the chemical equilibrium of reversible reactions and increasing reaction conversion rates. Simultaneously, it utilizes the heat of reaction to supply the energy required for distillation, achieving energy savings. Applying reactive distillation technology to the production of 2-hydrazino-4-methylbenzothiazole holds promise for solving the problems of high energy consumption, low efficiency, and long process duration inherent in traditional processes.

[0005] Existing reactive distillation equipment still faces some technical challenges when applied to such specific reactions. The hydrazine hydrate contained in the reaction system is highly toxic and volatile, and is prone to leakage during sampling and testing, posing a threat to the safety of operators. High-boiling-point polymers produced as byproducts during the reaction process tend to coke and accumulate on the inner walls of the equipment, affecting heat and mass transfer efficiency and, in severe cases, forcing the unit to shut down for cleaning. The efficiency of distillation separation is limited by the effectiveness of gas-liquid contact; traditional tray or packing structures struggle to achieve sufficient gas-liquid contact within a limited space, thus hindering the improvement of separation purity. Summary of the Invention

[0006] This invention addresses industry pain points in existing equipment, such as difficulty in cleaning coking, unsafe sampling operations, and high costs due to complex distillation section structures. Based on existing conventional designs, this invention proposes a steam-driven floating reciprocating coke scraping technology, a rotary safety sampling technology with mechanical interlocks, and a ring-shaped baffle-type built-in distillation technology. It achieves integrated reaction, distillation, self-cleaning, and safe sampling through a single reaction vessel, realizing continuous, energy-saving, and safe production. The invention presents an energy-saving integrated reactive distillation device and method for the production of 2-hydrazino-4-methylbenzothiazole.

[0007] To achieve the above objectives, the present invention adopts the following technical solution: An energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole includes a reactor, a baffle plate fixed inside the reactor, the baffle plate having a through hole, a coke scraping mechanism inside the through hole, and the coke scraping mechanism including a cross component fixed inside the through hole and a column fixed at the bottom of the cross component. It also includes a fixing ring fitted on the outer wall of the column, the bottom of which is fixed with a floating ring by a connecting rib plate, the inner wall of which is fixed with an inner scraper, the outer wall of which is fixed with an outer scraper, and the bottom of which is fixed with a turbine blade. When the steam generated at the bottom of the reactor rises to the through hole, it impacts the turbine blades and drives the floating ring to rotate. At the same time, the upward airflow forces the floating ring to float upward along the column. The coking on the outer wall of the column and the inner wall of the through hole is scraped off by the inner scraper and the outer scraper, respectively.

[0008] In one possible design, a limiting plate is fixed to the bottom end of the column, the limiting plate being used to prevent the floating ring from detaching from the column.

[0009] In one possible design, a sampling mechanism is provided on one side of the reactor. The sampling mechanism includes a guide tube fixedly penetrating one side of the reactor and a sampling tube rotatably sleeved on the outer wall of the guide tube. One end of the guide tube extends into the sampling tube. A piston plate is slidably connected inside the sampling tube. A sealing plate for closing the guide tube is fixed at the bottom of the piston plate, and a guide rod is fixed at the top. The top end of the guide rod slides through the sampling tube and extends above it. A tension spring is fixed between the piston plate and the top inner wall of the sampling tube. A support plate is fixed on one side of the reactor, and an arc plate that abuts against the top end of the guide rod is fixed on one side of the support plate. When the sampling tube rotates to a horizontal position, the guide rod is released from the constraint of the arc plate, and the tension spring drives the piston plate and the sealing plate to move upward, opening the guide tube for sampling.

[0010] In one possible design, the sampling mechanism further includes a discharge tube fixed to the bottom of the sampling tube, a ball valve rotatably connected inside the discharge tube, a transmission rod and a valve stem fixed to both sides of the ball valve respectively, one end of the transmission rod rotatably passing through the discharge tube and fixed to a rotating disk, and one end of the valve stem rotatably passing through the discharge tube and fixed to a handwheel; an arc-shaped fixing plate is fixed to one side of the reaction vessel, and two arc grooves are provided on one side of the arc-shaped fixing plate; a pivot that cooperates with the arc grooves is fixed to one side of the rotating disk at a position off-center; When the valve stem is turned to close the ball valve and the sampling tube is closed, the pivot rotates into the arc groove, allowing the sampling tube to rotate to a horizontal position for sampling. When the sampling tube returns to a vertical position, the handwheel is turned in the opposite direction to open the ball valve and the pivot rotates out of the arc groove, restricting the rotation of the sampling tube.

[0011] In one possible design, a collection box located below a baffle plate is fixed to one side of the inner wall of the reactor. The bottom inner wall of the collection box is provided with an inclined groove, and the bottom inner wall of the inclined groove is provided with a discharge port. One end of the guide pipe is obliquely cut and extends into the discharge port.

[0012] In one possible design, the bottom of the baffle plate has an annular ramp, the top inner diameter of which is smaller than the bottom inner diameter, and the collection box is located below the edge of the bottom inner diameter of the baffle plate.

[0013] In one possible design, an annular baffle I is fixed to the inner wall of the reactor above the feed pipe. A cylinder is fixed to the inner wall of the annular baffle I, and a fixed disk is fixed to the top of the cylinder. A distillation chamber is formed between the inner wall of the reactor, the annular baffle I, the cylinder, and the fixed disk. Multiple annular baffles II and III are fixed alternately from top to bottom in the distillation chamber. An annular gap I is formed between the inner wall of the annular baffle II and the outer wall of the cylinder, and an annular gap II is formed between the outer wall of the annular baffle III and the inner wall of the reactor. The rising steam enters the distillation chamber through the inlet hole, is gathered towards the center by the annular baffle II, moves upward through the annular gap I, and the falling condensate is guided to the edge of the inner wall of the reactor by the annular baffle III.

[0014] In one possible design, the bottom inner wall of the annular baffle I is provided with multiple drainage holes for allowing the vapor generated in the metal packing to enter the distillation chamber.

[0015] In one possible design, an exhaust pipe is fixedly installed through the top of the reactor, a condenser is fixed to one end of the exhaust pipe, and a drain pipe is fixed to the end of the condenser away from the exhaust pipe.

[0016] 1. The through hole of the baffle plate is equipped with a steam-driven floating reciprocating coke scraping mechanism, including a cross component, a column, a floating ring, an inner scraper, an outer scraper, and a turbine blade. The rising steam generated by the reaction drives the floating ring to rotate and float up and down, while removing coke from the inner wall of the through hole and the outer wall of the column.

[0017] 2. A rotary safety sampling mechanism with mechanical interlock is provided on one side of the reactor, including a guide tube, a rotating sampling tube, a piston plate, a sealing plate, a tension spring, a guide rod, an arc plate, a ball valve, a rotating disk, a pivot, and an arc-shaped fixing plate, to realize the interlock control between the ball valve and the guide tube and prevent the leakage of highly toxic materials.

