A hydrolysis apparatus for producing p-toluenesulfonyl chloride

Abstract

This invention relates to the field of p-toluenesulfonyl chloride production technology, specifically to a hydrolysis apparatus for producing p-toluenesulfonyl chloride. It includes a vessel body, a driving device mounted on the upper end of the vessel body, and a convex box fixed to the outer side of the upper part of the vessel body, communicating with the vessel body. A stirring device is installed inside the vessel body, and the driving device can drive the stirring device to stir the materials inside the vessel body. A pressurizing device is installed inside the convex box, and the movement of a limiting rod can drive the pressurizing device. The pressurizing device is connected to a water tank, and can intermittently pressurize water from the water tank into a connecting hole and an arc-shaped hole, and then spray it out through a nozzle. This invention enables a turntable to drive a rotating ring and a stirring rod to rotate eccentrically inside the vessel body. During the hydrolysis reaction, water can be evenly dripped into the hydrolysis reaction vessel, and stirring can be performed simultaneously during the even dripping of water into the hydrolysis reaction vessel, thereby improving the efficiency of the hydrolysis reaction.

Description

Technical Field

[0001] This invention relates to the field of p-toluenesulfonyl chloride production technology, specifically to a hydrolysis apparatus for producing p-toluenesulfonyl chloride. Background Technology

[0002] p-Toluenesulfonyl chloride, a fine chemical product, is widely used in the dye, pharmaceutical, and pesticide industries. In the dye industry, it is mainly used as an intermediate in the manufacture of disperse, ice dye, and acid dyes; in the pharmaceutical industry, it is mainly used in the production of sulfonamides such as mesotrione; and in the pesticide industry, it is mainly used in the production of mesotrione, sulfadiazine, and metalaxyl. With the continuous development of the dye, pharmaceutical, and pesticide industries, the international demand for this product is increasing, and the market prospects are broad.

[0003] The processing technology for p-toluenesulfonyl chloride includes the following steps: Step 1, toluenesulfonyl chloride production: A certain amount of chlorosulfonic acid is manually selected and added to a reaction vessel. Under an environment of 30-50℃, a certain amount of toluene is added dropwise to the reaction vessel under negative pressure. After the addition is complete, the temperature is raised and kept at that temperature. Step 2, hydrolysis reaction: The mixture in the reaction vessel from Step 1 is added to the hydrolysis reaction vessel and stirred, while water is added dropwise under negative pressure. Step 3, adjusting the reaction temperature: Simultaneously with Step 2, heat conduction is performed in the hydrolysis reaction vessel to slow down the cooling rate. Step 4, dissolution reaction: After the water has been added dropwise, stirring is started after a period of time. After stirring is completed, solvent gasoline from the oil container is introduced into the hydrolysis reaction vessel. Step 5, settling and separation: After settling, the layers are separated. The lower water layer is placed in a wastewater storage tank, and the solvent layer is added to a crystallization vessel for cooling and crystallization. After crystallization is complete, centrifugation is performed to obtain the finished product.

[0004] In step two above, the existing hydrolysis reactor cannot uniformly add water during the water droplet process. Therefore, it is necessary to increase the stirring time to ensure uniform mixing of the mixture and water, thereby reducing the efficiency of the hydrolysis reaction. Summary of the Invention

[0005] The technical problem to be solved by the present invention is a hydrolysis device for producing p-toluenesulfonyl chloride that can uniformly add water to the hydrolysis reactor during the hydrolysis reaction process, and can also stir while uniformly adding water to the hydrolysis reactor, thereby improving the efficiency of the hydrolysis reaction.

