A mixing device for o-tolidine solvent-free sulfonation reaction
By designing a mixing device that integrates abrasive, spraying, and stirring components, the safety hazards and incomplete mixing issues when mixing o-phenylenediamine and concentrated sulfuric acid were resolved, achieving a highly efficient reaction with controllable temperature.
Patent Information
- Application Number
- CN202521768675.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-20
- Publication Date
- 2026-08-25
- Estimated Expiration
- 2035-08-20
AI Technical Summary
When o-phenylenediamine is directly mixed with concentrated sulfuric acid, a violent reaction occurs, leading to safety hazards, difficulty in temperature control, insufficient mixing, and low product yield.
A mixing device was designed, which includes abrasive, spraying, stirring and reaction sections. The crushing, spraying and stirring mechanisms ensure that o-phenylenediamine and concentrated sulfuric acid are fully mixed, and the reaction temperature is stabilized by a temperature control system.
This reduces safety hazards, improves the thoroughness of mixing and product yield, and ensures the safety and efficiency of the reaction process.
Smart Images
Figure CN224672699U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to a mixing device, and more particularly to a device that can fully and reliably mix o-phenylenediamine and concentrated sulfuric acid, belonging to the technical field of mixing equipment. Background Technology
[0002] When o-phenylenediamine comes into direct contact with concentrated sulfuric acid, it triggers a violent exothermic reaction. Currently, the mixing of o-phenylenediamine and concentrated sulfuric acid involves directly adding both materials into a reaction vessel and stirring. This process produces a large amount of white smoke and a rapid temperature rise, making the reaction difficult to control and posing safety hazards on-site. Furthermore, the impellers in the current stirring vessel cannot break up agglomerates, resulting in high raw material residue and low main product yield, which affects the quality of the mixture. Therefore, a mixing device that can ensure thorough mixing without agglomeration and with controllable temperature is needed. Utility Model Content
[0003] The purpose of this invention is to overcome the shortcomings of the prior art and provide a mixing device for the solventless sulfonation reaction of o-phenylenediamine, which can not only reduce safety hazards during mixing, but also improve the fullness of mixing.
[0004] The problem described in this utility model is solved by the following technical solution: A mixing device for the solventless sulfonation reaction of o-phenylenediamine includes an abrasive section, a spraying section, a stirring section, and a reaction section; the abrasive section, the spraying section, and the stirring section are all disposed on the reaction section; the reaction section includes a reactor shell, an outer sheath, and a stainless steel coil; the reactor shell is disposed on the ground via a bottom support; the outer sheath is disposed at the bottom of the outer wall of the reactor shell, and there is a closed cavity between the outer sheath and the outer wall of the reactor, and a connector is provided in this closed cavity to connect to a water source via a water pipe, and a valve is provided on the water pipe; a drain valve is provided at the bottom of the outer insulation sleeve; the stainless steel coil is coiled on the inner wall of the reactor shell, and it is connected to a thermal oil furnace via a pipe.
[0005] The above-mentioned mixing device for solventless sulfonation reaction of o-phenylenediamine includes an abrasive section comprising a feeding hopper, a pulverizer, and a screw conveyor; the feeding hopper is located directly above the pulverizer; the discharge port of the pulverizer is connected to the inlet of the screw conveyor, and the discharge port of the screw conveyor is connected to the first pair of interfaces on the top surface of the side wall of the reactor shell.
[0006] The above-mentioned mixing device for the solventless sulfonation reaction of o-phenylenediamine includes a spraying section comprising a sulfuric acid storage tank, a fluoroplastic pump, and a stainless steel nozzle; the sulfuric acid storage tank is connected to the fluoroplastic pump via a pipeline; the stainless steel nozzle is located at the top of the side wall of the reactor shell, and the nozzle head is located inside the reactor shell; the outlet of the fluoroplastic pump is connected to the inlet of the stainless steel nozzle.
[0007] The above-mentioned mixing device for the solventless sulfonation reaction of o-phenylenediamine includes a stirring part comprising a lifting mechanism and a stirring mechanism; the lifting mechanism is disposed on the top surface of the outer wall of the reactor shell; the stirring mechanism is disposed on the lifting mechanism; a visible quartz glass is disposed on the top side wall of the reactor shell; a thermocouple is disposed at the bottom of the inner wall of the reactor shell; a display screen is disposed on the outer wall of the reactor shell, and the signal output terminal of the thermocouple is connected to the signal input terminal of the display screen.