[0018] 3. The reactor has an internal annular baffle-type distillation chamber at the top, which consists of annular baffle I, a cylinder, a fixed plate, and staggered annular baffles II and III, forming an S-shaped gas-liquid flow channel to achieve efficient distillation separation.

[0019] A method for using an energy-saving integrated reactive distillation unit for the production of 2-hydrazino-4-methylbenzothiazole includes the following steps: S1. The raw material is injected into the reactor through the feed pipe and falls into the metal packing area under gravity. It flows slowly downward along the surface of the packing. The heating coil heats the material in the reactor and maintains the temperature at 120 to 125°C. 4-Methyl-2-aminobenzothiazole reacts with hydrazine hydrate to generate 2-hydrazino-4-methylbenzothiazole, with ammonia as a byproduct. S2. The ammonia gas produced by the reaction escapes from the liquid phase and moves upward, passing through the metal packing and baffles, and enters the condenser from the exhaust pipe. After condensation to form ammonia water, it is collected through the drain pipe. S3. Hydrazine hydrate vaporizes upon heating to form vapor that rises into the distillation chamber. It then ascends along an S-shaped trajectory through annular gaps II and I, repeatedly contacting the descending condensate. After condensation, the ethylene glycol vapor falls back into the metal packing area, while the hydrazine hydrate vapor continues to rise to the top of the distillation chamber, condenses, and then falls back. S4. The liquid material generated by the reaction flows downward to the baffle plate, is guided to the edge by the annular inclined surface and drips into the collection box, and is collected by the inclined trough to the discharge port. It then flows continuously downward through the guide pipe and is finally discharged from the discharge pipe. S5. When the rising steam carries the by-products through the through hole, it impacts the turbine blades and drives the floating ring to rotate. The airflow force causes the floating ring to float upward along the column. After hitting the cross component, it rotates and falls back. The inner and outer scrapers cut and peel off the coking layer on the outer wall of the column and the inner wall of the through hole in the reciprocating motion. The fragments are discharged from the discharge pipe downward with the liquid phase. S6. When sampling, first turn the handwheel to close the ball valve and the sampling tube. Then turn the pivot on the rotating plate into the arc groove position. Then turn the sampling tube clockwise to the horizontal position. The top of the guide rod moves out from the bottom of the support plate and the arc plate. The tension spring pulls the piston plate and the sealing plate to move up and open the outlet of the guide tube. The material enters the sampling tube. S7. After sampling is completed, rotate the sampling tube counterclockwise to vertical position. The top of the guide rod contacts the support plate and the arc plate and is pressed down, pushing the piston plate and the sealing plate to move down and close the guide tube. The top of the guide rod is restricted below the support plate and the arc plate. Rotate the handwheel in the opposite direction to open the ball valve. The pivot rotates out of the arc groove and the sample is discharged from the discharge tube.

[0020] Beneficial effects: In this invention, a coke scraping mechanism consisting of a cross-shaped component, a column, a fixed ring, a floating ring, an inner scraper, an outer scraper, and a turbine blade is installed in the through hole of the baffle plate, thereby achieving the self-cleaning function of the gas channel. The kinetic energy of the rising steam generated during the reaction process is used as the driving force to drive the scraper to rotate and float up and down, thereby continuously and physically peeling off and removing the viscous coke adhering to the inner wall of the channel. This setup does not require the introduction of an external power source, nor does it require interruption of the production process for manual cleaning. It helps to maintain the long-term unobstructed flow of the through hole, ensures the stability of the gas flow cross-sectional area, thereby stabilizing the gas-liquid mass transfer and heat transfer efficiency of the reactive distillation process, reducing the frequency of shutdown and cleaning due to coke blockage, and ensuring that the device can operate continuously and stably for a long time. In this invention, a sampling mechanism is provided, which includes a guide tube, a rotatable sampling tube, a piston plate driven by a tension spring, a sealing plate, and a guide rod that cooperates with a support plate and an arc plate. This achieves a convenient and reliable online sampling method. In the non-sampling state, the sampling mechanism ensures that the guide tube is reliably sealed through mechanical limiting and spring force, avoiding continuous leakage of materials or gases in the reactor. During sampling, simply rotating the sampling tube will automatically open the guide tube to receive the sample. The operation is simple, and the sample is collected in an independent sampling tube, avoiding direct contact with the external environment. This helps to improve the safety of the sampling operation and reduce the pollution of volatile organic compounds to the environment. In this invention, a linkage interlocking structure consisting of a ball valve, a transmission rod, a rotating disk, a pivot, and an arc-shaped fixing plate is further provided in the sampling mechanism. This structure mechanically interlocks the opening and closing state of the ball valve with the rotation state of the sampling tube. Only when the ball valve is in the closed state, i.e., when the discharge tube is closed, can the sampling tube be rotated to the sampling position to open the guide tube to receive the sample. Conversely, during the discharge process, the ball valve can only be opened to discharge the sample when the sampling tube is in the vertical position and the guide tube is closed. This mandatory mechanical interlocking design avoids the risk of sample leakage from the discharge tube or gas escape from the guide tube in the reaction vessel during the sampling process due to incorrect operation sequence, thereby improving the safety and reliability of the sampling process. In this invention, a distillation chamber is constructed above the inside of the reactor, consisting of an annular baffle I, a cylinder, a fixed disk, and multiple staggered annular baffles II and III. Annular baffles II and III are respectively designed as inverted cones and cones, creating a compact distillation section with a tortuous gas-liquid contact path within the top space of the reactor. The rising vapor is forced to flow along an "S"-shaped path within the distillation chamber, repeatedly contacting the descending liquid. This prolongs the contact path and time between the gas and liquid phases, improving the distillation separation effect without significantly increasing the equipment height. This also helps improve the purity of the product collected after vaporization and condensation in the reaction zone, achieving integrated reaction and separation and energy coupling utilization.

[0021] In this invention, a steam-driven rotary lifting scraper mechanism is installed in the gas channel to automatically remove viscous coking material generated during the reaction process, helping to maintain long-term unobstructed flow and ensuring the stability of the reactive distillation process. Simultaneously, the device integrates a rotary sampling mechanism with mechanical interlocking. This mechanism, through the cooperation of guide rods, springs, and fixed baffles, as well as the linkage between ball valves and rotating disks, ensures the safety and reliability of the sampling and discharge process, preventing material leakage. Furthermore, the device's interior utilizes a compact distillation chamber constructed with specifically shaped and arranged annular baffles, extending the gas-liquid contact path and contributing to improved product separation purity. This device integrates reaction, distillation, online sampling, and channel anti-coking functions into one unit, with each function operating in coordination to jointly serve the continuity, safety, and stability of the production process and product quality. Attached Figure Description