[0006] To achieve the above objectives, the technical solution provided by this invention is as follows:

[0007] A hydrolysis apparatus for producing p-toluenesulfonyl chloride includes a vessel body with a driving device mounted on its upper end. The apparatus is characterized by a convex box fixed to the outer side of the upper part of the vessel body, the convex box communicating with the vessel body. A stirring device is installed inside the vessel body, and the driving device can drive the stirring device to stir the materials inside the vessel body. The stirring device includes a turntable eccentrically fixedly connected to the driving device, the turntable being rotatably engaged within a rotating ring. Multiple stirring rods are fixed to the lower end of the rotating ring, and a limiting rod is fixed to one side of the rotating ring. A rotating seat is rotatably connected inside the convex box, and the limiting rod passes through the rotating seat, slidingly connecting the limiting rod to the rotating seat. An arc-shaped hole is opened inside the rotating ring, and multiple spray holes communicating with the arc-shaped hole are opened at the lower end of the rotating ring. A connecting hole is opened inside the limiting rod, communicating with the arc-shaped hole. A water tank is fixed to the upper end of the convex box, communicating with the connecting hole. A pressurizing device is installed inside the convex box, and the movement of the limiting rod can drive the pressurizing device, which is connected to the water tank. The pressurizing device can intermittently press water from the water tank into the connecting hole and the arc-shaped hole, and then spray it out through the spray holes.

[0008] Specifically, a feed pipe is fixed at the upper end of the vessel body, and a discharge pipe is fixed at the lower end of the vessel body.

[0009] Specifically, a temperature sensor and a pressure sensor are installed inside the upper end of the vessel body, and a pressure regulating valve is installed at the upper end of the vessel body. The pressure regulating valve is electrically connected to the pressure sensor through a controller.

[0010] Specifically, the driving device includes a mounting plate fixed to the upper end of the vessel body, a motor fixed on the mounting plate, a first gear fixed on the output shaft of the motor, a rotating shaft rotatably connected to the upper end of the vessel body, a second gear fixed on the rotating shaft, the second gear meshing with the first gear, and the lower end of the rotating shaft eccentrically fixedly connected to the turntable.

[0011] Specifically, the pressurization device includes a piston plate that is slidably and sealed within the convex box. The piston plate is slidably and sealed to the inner wall of the convex box. The piston plate is elastically connected to the side wall of the convex box relative to the vessel body via a spring. The space between the side wall of the convex box parallel to the piston plate and the piston plate is connected to the upper end of the water tank via a connecting pipe. A water outlet is provided at the upper end of the convex box and is connected to the water tank. The water outlet is connected to a connecting hole via a flexible hose. A water inlet pipe is fixed at the upper end of the water tank. A first one-way valve is fixedly installed inside the water inlet pipe. The first one-way valve can only be opened to the inside of the water tank. A second one-way valve is fixedly installed inside the water outlet. The second one-way valve can only be opened to the outside of the water tank.

[0012] Specifically, the end of the limiting rod facing the piston plate is rotatably connected to a roller.

[0013] Specifically, the outer edge of the turntable is provided with an annular groove, and a retaining ring is fixed on the inner edge of the rotating ring, with the retaining ring located in the groove.

[0014] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0015] 1. This invention enables the turntable to drive the rotating ring and stirring rod to rotate eccentrically inside the reactor. During the hydrolysis reaction, water can be evenly added to the hydrolysis reactor. While the water is being evenly added to the hydrolysis reactor, stirring can be carried out, which can improve the efficiency of the hydrolysis reaction.

[0016] 2. The turntable drives the rotating ring and stirring rod to rotate eccentrically inside the vessel. The limiting rod reciprocates inside the convex box and intermittently drives the piston plate. During the reciprocating motion of the piston plate inside the convex box, it can intermittently press the water in the water tank into the connecting hole and the arc-shaped hole and spray it out through the spray hole, thereby realizing the intermittent dripping of water into the vessel. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the present invention.

[0018] Figure 2 This is a schematic diagram of the drive unit.

[0019] Figure 3 A cross-sectional view showing the fit between the turntable and the rotating ring.

[0020] Figure 4 This is a schematic diagram of the turntable.

[0021] Figure 5 This is a schematic diagram showing the interaction between the rotating ring and the stirring rod.