[0008] The above-mentioned mixing device for the solventless sulfonation reaction of o-phenylenediamine includes a stirring mechanism comprising a hydraulic motor, a central rod, an upper impeller, a lower impeller, and a sleeve; a hole is provided at the center of the top surface of the reactor shell, and a sleeve is installed inside the hole; the central rod passes through the sleeve; both the top and bottom ports of the sleeve are provided with lip seals made of fluororubber; a lower impeller is provided at the bottom of the side wall of the central rod, and an upper impeller is provided on the side wall of the central rod, with the upper impeller located directly above the lower impeller, and the maximum outer diameter of the upper impeller being smaller than the maximum outer diameter of the lower impeller; the output shaft of the hydraulic motor is connected to the top of the central rod.
[0009] The above-mentioned mixing device for the solventless sulfonation reaction of o-phenylenediamine includes a lifting mechanism comprising a hydraulic cylinder, a guide rod, and a fixed plate. The fixed plate is mounted on the top surface of the reactor shell via a bracket. The fixed plate has a through hole and a guide hole. The guide rod passes through the guide hole of the fixed plate, and its bottom end is connected to the top surface of the hydraulic motor housing. The hydraulic cylinder is mounted on the top surface of the fixed plate, and the end of its piston rod passes through the through hole of the fixed plate and is connected to the top surface of the hydraulic motor housing. The centerlines of the hydraulic cylinder piston rod, the guide rod, and the center rod are parallel.
[0010] This invention further refines o-phenylenediamine through an abrasive section, allowing for a more complete subsequent reaction; the spraying section enables concentrated sulfuric acid to be sprayed in finer form, resulting in a larger contact area between the concentrated sulfuric acid and o-phenylenediamine and a faster reaction; the stirring section ensures a more complete reaction between the concentrated sulfuric acid and o-phenylenediamine without agglomeration; and the temperature control in the reaction section ensures the reaction process is as safe as possible. Attached Figure Description
[0011] Figure 1 This is a schematic diagram of the structure of this utility model.
[0012] The list of labels in the diagram is as follows: 1. Reactor shell, 2. Outer sleeve, 3. Stainless steel coil, 4. Feeding hopper, 5. Crusher, 6. Screw conveyor, 7. Sulfuric acid storage tank, 8. Hydraulic motor, 9. Center rod, 10. Blade, 11. Sleeve, 12. Hydraulic cylinder, 13. Guide rod, 14. Fixing plate. Detailed Implementation
[0013] See Figure 1 This utility model includes an abrasive part, a spraying part, a stirring part, and a reaction part; the abrasive part, the spraying part, and the stirring part are all arranged on the reaction part; the function of the abrasive part is to further refine the o-phenylenediamine, so that its subsequent reaction is more complete; the stirring part makes the reaction more complete and prevents agglomeration; the reaction part effectively controls the temperature during the reaction process.
[0014] The reaction section includes a reactor shell 1, an outer sheath 2, and a stainless steel coil 3. The reactor shell 1 is mounted on the ground via a bottom support. The outer sheath 2 is located at the bottom of the outer wall of the reactor shell 1, and a closed cavity exists between the outer sheath 2 and the outer wall of the reactor. This closed cavity is equipped with a connector that connects to a water source via a water pipe, and a valve is installed on the water pipe. A drain valve is installed at the bottom of the outer sheath. Cooling water is injected into the outer sheath to lower the temperature inside the reactor shell 1, preventing the initial reaction temperature from becoming too high. The stainless steel coil 3 is coiled around the inner wall of the reactor shell 1 and is connected to a thermal oil heater via a pipe. Hot oil is injected into the stainless steel coil 3 through the thermal oil heater to heat the inside of the reactor shell, ensuring a more complete reaction in the later stages.
[0015] The abrasive section includes a feeding bin 4, a crusher 5, and a screw conveyor 6. The feeding bin 4 is located directly above the crusher 5. The discharge port of the crusher 5 is connected to the inlet of the screw conveyor 6, and the discharge port of the screw conveyor 6 is connected to the first pair of interfaces on the top side wall of the reactor shell 1. The o-phenylenediamine is placed in the feeding bin 4, and then further crushed and refined by the crusher 5, and finally transported to the interior of the reactor shell 1 by the screw conveyor 6.
[0016] The spraying section includes a sulfuric acid storage tank 7, a fluoroplastic pump, and a stainless steel nozzle. The sulfuric acid storage tank 7 is connected to the fluoroplastic pump via a pipeline. The sulfuric acid storage tank 7 stores concentrated sulfuric acid. The stainless steel nozzle is located at the top of the side wall of the reactor shell 1, and the nozzle head is located inside the reactor shell 1. The outlet of the fluoroplastic pump is connected to the inlet of the stainless steel nozzle. The fluoroplastic pump can effectively pump the concentrated sulfuric acid in the sulfuric acid storage tank 7 to the stainless steel nozzle, and finally spray it from the stainless steel nozzle into the interior of the reactor shell.