[0022] Figure 1 This is a three-dimensional structural schematic diagram of an energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole provided by the present invention. Figure 2 This is a three-dimensional cross-sectional view of an energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole provided by the present invention. Figure 3 This is a cross-sectional schematic diagram of an energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole provided by the present invention; Figure 4 A three-dimensional cross-sectional view of the baffle plate of an energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole provided by the present invention; Figure 5 A three-dimensional structural schematic diagram of the cross-shaped component, column, and floating ring of an energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole provided by the present invention; Figure 6A three-dimensional exploded structural diagram of the fixed ring, floating ring, and turbine blades of an energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole provided by the present invention; Figure 7 A three-dimensional exploded structural diagram of the collection box, sampling tube, and support plate of an energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole provided by the present invention; Figure 8 A three-dimensional cross-sectional view of the sampling tube of an energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole provided by the present invention. Figure 9 This is a three-dimensional exploded view of the ball valve, arc-shaped fixing plate, and pivot of an energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole provided by the present invention. Figure 10 This is a cross-sectional view of the annular partition II, annular partition III, and cylinder of an energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole provided by the present invention. Figure 11 This is a three-dimensional cross-sectional view of the annular partition II and annular partition III of an energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole provided by the present invention.

[0023] In the diagram: 1. Reactor; 2. Feed pipe; 3. Baffle plate; 4. Metal packing; 5. Heating coil; 6. Discharge pipe; 7. Exhaust pipe; 8. Condenser; 9. Drain pipe; 10. Through hole; 11. Cross component; 12. Column; 13. Limiting plate; 14. Fixing ring; 15. Floating ring; 16. Inner scraper; 17. Outer scraper; 18. Turbine blade; 19. Collection box; 20. Inclined chute; 21. Discharge port; 22. Sampling tube; 23. Guide tube; 24. Piston plate 25. Sealing plate; 26. Guide rod; 27. Tension spring; 28. Ball bearing; 29. ​​Sample outlet tube; 30. Ball valve; 31. Valve stem; 32. Transmission rod; 33. Rotating disc; 34. Arc-shaped fixing plate; 35. Arc groove; 36. Pivot; 37. Annular partition I; 38. Cylinder; 39. Fixing disc; 40. Annular partition II; 41. Annular gap I; 42. Annular partition III; 43. Annular gap II; 44. Distillation chamber; 45. Drainage hole; 46. Support plate; 47. Arc plate. Detailed Implementation

[0024] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments.

[0025] In one embodiment: Refer to Figures 1-3An energy-saving reactive distillation integrated device for the production of 2-hydrazino-4-methylbenzothiazole is disclosed, relating to the field of chemical production technology. The device includes a reactor 1, which is a vertical cylindrical container made of corrosion-resistant metal material. A feed pipe 2 is fixed on one side of the reactor 1, penetrating the side wall of the reactor 1 and located in the upper middle part of the reactor 1. The outer end of the feed pipe 2 is provided with a flange interface for connecting to the raw material conveying pipeline. The inner end of the feed pipe 2 is bent downward so that the raw material can be evenly distributed above the metal packing 4 after injection.

[0026] Reference Figure 2 and Figure 3 A baffle plate 3 is fixed inside the reactor 1. The baffle plate 3 is an annular plate structure, and its outer edge is sealed and fixed to the inner wall of the reactor 1. The baffle plate 3 is located below the feed pipe 2. The central area of ​​the baffle plate 3 is provided with a through hole 10 for the upward steam to pass through. The bottom of the baffle plate 3 is provided with an annular inclined surface. The inner diameter of the top of the annular inclined surface is smaller than the inner diameter of the bottom, forming a conical surface that gradually expands from top to bottom. The top of the baffle plate 3 is fixed with a metal packing 4 located below the feed pipe 2. The metal packing 4 is a stepped ring or Pall ring packing made of stainless steel. The metal packing 4 is used to make the injected raw material move slowly downward under the action of gravity, prolong the residence time of the raw material in the reaction zone, and at the same time provide a surface for gas-liquid mass transfer.

[0027] Reference Figure 2 and Figure 3 A heating coil 5 is fixed near the bottom inside the reactor 1. The heating coil 5 is a spiral coil structure made of corrosion-resistant metal material. The steam inlet and steam outlet of the heating coil 5 pass through the side wall of the reactor 1. The steam inlet is connected to an external steam source, and the steam outlet is connected to a steam trap and a condensate recovery system. Steam is introduced into the heating coil 5 to provide heat energy to the inside of the reactor 1, so that the temperature of the reactants is maintained in the range of 120 to 125°C. A discharge pipe 6 is fixed at the bottom of the reactor 1. The discharge pipe 6 is located at the lowest point of the reactor 1 and is used to continuously collect the reacted material. A regulating valve is installed on the discharge pipe 6 to control the discharge flow rate and maintain a stable liquid level inside the reactor 1.

[0028] Reference Figure 3 and Figure 4 The baffle plate 3 has a through hole 10, and a coke scraping mechanism is provided in the through hole 10 to remove the coke adhering to the inner wall of the through hole 10 during the reaction process. The coke scraping mechanism includes a cross component 11 fixed in the through hole 10 and a column 12 fixed at the bottom of the cross component 11. The cross component 11 is composed of two metal strips that intersect each other perpendicularly. Both ends are welded and fixed to the inner wall of the through hole 10 to form a cross-shaped support structure. The column 12 is a cylindrical metal rod. The upper end is welded and fixed to the center position of the cross component 11, and the lower end extends vertically downward. The surface of the column 12 is polished to reduce surface roughness and reduce coke adhesion.

[0029] Reference Figures 4-6 The coking mechanism also includes a fixing ring 14 fitted onto the outer wall of the column 12. The fixing ring 14 is a circular metal part with an inner diameter larger than the outer diameter of the column 12. The inner wall of the fixing ring 14 and the outer wall of the column 12 have a smooth sliding fit. The bottom of the fixing ring 14 is fixedly connected to a floating ring 15 by multiple connecting ribs evenly distributed around the circumference. The number of connecting ribs is 3 to 4, evenly distributed around the circumference. The connecting ribs form an angle of 15 to 30 degrees with the vertical direction. The floating ring 15 is a circular metal part. The floating ring 15 is coaxially arranged with the column 12. Multiple inner scrapers 16 are fixed to the inner wall of the floating ring 15 for scraping away coking from the outer wall of the column 12. There are six inner scrapers 16, evenly distributed along the circumference of the inner wall of the floating ring 15. Each inner scraper 16 is a sheet-like metal structure with its blade facing the surface of the column 12 and contacting the outer wall of the column 12. Multiple outer scrapers 17 are fixed to the outer wall of the floating ring 15 for scraping away coking from the inner wall of the through hole 10. There are twelve outer scrapers 17, distributed along the circumference of the inner wall of the floating ring 15. The outer wall is evenly distributed around the circumference. The outer scraper 17 is a metal sheet structure with its cutting edge facing the inner wall of the through hole 10 and contacting it. Multiple turbine blades 18 are fixed to the bottom of the floating ring 15. The turbine blades 18 are oblique-bladed and drive the floating ring 15 to rotate under the impact of rising steam. There are nine turbine blades 18, evenly distributed along the bottom circumference of the floating ring 15. The turbine blades 18 are made of metal plates and are inclined at an angle of 30 to 60 degrees to the horizontal plane. When rising steam enters the through hole... Within 10 seconds, the kinetic energy of the steam impacts the turbine blade 18, and the floating ring 15 is forced to rise along the axis of the column 12 while rotating. When the floating ring 15 rises to its limit position and collides with the cross member 11, the airflow field below the turbine blade 18 is instantly disrupted, generating local turbulence and stall, and the upward aerodynamic thrust is drastically reduced. At this time, the weight of the floating ring 15 is greater than the thrust, and it automatically rotates and falls back on the column 12. After falling a certain distance, the airflow field returns to stability, and it is pushed up by the steam again.