[0022] Figure 6 for Figure 2 A magnified view of region A in the middle.

[0023] Figure 7 for Figure 3 A magnified view of region B in the middle.

[0024] The names of the parts in the attached diagram are:

[0025] 1. Kettle body; 2. Feed pipe; 3. Discharge pipe; 4. Mounting plate; 5. Motor; 51. First gear; 6. Second gear; 7. Rotating shaft; 8. Turntable; 9. Slot; 10. Rotating ring; 11. Snap ring; 12. Stirring rod; 13. Limiting rod; 14. Arc-shaped hole; 141. Connecting hole; 15. Spray hole; 16. Rotating seat; 17. Roller; 18. Piston plate; 19. Spring; 20. Connecting pipe; 21. Water tank; 22. Water inlet pipe; 23. Water outlet; 24. Temperature sensor; 25. Pressure sensor; 26. Pressure regulating valve; 27. Hose; 28. Protruding box. Detailed Implementation

[0026] like Figures 1-7As shown, a hydrolysis apparatus for producing p-toluenesulfonyl chloride includes a vessel body 1. A feed pipe 2 is fixed to the upper end of the vessel body 1, and a discharge pipe 3 is fixed to the lower end. A temperature sensor 24 and a pressure sensor 25 are installed inside the upper end of the vessel body 1. A pressure regulating valve 26 is also installed at the upper end of the vessel body 1, and the pressure regulating valve 26 is electrically connected to the pressure sensor 25 via a controller. The temperature sensor 24 monitors the temperature inside the vessel body 1 in real time. The pressure sensor 25 monitors the pressure inside the vessel body 1 in real time. When the negative pressure inside the vessel body 1 falls below a set pressure, the controller opens the pressure regulating valve 26, allowing outside air to enter the vessel body 1 and thus regulating the internal pressure.

[0027] A drive unit is installed at the upper end of the vessel body 1. A protruding box 28 is fixed to the outer side of the upper part of the vessel body 1, and the protruding box 28 is connected to the vessel body 1. A stirring device is installed inside the vessel body 1, and the drive unit can drive the stirring device to stir the material inside the vessel body 1.

[0028] The driving device includes a mounting plate 4 fixed to the upper end of the vessel body 1, a motor 5 fixed on the mounting plate 4, and a first gear 51 fixed on the output shaft of the motor 5. A rotating shaft 7 is rotatably connected to the upper end of the vessel body 1, and a second gear 6 is fixed on the rotating shaft 7. The second gear 6 meshes with the first gear 51. The lower end of the rotating shaft 7 is eccentrically fixedly connected to a turntable 8.

[0029] The stirring device includes a turntable 8 eccentrically fixedly connected to a drive device. An annular groove 9 is formed on the outer edge of the turntable 8, and a retaining ring 11 is fixed to the inner edge of a rotating ring 10, with the retaining ring 11 located within the groove 9. Multiple stirring rods 12 are fixed to the lower end of the rotating ring 10. A limiting rod 13 is fixed to one side of the rotating ring 10, and a rotating seat 16 is rotatably connected inside a convex box 28. The limiting rod 13 passes through the rotating seat 16, and the limiting rod 13 is slidably connected to the rotating seat 16.

[0030] An arc-shaped hole 14 is provided inside the rotating ring 10, and multiple spray holes 15 communicating with the arc-shaped hole 14 are provided at the lower end of the rotating ring 10. A connecting hole 141 is provided inside the limiting rod 13, and the connecting hole 141 communicates with the arc-shaped hole 14. A water tank 21 is fixed at the upper end of the convex box 28, and the water tank 21 communicates with the connecting hole 141. A pressurizing device is provided inside the convex box 28. During the movement of the limiting rod 13, the pressurizing device can be driven. The pressurizing device is connected to the water tank 21, and the pressurizing device can force the water in the water tank 21 into the connecting hole 141 and the arc-shaped hole 14 and spray it out through the spray holes 15.

