Deep sulfonation device and method for improving active matter

Abstract

The invention discloses a deep sulfonation device and method for improving active matter, and relates to the technical field of sulfonation process.The deep sulfonation device comprises a tank body and an adjusting mechanism, the inner wall of the tank body is sequentially connected with a top plate, a partition plate and a bottom plate from top to bottom, and a plurality of reaction pipes are connected between the partition plate and the bottom plate in an annular array mode; the upper end of each reaction tube penetrates through the partition plate and is coaxially connected with a liquid supply cylinder, the lower end of each reaction tube penetrates through the bottom plate, the upper end of each liquid supply cylinder penetrates through the top plate, each liquid supply cylinder is provided with an annular slit, and the adjusting mechanism is installed in the tank body and used for adjusting the sulfonation reaction intensity on the inner walls of the reaction tubes. According to the invention, the sulfonation reaction intensity in the reaction tube is periodically adjusted, and the rising temperature in the high-intensity sulfonation reaction time period is cooled by utilizing the low-intensity sulfonation reaction time, so that the temperature in the reaction tube is always kept within a proper threshold value, and the generation of by-products is avoided, thereby improving the content of active matters.

Description

Technical Field

[0001] This invention relates to the field of sulfonation technology, and in particular to an apparatus and method for improving the depth of sulfonation of active ingredients. Background Technology

[0002] Sulfonation is an important organic chemical reaction process, which refers to the reaction process of introducing sulfonic acid groups into organic compound molecules. It has wide applications in many fields such as chemical industry, pharmaceutical industry, and dye industry. Dodecylbenzene sulfonation is the process of converting dodecylbenzene into dodecylbenzene sulfonic acid through a chemical reaction.

[0003] In the sulfonation process of dodecylbenzenesulfonic acid, a multi-tube membrane sulfonation reactor is mainly used. The multi-tube membrane sulfonation reactor realizes a heterogeneous gas-liquid two-phase reaction through vertically arranged tube bundles. Since the sulfonation reaction is a strongly exothermic process, the upper region of the tube bundle has a high SO3 concentration and slow liquid film flow, resulting in a strong sulfonation reaction. However, the cooling and heat dissipation capacity of traditional jackets is limited. After a period of use, local overheating will occur in the upper part of the tube bundle of the multi-tube membrane sulfonation reactor. The occurrence of overheating can easily induce the generation of by-products and reduce the content of active ingredients. Therefore, a device and method for improving the depth of sulfonation of active ingredients is proposed. Summary of the Invention

[0004] The purpose of this invention is to solve the problems in the prior art by providing an apparatus and method for improving the depth of sulfonation of active ingredients.

[0005] A device and method for improving the deep sulfonation of active ingredients includes a tank and an adjustment mechanism. A top plate, a partition plate, and a bottom plate are sequentially connected from top to bottom on the inner wall of the tank. Multiple reaction tubes are connected between the partition plate and the bottom plate in a ring array. The upper end of each reaction tube penetrates the partition plate and is coaxially connected to a liquid supply cylinder. The lower end of each reaction tube penetrates the bottom plate, and the upper end of the liquid supply cylinder penetrates the top plate. Each liquid supply cylinder has an annular slit. The adjustment mechanism is installed inside the tank and is used to adjust the sulfonation reaction intensity on the inner wall of the reaction tubes.

[0006] Preferably, the adjusting mechanism includes a motor and multiple annular rotating plates. The motor is mounted on the top outer wall of the tank. A rotating shaft is rotatably connected to the center of the top of the tank. The output shaft of the motor is coaxially connected to the rotating shaft. The lower end of the rotating shaft is connected to an outer arc-shaped rack and an inner arc-shaped rack via two connecting rods. Four sliding grooves are formed around each liquid supply cylinder on the top plate. A slider is slidably connected in each sliding groove. A 90° fan-shaped baffle is connected to the top of each slider. Four guide blocks are connected around each liquid supply cylinder on the top plate. Four guide grooves are formed on each annular rotating plate. The four guide blocks are slidably connected to the four guide grooves on the annular rotating plate, allowing the annular rotating plate to rotate slightly. The annular rotating plate is coaxially arranged with the liquid supply cylinder. A limit rod is connected to each baffle. Four arc-shaped limit grooves are formed on each annular rotating plate. The four limit rods are slidably connected to the four limit grooves on the annular rotating plate. A gear ring is coaxially connected to the outer ring surface of each annular rotating plate.