[0030] In another embodiment, to further precisely control the reciprocating stroke of the coke scraping mechanism, the outer wall of the column 12 is machined with a reciprocating cross-spiral groove along the axial direction, and the inner wall of the fixing ring 14 is fixed with a guide pin that slides in cooperation with the cross-spiral groove. In this embodiment, the rising steam impacts the turbine blade 18, which only needs to provide the power to drive the floating ring 15 to rotate continuously in one direction. While rotating, the floating ring 15 is guided by the guide pin in the trajectory within the cross-spiral groove and is forced to spiral upward along the axial direction of the column 12. When the floating ring 15 rises to its limit position, the guide pin slides into the descending return section of the cross-spiral groove. Under the combined guidance of gravity and the return groove, the floating ring 15 continues to rotate and falls downward, thereby achieving stable reciprocating coke scraping under trajectory limitation.

[0031] Reference Figure 5 and Figure 6A limiting plate 13 is fixed to the bottom end of the column 12. The limiting plate 13 is a circular metal plate with a diameter larger than the inner diameter of the floating ring 15. The limiting plate 13 is used to limit the floating ring 15 and the inner scraper 16 to prevent the floating ring 15 from detaching from the column 12. The limiting plate 13 is welded and fixed to the bottom end of the column 12.

[0032] Specifically, steam introduced into the heating coil 5 heats the bottom of the reactor 1, causing the reactants to boil and vaporize, generating high-temperature steam. The steam contains excess hydrazine hydrate, ethylene glycol, and a small amount of byproducts. The steam flows upward, passing through the metal packing 4 area. When the rising steam enters the through-hole 10, the kinetic energy of the steam impacts the turbine blades 18. The inclined surface of the turbine blades 18 converts the airflow into rotational torque, pushing the floating ring 15, inner scraper 16, and outer scraper 17 to rotate on the column 12. At the same time, the upward airflow force acts on the turbine blades 18 and the floating ring 15, overcoming the gravity of the floating ring 15 and the turbine blades 18, causing them to float upward along the column 12. When the moving or fixed ring 14 impacts the cross member 11, the upward force weakens or disappears, and the floating ring 15, inner scraper 16 and outer scraper 17 will rotate and fall back under the action of gravity. This purely mechanical motion of rotating and floating up and down while relying on the internal steam fluid power of the system can continuously physically cut and peel off the viscous polymer attached to the outer wall of the column 12 and the inner wall of the through hole 10. During the rotation and up and down movement, the inner scraper 16 cuts and peels off the coking layer attached to the outer wall of the column 12, and the outer scraper 17 cuts and peels off the coking layer attached to the inner wall of the through hole 10. The peeled coking fragments flow downward with the liquid phase and are finally discharged from the discharge pipe 6, avoiding accumulation in the through hole 10 area and causing blockage.

[0033] Reference Figure 3 and Figure 7 A sampling mechanism is provided on one side of the reactor 1, located below the baffle plate 3, for sampling during the reaction process to facilitate subsequent testing. The sampling mechanism includes a guide pipe 23 fixedly penetrating one side of the reactor 1 and a sampling pipe 22 located on one side of the reactor 1. A collection box 19 is fixed on the inner wall of one side of the reactor 1, located below the baffle plate 3, for collecting the sample after the reaction. The collection box 19 is a box-shaped structure with an upward opening, located below the edge of the bottom inner diameter of the baffle plate 3, to receive the material after the reaction dripping from the annular inclined surface of the baffle plate 3. The bottom inner wall of the collection box 19 is provided with a trough 20 for collecting the sample. The trough 20 is a V-shaped or U-shaped groove that slopes from the bottom inner wall of the collection box 19 towards the center, with the lowest point located in the central area of ​​the collection box 19. The bottom inner wall of the trough 20 is provided with a discharge port 21 for allowing the sample to move downward when not sampling. The discharge port 21 is a circular through hole located at the lowest point of the trough 20.

[0034] Reference Figure 3 and Figure 7One end of the guide tube 23 extends into the discharge port 21. The guide tube 23 is a metal round tube. One end of the guide tube 23 is beveled with an angle of 30°-60°. The sample in the discharge port 21 enters the guide tube 23 through the bevel. The bevel increases the opening area at the end of the guide tube 23, ensuring that the material enters the guide tube 23 smoothly and avoiding material accumulation and blockage at the tube opening. The other end of the guide tube 23 penetrates the side wall of the reactor 1 and extends to the outside of the reactor 1. The guide tube 23 is fixed to the side wall of the reactor 1 by sealing welding.

[0035] Reference Figure 8 The sampling tube 22 is rotatably sleeved on the outer wall of the guide tube 23, with one end of the guide tube 23 extending into the sampling tube 22. The sampling tube 22 is a metal circular tube. A rotary sealing structure is provided between the sampling tube 22 and the guide tube 23. This rotary sealing structure includes at least two high-temperature resistant graphite packing seals sleeved on the guide tube 23, and an annular isolation cavity set between the two seals. The isolation cavity is connected to an external nitrogen source through a pipeline to form an air curtain barrier to prevent external air from entering and internal highly toxic gas from leaking. The packing in the sealing stuffing box is also made of high-temperature resistant graphite material, and a pressure cap adjusting bolt is provided on the stuffing box to compensate for packing wear. Thus, the sampling tube 22 can rotate around the axis of the guide tube 23 while maintaining a seal. A piston plate 24 is slidably connected inside the sampling tube 22. The piston plate 24 is a circular metal plate with an outer diameter matching the inner diameter of the sampling tube 22. A sealing ring is provided circumferentially on the piston plate 24 to form a sliding seal with the inner wall of the sampling tube 22. A sealing plate 25 for sealing the guide tube 23 is fixed to the bottom of the piston plate 24. The sealing plate 25 is fixedly connected to the bottom surface of the piston plate 24 via a connecting rod. The sealing plate 25 is positioned opposite to the end of the guide tube 23. When the piston plate 24 is located below the sampling tube 22, the sealing plate 25 presses against the end of the guide tube 23, sealing the outlet of the guide tube 23. A guide rod 26 is fixed to the top of the piston plate 24. The guide rod 26 is a metal round rod, and the top end of the guide rod 26 slides through the top inner wall of the sampling tube 22 and... Extending above the sampling tube 22, a guide sleeve is provided between the guide rod 26 and the top of the sampling tube 22 to ensure that the guide rod 26 moves vertically up and down. A tension spring 27 is fixed between the top of the piston plate 24 and the top inner wall of the sampling tube 22 through a spring seat. The upper end of the tension spring 27 is hooked on the spring seat on the top inner wall of the sampling tube 22, and the lower end is hooked on the spring seat on the top of the piston plate 24. The tension spring 27 is in a stretched state during installation, applying an upward pulling force to the piston plate 24.