[0031] The pressurization device includes a piston plate 18 that is slidably and sealingly connected to the convex box 28. A roller 17 is rotatably connected to one end of the limiting rod 13 facing the piston plate 18. The piston plate 18 is slidably and sealingly connected to the inner wall of the convex box 28. The piston plate 18 and the convex box 28 are elastically connected to the side wall of the vessel body 1 by a spring 19. The space between the side wall of the convex box 28 parallel to the piston plate 18 and the piston plate 18 is connected to the upper end of the water tank 21 via a connecting pipe 20. An outlet 23 is provided at the upper end of the convex box 28, which is connected to the water tank 21 and is connected to a connecting hole 141 via a flexible hose 27. An inlet pipe 22 is fixedly installed at the upper end of the water tank 21. A first one-way valve is fixedly installed inside the inlet pipe 22, which can only open into the water tank 21. A second one-way valve is fixedly installed inside the outlet 23, which can only open outwards from the water tank 21. The water level in water tank 21 is lower than the position of water inlet pipe 22.

[0032] In use, the inside of the vessel body 1 is heated by a heating coupler, and the material is added into the vessel body 1 through the feed pipe 2. Then, the vessel body 1 is evacuated to maintain the set negative pressure.

[0033] Then, motor 5 is started. Motor 5 drives the rotating shaft 7 to rotate via the first gear 51 and the second gear 6. During the rotation of the rotating shaft 7, the turntable 8 and the rotating ring 10 are driven to rotate eccentrically. As the turntable 8 drives the rotating ring 10 to rotate eccentrically inside the vessel body 1, the rotating ring 10 will cause the limiting rod 13 to swing on the rotating seat 16. During the swinging of the limiting rod 13 on the rotating seat 16, it will slide on the rotating seat 16. That is, during the eccentric rotation of the rotating ring 10 and the turntable 8 inside the vessel body 1, the limiting rod 13 will continuously swing and slide inside the convex box 28. During the eccentric rotation of the rotating ring 10 and the turntable 8 inside the vessel body 1, the stirring rod 12 can stir the material inside the vessel body 1.

[0034] As the limiting rod 13 continuously swings and slides within the convex box 28, the roller 17 on the limiting rod 13 intermittently presses the piston plate 18. Under the push of the limiting rod 13 and the roller 17, the piston plate 18 moves away from the vessel body 1, compressing the spring 19 and increasing the pressure inside the water tank 21. At this time, the second one-way valve in the outlet 23 opens, and the first one-way valve closes. Water from the water tank 21 enters the connecting hole 141 and the arc-shaped hole 14 through the hose 27 and is sprayed into the vessel body 1 through the spray hole 15.

[0035] When the limit rod 13 and roller 17 move away from the piston plate 18, the piston plate 18 moves towards the vessel body 1 under the elastic force of the spring 19, creating negative pressure in the water tank 21. At this time, the first one-way valve in the water inlet pipe 22 opens and the second one-way valve closes, allowing external water to enter the water tank 21 and replenish it.

[0036] As the rotating ring 10 rotates eccentrically within the vessel body 1, the water discharged from the nozzle 15 can be evenly dripped into the vessel body 1. Simultaneously, the stirring rod 12 rotates along with the rotating ring 10. Therefore, during the hydrolysis reaction, water can be evenly dripped into the vessel body 1, and stirring can be performed simultaneously, thus improving the efficiency of the hydrolysis reaction.

[0037] After the hydrolysis reaction is complete, gasoline solvent is added. After settling, the mixture automatically separates into layers. The lower aqueous layer is placed in a wastewater storage tank, and the solvent layer is added to a crystallization reactor for cooling and crystallization. After crystallization is complete, centrifugation is performed to obtain the final product.