[0007] Preferably, each of the liquid supply cylinders has an annular groove communicating with an annular slit, and a lifting ring is slidably connected in the annular groove. The top of the liquid supply cylinder has two symmetrically distributed lifting grooves communicating with the annular groove. The upper part of the lifting ring is connected to two symmetrical lifting blocks, and the two lifting blocks are slidably connected to the two lifting grooves respectively. The top of the lifting ring is connected to multiple springs, and the upper end of each spring is connected to the top wall of the annular groove. The bottom of the two baffles near the lifting grooves is connected to inclined blocks.

[0008] Preferably, the outer arc-shaped rack and the inner arc-shaped rack have the same number of teeth, and both the outer arc-shaped rack and the inner arc-shaped rack mesh with the gear ring when they rotate. The angle between the outer arc-shaped rack and the inner arc-shaped rack on the rotating shaft can be adjusted.

[0009] Preferably, the top of the tank is provided with an air inlet, the bottom of the tank is provided with a discharge outlet, the bottom outer wall of the tank is connected with multiple support legs, the inner wall of the tank is connected with a liquid collection hopper located directly below the bottom plate, and the outer wall of the tank is provided with an air outlet located below the liquid collection hopper.

[0010] Preferably, an inlet is provided on the outer wall of the tank, between the top plate and the partition, and a water inlet and an outlet are provided on the outer wall of the tank, between the partition and the bottom plate.

[0011] A method of using a device for enhancing the deep sulfonation of active ingredients includes the following steps:

[0012] S1. Prepare a sulfur trioxide-air mixture containing 4% to 7% sulfur trioxide as a sulfonating agent, and prepare a dodecylbenzene solution;

[0013] S2. The sulfonating agent is introduced into the tank through the air inlet, and the dodecylbenzene solution is injected into the tank through the liquid inlet. The dodecylbenzene solution forms a liquid film in the reaction tube and reacts with the introduced sulfonating agent.

[0014] S3. During the production of dodecylbenzene sulfonic acid in the device, the regulating mechanism is activated to periodically adjust the sulfonation reaction intensity in each reaction tube to increase the content of active ingredients.

[0015] Compared with existing technologies, the advantages of this invention are:

[0016] The present invention is equipped with an adjustment mechanism that periodically adjusts the intensity of the sulfonation reaction in the reaction tube. By using the low-intensity sulfonation reaction time to cool the temperature rise during the high-intensity sulfonation reaction time, the temperature in the reaction tube is always kept within a suitable threshold, avoiding the formation of by-products and thus increasing the content of active ingredients. Attached Figure Description

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

[0018] Figure 2 This is a cross-sectional view of the structure of the present invention.

[0019] Figure 3 This is a schematic diagram of the adjustment mechanism in this invention.

[0020] Figure 4 This is a schematic diagram of the bottom structure of the annular rotating plate in this invention.

[0021] Figure 5 This is a cross-sectional view of the adjusting mechanism in this invention.

[0022] Figure 6 for Figure 5 Enlarged diagram of point A in the middle.

[0023] Figure 7 This is a cross-sectional view of the liquid supply cylinder in this invention.