[0017] The stirring section includes a lifting mechanism and a stirring mechanism; the lifting mechanism is located on the top surface of the outer wall of the reactor shell 1; the lifting mechanism can adjust the vertical position of the stirring mechanism to ensure that it can mix and stir the materials in the reactor at a suitable position; the stirring mechanism is mounted on the lifting mechanism; a visible quartz glass is provided on the top side wall of the reactor shell 1; the visible quartz glass is a standard configuration for reactors, and its function is to facilitate the observation of the internal conditions of the reactor by the staff; a thermocouple is provided at the bottom of the inner wall of the reactor shell 1, and a display screen is provided on the outer wall of the reactor shell 1, with the signal output terminal of the thermocouple connected to the signal input terminal of the display screen; the thermocouple can monitor the temperature inside the reactor in real time, and then display the internal temperature of the reactor through the display screen.
[0018] The stirring mechanism includes a hydraulic motor 8, a central rod 9, an upper blade, a lower blade 10, and a sleeve 11. A hole is provided at the center of the top surface of the reactor shell 1, and the sleeve 11 is installed inside the hole. The central rod 9 passes through the sleeve 11. Both the top and bottom ports of the sleeve 11 are equipped with lip seals made of fluororubber. The lower blade 10 is located at the bottom of the side wall of the central rod 9, and the upper blade is located on the side wall of the central rod, directly above the lower blade. The maximum outer diameter of the upper blade is smaller than the maximum outer diameter of the lower blade 10. This results in a lower linear velocity at the edge of the upper blade compared to the edge of the lower blade. The output shaft of the hydraulic motor 8 is connected to the top of the central rod 9. The rotating central rod 9 drives the blades to rotate, and the rotating blades stir and mix the materials inside the reactor. The hydraulic motor drives the central rod 9 to rotate, thereby stirring the materials inside the reactor.
[0019] The lifting mechanism includes a hydraulic cylinder 12, a guide rod 13, and a fixed plate 14. The fixed plate 14 is mounted on the top surface of the reactor shell 1 via a bracket. The fixed plate 14 has through holes and guide holes. The guide rod 13 passes through the guide hole of the fixed plate 14, and the bottom end of the guide rod 13 is connected to the top surface of the hydraulic motor 8 housing. The guide rod 13 provides guidance for the lifting of the hydraulic motor 8, ensuring its reliable lifting. The hydraulic cylinder 12 is mounted on the top surface of the fixed plate 14, and the end of its piston rod passes through the through hole of the fixed plate 14 and is connected to the top surface of the hydraulic motor 8 housing. The hydraulic cylinder 12 can drive the hydraulic motor 8 to lift vertically, thereby adjusting the position of the blades so that the blades can appear at the appropriate height at the appropriate time. The axis of the piston rod of the hydraulic cylinder 12, the axis of the guide rod 13, and the axis of the center rod 9 are parallel.
[0020] Operating principle: A certain amount of concentrated sulfuric acid is pre-added into the reactor. The concentrated sulfuric acid serves as the substrate, meaning it is both a reactant and a solvent. o-Phenylenediamine is placed in the feeding hopper 4 and awaits feeding. The crusher 5 is started to crush and refine the material in the feeding hopper 4, and the feeding is controlled by the screw conveyor 6. The screw conveyor 6 feeds the material every three to five minutes, and all the o-Phenylenediamine is added into the reactor shell 1 within five feeding cycles. During the feeding process, concentrated sulfuric acid in the sulfuric acid storage tank 7 is sprayed into the reactor shell 1 through a fluoroplastic pump and stainless steel nozzles to participate in the reaction. During the above process, the height of the lower impeller 10 is controlled by the hydraulic cylinder 12, maintaining it at the middle height of the reactants and stirring at a speed of 250 rpm to break up the materials and prevent agglomeration. During the feeding process, the cooling water inside the outer casing 2 is used to control the reaction temperature of the material in the reactor below 60°C until all the material has been added. After all the material has been added, and it has reached a completely melted state with a stable temperature below 60°C, the cooling water inside the outer casing 2 is drained to cancel the cooling operation. The thermal oil heater is started to inject hot oil into the stainless steel coil 3 to heat the material in the reactor until it reaches 140°C. Then, the lower impeller is lowered to the bottom and rotated at a speed of 1000-1200 rpm. The upper and lower impellers simultaneously stir the material, accelerating the reaction and high-shear dispersion to prevent material agglomeration and break it up. After the reaction is completed, the thermal oil heater is turned off and allowed to cool down until it drops below 60°C, at which point the reaction is complete.