[0038] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A hydrolysis apparatus for producing p-toluenesulfonyl chloride, comprising a vessel body (1), wherein a driving device is mounted on the upper end of the vessel body (1), characterized in that, A protruding box (28) is fixed on the outer side of the upper part of the vessel body (1). The protruding box (28) is connected to the vessel body (1). A stirring device is installed inside the vessel body (1). The driving device can drive the stirring device to stir the material inside the vessel body (1). The stirring device includes a turntable (8) that is eccentrically fixed to the driving device. The turntable (8) is rotatably engaged in the rotating ring (10). Multiple stirring rods (12) are fixed at the lower end of the rotating ring (10). A limiting rod (13) is fixed on one side of the rotating ring (10). A rotating seat (16) is rotatably connected inside the protruding box (28). The limiting rod (13) passes through the rotating seat (16). The limiting rod (13) is slidably connected to the rotating seat (16). The rotating ring ( 10) An arc-shaped hole (14) is provided inside. Multiple spray holes (15) communicating with the arc-shaped hole (14) are provided at the lower end of the rotating ring (10). A connecting hole (141) is provided inside the limiting rod (13). The connecting hole (141) is connected with the arc-shaped hole (14). A water tank (21) is fixed at the upper end of the convex box (28). The water tank (21) is connected with the connecting hole (141). A pressurizing device is provided inside the convex box (28). The pressurizing device can drive the pressurizing device during the movement of the limiting rod (13). The pressurizing device is connected with the water tank (21). The pressurizing device can intermittently press the water in the water tank (21) into the connecting hole (141) and the arc-shaped hole (14) and through the spray holes (15). The drive device includes a mounting plate (4) fixed to the upper end of the vessel body (1), a motor (5) fixed on the mounting plate (4), a first gear (51) fixed on the output shaft of the motor (5), a rotating shaft (7) rotatably connected to the upper end of the vessel body (1), a second gear (6) fixed on the rotating shaft (7), the second gear (6) meshing with the first gear (51), and the lower end of the rotating shaft (7) eccentrically fixedly connected to the turntable (8); the pressurizing device includes a piston plate (18) slidably sealed in the convex box (28), the piston plate (18) slidably sealed to the inner wall of the convex box (28), and the piston plate (18) and the convex box (28) are connected to the side wall of the vessel body (1) through. The space between the side wall of the convex box (28) parallel to the piston plate (18) and the piston plate (18) is connected to the upper end of the water tank (21) through the connecting pipe (20) via the connecting pipe (20). The upper end of the convex box (28) is provided with a water outlet (23), which is connected to the water tank. The water outlet (23) is connected to the connecting hole (141) through the flexible hose (27). The upper end of the water tank (21) is fixed with a water inlet pipe (22). A first one-way valve is fixedly installed inside the water inlet pipe (22). The first one-way valve can only be opened into the water tank (21). A second one-way valve is fixedly installed inside the water outlet (23). The second one-way valve can only be opened out of the water tank (21).

2. The hydrolysis apparatus for producing p-toluenesulfonyl chloride according to claim 1, characterized in that, The upper end of the vessel body (1) is fixed with a feed pipe (2), and the lower end of the vessel body (1) is fixed with a discharge pipe (3).

3. The hydrolysis apparatus for producing p-toluenesulfonyl chloride according to claim 1, characterized in that, A temperature sensor (24) and a pressure sensor (25) are installed inside the upper end of the vessel body (1). A pressure regulating valve (26) is installed at the upper end of the vessel body (1). The pressure regulating valve (26) is electrically connected to the pressure sensor (25) through a controller.

4. The hydrolysis apparatus for producing p-toluenesulfonyl chloride according to claim 1, characterized in that, The end of the limiting rod (13) facing the piston plate (18) is rotatably connected to a roller (17).

5. The hydrolysis apparatus for producing p-toluenesulfonyl chloride according to claim 1, characterized in that, The turntable (8) has an annular groove (9) on its outer edge, and a retaining ring (11) is fixed on the inner edge of the rotating ring (10), with the retaining ring (11) located in the groove (9).

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