[0036] Reference Figure 3 , Figure 7 and Figure 8The top of the guide rod 26 is provided with a rolling ball 28 to reduce the friction between the guide rod 26 and the support plate 46 and the arc plate 47. The ball 28 is a stainless steel ball that is embedded in the groove at the top of the guide rod 26 and can roll freely. The support plate 46 is fixed on one side of the reactor 1. The support plate 46 is a metal plate that is horizontally fixed to the outer wall of the reactor 1 and located above the sampling tube 22. The arc plate 47 is fixed on one side of the support plate 46. The arc plate 47 is an arc-shaped metal plate that is fixedly connected to the support plate 46. The arc-shaped curved surface of the arc plate 47 faces downward and abuts against the ball 28 at the top of the guide rod 26. When the sampling tube 22 is in a vertical state, the ball 28 contacts the arc-shaped curved surface of the arc plate 47. The arc plate 47 applies downward pressure to the guide rod 26 through the ball 28, restricting the guide rod 26 from moving upward.

[0037] Reference Figure 3 and Figures 7-9 The sampling mechanism also includes a discharge pipe 29 fixed to the bottom of the sampling tube 22 for discharging the sample. The discharge pipe 29 is a metal round tube that communicates with the inside of the sampling tube 22. A ball valve 30 is rotatably connected inside the discharge pipe 29 to control its opening or closing. The ball valve 30 has a ball through which fluid can pass. A transmission rod 32 and a valve stem 31 are fixed to both sides of the ball valve 30, respectively. One end of the valve stem 31 rotatably passes through the discharge pipe 29 and is fixed with a handwheel. The handwheel is used to operate the valve stem 31 to rotate. A sealing packing gland is provided between the valve stem 31 and the discharge pipe 29 to ensure sealing during rotation. One end of the transmission rod 32 rotatably passes through the discharge pipe 29. A rotating disk 33 is fixed thereon, and a sealing structure is also provided between the transmission rod 32 and the sample discharge tube 29. An arc-shaped fixing plate 34 is fixed on one side of the reactor 1. The arc-shaped fixing plate 34 is a metal plate with an arc shape. The radius of the arc matches the rotation trajectory of the sampling tube 22. Two arc grooves 35 are provided on one side of the arc-shaped fixing plate 34, corresponding to the position of the pivot 36 when the sampling tube 22 is in the horizontal and vertical states. The arc groove 35 is an oblong groove with a width slightly larger than the diameter of the pivot 36. A pivot 36 is fixed on one side of the rotating disk 33 at a position off the center. The pivot 36 is a cylindrical metal pin. The pivot 36 cooperates with the arc groove 35 and can be embedded in the arc groove 35.

[0038] Specifically, when sampling is required, first turn the handwheel, which drives the ball valve 30 to rotate 90 degrees via the valve stem 31, causing the ball valve 30 to close the sampling tube 29. When the valve stem 31 rotates, it drives the rotating disk 33 to rotate synchronously via the transmission rod 32. The pivot 36 on the rotating disk 33 rotates accordingly. When the ball valve 30 completely closes the sampling tube 29, the pivot 36 rotates to the position of the arc groove 35 on the arc-shaped fixing plate 34 and is embedded in the arc groove 35. After the sampling tube 29 is closed, rotate the sampling tube 22 clockwise to make it horizontal. During the rotation of the sampling tube 22, the ball bearing 28 at the top of the guide rod 26 moves out from the bottom of the support plate 46 and the arc plate 47, releasing the limit on the guide rod 26. The tension of the tension spring 27 acts on the piston plate 24, pulling the piston plate 24 and the sealing plate 25 upward. After the sealing plate 25 moves upward, the outlet of the guide tube 23 is opened. The raw materials that have reacted in the reactor 1 through the metal packing 4 enter the sampling tube 22 through the guide tube 23. The oblique cut at the end of the guide tube 23 ensures that the material enters smoothly, completing the sampling operation. After sampling is completed, the sampling tube 22 is rotated counterclockwise to restore it to a vertical position. During the rotation of the sampling tube 22, the ball bearing 28 at the top of the guide rod 26 gradually contacts the support plate 46 and the arc plate 47. The arc-shaped surface of the arc plate 47 pushes the guide rod 26 downward, overcoming the tension of the tension spring 27, causing the piston plate 24 and the sealing plate 25 to move down and reset. The sealing plate 25 re-closes the outlet of the guide tube 23. When the sampling tube 22 is completely vertical, the ball bearing 28 is located below the support plate 46 and the arc plate 47 and is restricted from moving upward, keeping the guide tube 23 in a closed state. At this time, the pivot 36 is once again in another position. When a sample needs to be discharged for testing at the end of the arc groove 35, the handwheel is turned in the opposite direction, which drives the ball valve 30 to rotate via the valve stem 31. The ball valve 30 opens the discharge tube 29, and at the same time, the transmission rod 32 drives the rotating disk 33 to rotate. The pivot 36 rotates out of the arc groove 35, and the sample in the sampling tube 22 is discharged and collected through the discharge tube 29. The ball bearing 28 at the top of the guide rod 26 keeps the guide tube 23 closed under the restriction of the support plate 46 and the arc plate 47. After the sample is discharged, the handwheel is turned again to close the discharge tube 29 with the ball valve 30. At the same time, the pivot 36 rotates back to the position of the arc groove 35 to prepare for the next sampling.

[0039] Reference Figure 3 An exhaust pipe 7 is fixedly installed through the top of the reactor 1. The exhaust pipe 7 is located at the center of the top of the reactor 1. A condenser 8 is fixed at one end of the exhaust pipe 7. The condenser 8 is a shell-and-tube or plate heat exchanger. A drain pipe 9 is fixed at the end of the condenser 8 away from the exhaust pipe 7. The ammonia gas generated in the reactor 1 enters the condenser 8 through the exhaust pipe 7 and is condensed to form ammonia water. The ammonia water is discharged and collected through the drain pipe 9 for subsequent treatment or as a by-product.