Claims
1. A mixing apparatus for the solvent-free sulfonation reaction of o-phenylenediamine, characterized in that: It includes an abrasive section, a spraying section, a stirring section, and a reaction section; the abrasive section, the spraying section, and the stirring section are all located on the reaction section; the reaction section includes a reactor shell (1), an outer sleeve (2), and a stainless steel coil (3); the reactor shell (1) is set on the ground by a bottom support; the outer sleeve (2) is located at the bottom of the outer wall of the reactor shell (1), and there is a closed cavity between the outer sleeve (2) and the outer wall of the reactor, and a connector is provided in this closed cavity to connect to a water source through a water pipe, and a valve is provided on the water pipe, and a drain valve is provided at the bottom of the outer insulation sleeve; the stainless steel coil (3) is coiled on the inner wall of the reactor shell (1), and it is connected to the heat transfer oil furnace through a pipe.
2. The mixing apparatus for the solventless sulfonation reaction of o-phenylenediamine according to claim 1, characterized in that: The abrasive part includes a feeding bin (4), a crusher (5) and a screw conveyor (6); the feeding bin (4) is located directly above the crusher (5); the discharge port of the crusher (5) is connected to the inlet of the screw conveyor (6), and the discharge port of the screw conveyor (6) is connected to the first pair of interfaces on the top side wall of the reactor shell (1).
3. The mixing apparatus for the solventless sulfonation reaction of o-phenylenediamine according to claim 2, characterized in that: The spraying section includes a sulfuric acid storage tank (7), a fluoroplastic pump, and a stainless steel nozzle; the sulfuric acid storage tank (7) is connected to the fluoroplastic pump through a pipeline; the stainless steel nozzle is located at the top of the side wall of the reactor shell (1), and the nozzle head of the stainless steel nozzle is located inside the reactor shell (1); the outlet of the fluoroplastic pump is connected to the inlet of the stainless steel nozzle.
4. The mixing apparatus for the solventless sulfonation reaction of o-phenylenediamine according to claim 3, characterized in that: The stirring part includes a lifting mechanism and a stirring mechanism; the lifting mechanism is set on the top surface of the outer wall of the reactor shell (1); the stirring mechanism is set on the lifting mechanism; a visible quartz glass is set on the top side wall of the reactor shell (1); a thermocouple is set at the bottom of the inner wall of the reactor shell (1); a display screen is set on the outer wall of the reactor shell (1), and the signal output end of the thermocouple is connected to the signal input end of the display screen.
5. The mixing apparatus for the solventless sulfonation reaction of o-phenylenediamine according to claim 4, characterized in that: The stirring mechanism includes a hydraulic motor (8), a central rod (9), an upper blade, a lower blade (10), and a sleeve (11); a hole is provided at the center of the top surface of the reactor shell (1), and a sleeve (11) is provided inside the hole; the central rod (9) passes through the sleeve (11); the top and bottom ports of the sleeve (11) are provided with lip seals, and the material of the lip seals is fluororubber; the bottom of the side wall of the central rod (9) is provided with a lower blade (10), and an upper blade is provided on the side wall of the central rod, and the upper blade is located directly above the lower blade, and the maximum outer diameter of the upper blade is smaller than the maximum outer diameter of the lower blade (10); the output shaft of the hydraulic motor (8) is connected to the top of the central rod (9).
6. The mixing apparatus for the solventless sulfonation reaction of o-phenylenediamine according to claim 5, characterized in that: The lifting mechanism includes a hydraulic cylinder (12), a guide rod (13), and a fixed plate (14); the fixed plate (14) is mounted on the top surface of the reactor shell (1) by a bracket; the fixed plate (14) is provided with a through hole and a guide hole; the guide rod (13) passes through the guide hole of the fixed plate (14), and the bottom end of the guide rod (13) is connected to the top surface of the hydraulic motor (8) shell; the hydraulic cylinder (12) is mounted on the top surface of the fixed plate (14), and the end of its piston rod passes through the through hole of the fixed plate (14) and is connected to the top surface of the hydraulic motor (8) shell; the center line of the piston rod of the hydraulic cylinder (12), the center line of the guide rod (13), and the center line of the central rod (9) are parallel.