[0040] In another embodiment: Refer to Figure 10 and Figure 11An annular baffle I 37 is fixed to the inner wall of the reactor 1 above the feed pipe 2. The annular baffle I 37 is an annular plate structure, and its outer edge is sealed and fixedly connected to the inner wall of the reactor 1. A cylindrical body 38 is fixed to the inner wall of the annular baffle I 37. The cylindrical body 38 is a cylindrical structure and is coaxially arranged with the annular baffle I 37. The lower end of the cylindrical body 38 is sealed and fixedly connected to the inner edge of the annular baffle I 37. A fixed plate 39 is fixed to the top of the cylindrical body 38. The fixed plate 39 is a circular plate structure and is sealed and fixedly connected to the top of the cylindrical body 38. A distillation chamber 44 is formed between the inner wall of the reactor 1, the annular baffle I 37, the cylindrical body 38, and the fixed plate 39. The distillation chamber 44 is an annular space. Multiple annular baffles II 40 and annular baffles III 42 are fixed from top to bottom in the distillation chamber 44. The multiple annular baffles II 40 and annular baffles III 42 are arranged alternately. The number of annular baffles II 40 is 3 to 6. The number of III42 is 3 to 6, and the number of both is the same. The annular partition II40 is an annular plate structure, and its outer edge is sealed and fixedly connected to the inner wall of the reactor 1. An annular gap I41 is formed between the inner wall of the annular partition II40 and the outer wall of the cylinder 38. The top diameter of the annular partition II40 is larger than the bottom diameter, forming a conical surface that gradually decreases from top to bottom. The annular partition III42 is an annular plate structure, and its inner edge is sealed and fixedly connected to the outer wall of the cylinder 38. An annular gap II43 is formed between the outer wall of the annular partition III42 and the inner wall of the reactor 1. The top diameter of the annular partition III42 is smaller than the bottom diameter, forming a conical surface that gradually increases from top to bottom. The bottom inner wall of the annular partition I37 is provided with multiple drainage holes 45. The number of drainage holes 45 is 6 to 12, and they are evenly distributed along the circumference. They are used to allow the vapor generated in the metal packing 4 during the reaction to enter the distillation chamber 44 through the drainage holes 45.

[0041] Specifically, the rising steam enters the distillation chamber 44 through the guide hole 45, passes through annular gap II 43 and annular gap I 41, and continues to rise. The steam is forced to flow towards the inner wall of the reactor 1, and moves upward along an S-shaped trajectory within the distillation chamber 44, repeatedly contacting the descending condensate in the annular space. The higher-boiling-point ethylene glycol vapor gradually condenses into liquid during its movement, flows downward under gravity, is guided to the edge of the column wall by annular baffle III 42, falls back through annular gap II 43 and annular gap I 41 to the area of ​​annular baffle I 37, and then returns to the metal packing 4 area through the guide hole 45. The lower-boiling-point hydrazine hydrate vapor continues to rise to the top of the distillation chamber 44, condenses into liquid when it encounters the lower-temperature areas such as the fixed plate 39 and the top of the reactor 1, and similarly falls back to the reaction zone. This physical structure forces the gas and liquid phases to form a cross-cutting trajectory within the annular space, prolonging the physical contact time between gas and liquid and improving the distillation purity.

[0042] A method for using an energy-saving integrated reactive distillation unit for the production of 2-hydrazino-4-methylbenzothiazole includes the following steps: S1. The raw material is injected into the reactor 1 through the feed pipe 2 and falls into the metal packing 4 area under the action of gravity. The metal packing 4 is composed of a metal material with a large specific surface area. The raw material spreads into a liquid film on the surface of the packing and flows slowly downward along the tortuous channel of the packing, which prolongs the residence time in the reaction zone. The heating coil 5 is installed near the bottom of the reactor 1 and a heating medium is introduced to provide heat energy to the material in the reactor. The reaction temperature is maintained in the range of 120 to 125°C. 4-Methyl-2-aminobenzothiazole and hydrazine hydrate undergo a nucleophilic substitution reaction under high temperature conditions to generate the target product 2-hydrazino-4-methylbenzothiazole, while ammonia is produced as a byproduct. S2. The ammonia gas produced during the reaction has an extremely low boiling point and exists in gaseous form at the reaction temperature. After escaping from the liquid phase, it moves upward, passes through the metal packing 4 region and the baffle 3, and finally enters the condenser 8 from the exhaust pipe 7 at the top of the reactor 1. The ammonia gas is condensed by the cooling medium in the condenser 8 to form ammonia water, which is collected through the drain pipe 9 and recycled as a by-product. The ammonia gas is continuously removed from the reaction system, pushing the reaction equilibrium to the positive direction and improving the raw material conversion rate. S3. In the reaction system, the excess hydrazine hydrate has a boiling point of approximately 120°C, close to the reaction temperature. Some of the hydrazine hydrate vaporizes upon heating, forming steam that rises. The ethylene glycol solvent has a boiling point of approximately 197°C, and only a small amount vaporizes at the reaction temperature. The rising mixed vapor enters the distillation chamber 44 for separation. The rising vapor enters the bottom of the distillation chamber 44 through the guide hole 45, and moves upward along an S-shaped trajectory within the distillation chamber 44 through annular gaps II 43 and I 41, repeatedly contacting the descending condensate in the annular space. The higher-boiling-point ethylene glycol vapor... During the movement, it gradually condenses into a liquid and flows downward under the action of gravity. It is guided to the edge of the tower wall by the annular baffle III 42 and falls back to the metal packing 4 area through the annular gap to continue to participate in the reaction. The hydrazine hydrate vapor with a lower boiling point continues to rise to the top of the distillation chamber 44. When it encounters the cooler equipment wall, it condenses into a liquid and falls back to the reaction zone. Through this gas-liquid countercurrent contact, the initial separation of hydrazine hydrate and ethylene glycol is achieved. The hydrazine hydrate vapor rises to the top of the tower and condenses and flows back, while the ethylene glycol condenses and falls back in the distillation chamber 44, forming an internal circulation. S4. The 2-hydrazino-4-methylbenzothiazole produced in the reaction has a high boiling point and exists in liquid form at the reaction temperature. It flows downward along with excess hydrazine hydrate and ethylene glycol. When the material flows to the region of baffle 3, baffle 3 acts as a barrier and convergence point for the liquid phase. The bottom of baffle 3 has an annular inclined surface with an inner diameter that gradually increases from top to bottom, guiding the downward-flowing liquid to the edge of the annular inclined surface and finally dripping into the collection box 19. The collection box 19 is located at the bottom inner diameter of baffle 3. Below the edge, the liquid phase material after the reaction is received. The bottom inner wall of the collection box 19 is provided with a sloping groove 20, which allows the material to converge at the lowest point of the sloping groove 20. The bottom of the sloping groove 20 is provided with a discharge port 21. One end of the guide pipe 23 extends into the discharge port 21, and the end of the guide pipe 23 is slanted to facilitate the material to enter the guide pipe 23. In the non-sampling state, the material flows continuously downward through the discharge port 21 and the guide pipe 23, and is finally discharged from the discharge pipe 6 at the bottom of the reactor 1 to enter the subsequent process. S5. During the reaction, when the rising steam carries a small amount of high-boiling-point byproducts through the through-hole 10, due to the small cross-section of the through-hole 10, the flow velocity increases. Some byproducts condense and accumulate on the inner wall of the through-hole 10 and the outer wall of the column 12, gradually forming a coking layer. The coking scraping mechanism automatically removes these coke deposits using the hydrodynamic force of the rising steam. The steam generated by the heating coil 5 flows from bottom to top. When the steam enters the area of ​​the through-hole 10, the kinetic energy of the steam impacts the turbine blades 18, pushing the floating ring 15, the inner scraper 16, and the outer scraper 17 to rotate around the column 12. Depending on the specific mechanical configuration of the device, the reciprocating motion of the floating ring 15 is achieved through one of the following two methods: Method 1: The airflow force causes the floating ring to... 15 floats upward along the smooth column 12. After hitting the cross component 11, it loses its support due to the airflow disturbance and rotates back under the action of gravity. Alternatively, the rising steam drives the floating ring 15 to rotate in one direction. Through the cooperation of the guide pin on the inner wall of the fixed ring 14 and the reciprocating cross spiral groove on the outer wall of the column 12, the floating ring 15 is forced to move up and down along a predetermined mechanical trajectory. During the rotation and up and down movement, the inner scraper 16 cuts and peels off the coking layer attached to the outer wall of the column 12. The outer scraper 17 cuts and peels off the coking layer attached to the inner wall of the through hole 10. The peeled coking fragments flow downward with the liquid phase and are finally discharged from the discharge pipe 6, avoiding accumulation in the through hole 10 area and causing blockage. S6. When sampling and testing are required during the reaction process, operate the sampling mechanism to collect materials. Before sampling, first turn the handwheel to drive the ball valve 30 to rotate 90 degrees via the valve stem 31, so that the ball valve 30 closes the discharge pipe 29. When the valve stem 31 rotates, it drives the rotating disk 33 to rotate synchronously via the transmission rod 32. The pivot 36 on the rotating disk 33 rotates accordingly. When the ball valve 30 completely closes the discharge pipe 29, the pivot 36 rotates exactly to the position of the arc groove 35 on the arc-shaped fixing plate 34. The arc-shaped fixing plate 34 is fixed to one side of the reactor 1 and has two arc grooves 35, which correspond to the positions of the pivot 36 when the sampling pipe 22 is in the horizontal and vertical states, respectively. After the discharge pipe 29 is closed, rotate clockwise. The sampling tube 22 is placed in a horizontal position. During the rotation of the sampling tube 22, the top of the guide rod 26 moves out from the bottom of the support plate 46 and the arc plate 47, releasing the limit on the guide rod 26. The tension of the tension spring 27 acts on the piston plate 24, pulling the piston plate 24 and the sealing plate 25 upward. After the sealing plate 25 moves upward, the outlet of the guide tube 23 is opened. The material in the reactor 1 that has reacted in the area of ​​the metal packing 4 enters the sampling tube 22 through the guide tube 23. The end of the guide tube 23 extends into the discharge port 21 and is obliquely cut to ensure that the material enters the guide tube 23 smoothly. When the sampling tube 22 is rotated to a horizontal position, the pivot 36 is exactly located in the arc groove 35, so that the sampling tube 22 can rotate smoothly into position. S7. After the material enters the sampling tube 22 and fills its internal space, after sampling is completed, the sampling tube 22 is rotated counterclockwise to restore its vertical position. During the rotation of the sampling tube 22, the top of the guide rod 26 gradually contacts the support plate 46 and the arc plate 47. The arc-shaped surface of the arc plate 47 pushes the guide rod 26 downward, overcoming the tension of the tension spring 27, causing the piston plate 24 and the sealing plate 25 to move down and reset. The sealing plate 25 re-closes the outlet of the guide tube 23. When the sampling tube 22 is completely vertical, the top of the guide rod 26 is located below the support plate 46 and the arc plate 47 and is restricted from moving upward, keeping the guide tube 23 in a closed state. At this time, the pivot 36 is again located... At the end of the other arc groove 35, when a sample needs to be discharged for testing, the handwheel is turned in the opposite direction, which drives the ball valve 30 to rotate via the valve stem 31. The ball valve 30 opens the discharge pipe 29, and at the same time, the transmission rod 32 drives the rotating disk 33 to rotate. The pivot 36 rotates out of the arc groove 35, and the sample in the sampling tube 22 is discharged and collected through the discharge pipe 29. After the sample is discharged, the handwheel is turned again to close the discharge pipe 29 with the ball valve 30. At the same time, the pivot 36 rotates back to the position of the arc groove 35 to prepare for the next sampling. During the entire sampling process, the ball valve 30 and the outlet of the guide pipe 23 cannot be opened at the same time to ensure that the highly toxic material in the reactor 1 is always isolated from the outside world.

[0043] Those skilled in the art will understand that, in order to ensure the long-term stable operation of the device, the wear of the inner scraper 16 and the outer scraper 17 of the coke scraping mechanism needs to be checked regularly, and the floating ring 15 assembly needs to be replaced as needed; at the same time, the rotary sealing structure and stuffing box in the sampling mechanism also need to be checked and maintained regularly, and the sealing packing needs to be replaced when necessary, in order to ensure the sealing performance of the device.

[0044] The accompanying drawings in this application are for illustrative purposes only. The dimensions and shapes of the components shown are not actual limitations but are merely schematic representations. In actual implementation, the components can be reasonably configured and adjusted according to specific needs and actual conditions.

[0045] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. An energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole, comprising a reactor (1), wherein a baffle plate (3) is fixed inside the reactor (1), and the baffle plate (3) is provided with through holes (10), characterized in that, The through hole (10) is provided with a coke scraping mechanism, which includes a cross component (11) fixed in the through hole (10) and a column (12) fixed at the bottom of the cross component (11). It also includes a fixing ring (14) fitted on the outer wall of the column (12). The bottom of the fixing ring (14) is fixed with a floating ring (15) by a connecting rib plate. The inner wall of the floating ring (15) is fixed with an inner scraper (16), the outer wall is fixed with an outer scraper (17), and the bottom is fixed with a turbine blade (18). When the steam generated at the bottom of the reactor (1) rises to the through hole (10), it impacts the turbine blade (18) and drives the floating ring (15) to rotate. At the same time, the upward airflow forces the floating ring (15) to float upward along the column (12). The coking on the outer wall of the column (12) and the inner wall of the through hole (10) are scraped off by the inner scraper (16) and the outer scraper (17), respectively.

2. The energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole according to claim 1, characterized in that, A limiting plate (13) is fixed to the bottom end of the column (12), and the limiting plate (13) is used to restrict the floating ring (15) from detaching from the column (12).

3. The energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole according to claim 2, characterized in that, A sampling mechanism is provided on one side of the reactor (1). The sampling mechanism includes a guide pipe (23) fixedly penetrating one side of the reactor (1) and a sampling tube (22) rotatably sleeved on the outer wall of the guide pipe (23). One end of the guide pipe (23) extends into the sampling tube (22). A piston plate (24) is slidably connected inside the sampling tube (22). A sealing plate (25) for sealing the guide pipe (23) is fixed at the bottom of the piston plate (24), and a guide rod (26) is fixed at the top. The top of the guide rod (26) slides through to take samples. The tube (22) extends above it, and a tension spring (27) is fixed between the piston plate (24) and the top inner wall of the sampling tube (22); a support plate (46) is fixed on one side of the reactor (1), and an arc plate (47) that abuts against the top of the guide rod (26) is fixed on one side of the support plate (46); when the sampling tube (22) rotates to a horizontal state, the guide rod (26) is released from the constraint of the arc plate (47), and the tension spring (27) drives the piston plate (24) and the sealing plate (25) to move upward, opening the guide tube (23) for sampling.

4. The energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole according to claim 3, characterized in that, The sampling mechanism also includes a discharge pipe (29) fixed at the bottom of the sampling tube (22). A ball valve (30) is rotatably connected inside the discharge pipe (29). A transmission rod (32) and a valve stem (31) are fixed on both sides of the ball valve (30). One end of the transmission rod (32) rotatably passes through the discharge pipe (29) and is fixed with a rotating disk (33). One end of the valve stem (31) rotatably passes through the discharge pipe (29) and is fixed with a handwheel. An arc-shaped fixing plate (34) is fixed on one side of the reactor (1). Two arc grooves (35) are provided on one side of the arc-shaped fixing plate (34). A pivot (36) that cooperates with the arc grooves (35) is fixed on one side of the rotating disk (33) at a position off-center.

5. The energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole according to claim 4, characterized in that, A collection box (19) located below the baffle plate (3) is fixed on one side of the inner wall of the reactor (1). The bottom inner wall of the collection box (19) is provided with a sloping groove (20). The bottom inner wall of the sloping groove (20) is provided with a discharge port (21). One end of the guide pipe (23) is sloping and extends into the discharge port (21).

6. The energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole according to claim 5, characterized in that, The bottom of the baffle plate (3) is provided with an annular inclined surface, the top inner diameter of the annular inclined surface is smaller than the bottom inner diameter, and the collection box (19) is located below the edge of the bottom inner diameter of the baffle plate (3).

7. The energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole according to claim 6, characterized in that, The inner wall of the reactor (1) is fixed with an annular baffle I (37) located above the feed pipe (2). The inner wall of the annular baffle I (37) is fixed with a cylinder (38). The top of the cylinder (38) is fixed with a fixed plate (39). A distillation chamber (44) is formed between the inner wall of the reactor (1), the annular baffle I (37), the cylinder (38) and the fixed plate (39). Multiple annular baffles II (40) and annular baffles III (42) are fixed alternately from top to bottom in the distillation chamber (44). An annular gap I (41) is formed between the inner wall of the annular baffle II (40) and the outer wall of the cylinder (38). An annular gap II (43) is formed between the outer wall of the annular baffle III (42) and the inner wall of the reactor (1). The rising steam enters the distillation chamber (44) through the guide hole (45), is gathered towards the center by the annular baffle II (40), moves upward through the annular gap I (41), and the falling condensate is guided to the inner wall edge of the reactor (1) by the annular baffle III (42).

8. The energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole according to claim 7, characterized in that, The bottom inner wall of the annular partition I (37) is provided with multiple drainage holes (45) for allowing the steam generated in the metal packing (4) to enter the distillation chamber (44).

9. The energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole according to claim 8, characterized in that, An exhaust pipe (7) is fixedly inserted through the top of the reactor (1). A condenser (8) is fixed at one end of the exhaust pipe (7), and a drain pipe (9) is fixed at the end of the condenser (8) away from the exhaust pipe (7).

10. A method of using an energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole, applied to the energy-saving integrated reactive distillation apparatus for the production of 2-hydrazino-4-methylbenzothiazole as described in claim 9, characterized in that... Includes the following steps: S1. The raw material is injected into the reactor (1) through the feed pipe (2) and falls into the metal packing (4) area under the action of gravity. It flows slowly downward along the surface of the packing. The heating coil (5) heats the material in the reactor and maintains the temperature at 120 to 125°C. 4-methyl-2-aminobenzothiazole reacts with hydrazine hydrate to generate 2-hydrazyl-4-methylbenzothiazole, and ammonia is produced as a byproduct. S2. The ammonia gas produced by the reaction escapes from the liquid phase and moves upward, passing through the metal packing (4) and the baffle (3), and enters the condenser (8) from the exhaust pipe (7). After condensation to form ammonia water, it is collected through the drain pipe (9). S3, hydrazine hydrate vaporizes upon heating to form steam that enters the distillation chamber (44) upwards. It rises along an S-shaped trajectory through annular gap II (43) and annular gap I (41), repeatedly contacting the descending condensate. After the ethylene glycol vapor condenses, it falls back to the metal packing (4) area. The hydrazine hydrate vapor continues to rise to the top of the distillation chamber (44), condenses, and then falls back. S4. The liquid material generated by the reaction flows downward to the baffle plate (3), is guided to the edge by the annular inclined surface and drips into the collection box (19), and is gathered to the discharge port (21) through the inclined groove (20), and flows continuously downward through the guide pipe (23) and is finally discharged from the discharge pipe (6); S5. When the rising steam carries the by-products through the through hole (10), it impacts the turbine blades (18) and pushes the floating ring (15) to rotate. The airflow force causes the floating ring (15) to float upward along the column (12). After hitting the cross component (11), it rotates and falls back. The inner scraper (16) and the outer scraper (17) cut and peel off the coking layer on the outer wall of the column (12) and the inner wall of the through hole (10) in the reciprocating motion. The fragments are discharged from the discharge pipe (6) with the liquid phase downward. S6. When sampling, first turn the handwheel to close the discharge tube (29) with the ball valve (30), turn the pivot (36) on the rotating disk (33) into the arc groove (35) position, then turn the sampling tube (22) clockwise to the horizontal position, the top of the guide rod (26) moves out from the bottom of the support plate (46) and the arc plate (47), the tension spring (27) pulls the piston plate (24) and the closing plate (25) to move upward, open the outlet of the guide tube (23), and the material enters the sampling tube (22). S7. After sampling is completed, rotate the sampling tube (22) counterclockwise to vertical. The top of the guide rod (26) is pressed down after contacting the support plate (46) and the arc plate (47), pushing the piston plate (24) and the sealing plate (25) to move down and close the guide tube (23). The top of the guide rod (26) is restricted below the support plate (46) and the arc plate (47). Rotate the handwheel in the opposite direction to open the ball valve (30). The pivot (36) rotates out from the arc groove (35), and the sample is discharged from the discharge tube (29).

Images