[0024] In the diagram: 1. Tank body, 11. Top plate, 12. Baffle plate, 13. Bottom plate, 14. Reaction tube, 141. Water inlet, 142. Water outlet, 15. Liquid collection hopper, 151. Gas outlet, 16. Support leg, 17. Gas inlet, 18. Liquid inlet, 19. Discharge outlet, 2. Adjustment mechanism, 21. Liquid supply cylinder, 211. Annular slit, 22. Motor, 23. Rotating shaft, 231. Outer arc rack, 232. Inner arc rack, 24. Slide groove, 241. Sliding block, 25. Baffle, 251. Limiting rod, 26. Annular rotating plate, 261. Guide block, 262. Guide groove, 263. Limiting groove, 264. Gear ring, 27. Lifting ring, 271. Annular groove, 272. Lifting groove, 273. Lifting block, 274. Spring, 28. Inclined block. Detailed Implementation

[0025] To make the technical means, creative features, objectives and effects of this invention easier to understand, the invention will be further described below in conjunction with specific embodiments.

[0026] Reference Figure 1-7 As shown, a device for improving the deep sulfonation of active ingredients includes a tank 1 and an adjustment mechanism 2. A top plate 11, a partition plate 12, and a bottom plate 13 are connected sequentially from top to bottom on the inner wall of the tank 1. Multiple reaction tubes 14 are connected between the partition plate 12 and the bottom plate 13 in a ring array. The upper end of each reaction tube 14 passes through the partition plate 12 and is coaxially connected to a liquid supply cylinder 21. The lower end of each reaction tube 14 passes through the bottom plate 13. The upper end of the liquid supply cylinder 21 passes through the top plate 11. Each liquid supply cylinder 21 has an annular slit 211. The adjustment mechanism 2 is installed inside the tank 1 and is used to adjust the intensity of the sulfonation reaction on the inner wall of the reaction tubes 14.

[0027] In this embodiment, the adjusting mechanism 2 includes a motor 22 and multiple annular rotating plates 26. The motor 22 is mounted on the top outer wall of the tank 1. The motor 22 is a low-speed motor. A rotating shaft 23 is rotatably connected to the center of the top of the tank 1. The output shaft of the motor 22 is coaxially connected to the rotating shaft 23. The lower end of the rotating shaft 23 is connected to an outer arc-shaped rack 231 and an inner arc-shaped rack 232 respectively via two connecting rods. Four sliding grooves 24 are formed around each liquid supply cylinder 21 on the top plate 11. A slider 241 is slidably connected in each of the sliding grooves 24. A 90° fan-shaped baffle 25 is connected to the top of the slider 241. Four guide blocks 261 are connected around each liquid supply cylinder 21. Each annular rotating plate 26 has four guide grooves 262. The four guide blocks 261 are slidably connected to the four guide grooves 262 on the annular rotating plate 26, allowing the annular rotating plate 26 to rotate slightly. The annular rotating plate 26 is coaxially arranged with the liquid supply cylinder 21. Each baffle 25 is connected to a limit rod 251. Each annular rotating plate 26 has four arc-shaped limit grooves 263. The four limit rods 251 are slidably connected to the four limit grooves 263 on the annular rotating plate 26. A toothed ring 264 is coaxially connected to the outer ring surface of each annular rotating plate 26.

[0028] In this embodiment, each liquid supply cylinder 21 has an annular groove 271 communicating with an annular slit 211. A lifting ring 27 is slidably connected in the annular groove 271. The top of the liquid supply cylinder 21 has two symmetrically distributed lifting grooves 272 communicating with the annular groove 271. The upper part of the lifting ring 27 is connected to two symmetrical lifting blocks 273. The two lifting blocks 273 are slidably connected to the two lifting grooves 272 respectively. The top of the lifting ring 27 is connected to multiple springs 274. The upper end of each spring 274 is connected to the top wall of the annular groove 271. The bottom of the two baffles 25 near the lifting grooves 272 is connected to inclined blocks 28. The springs 274 are always in a stretched state.

[0029] In this embodiment, the outer arc-shaped rack 231 and the inner arc-shaped rack 232 have the same number of teeth, and both mesh with the gear ring 264 when they rotate. Since the outer arc-shaped rack 231 and the inner arc-shaped rack 232 have the same number of teeth, their meshing causes the annular rotating plate 26 to rotate at the same angle. Because the angle between the outer arc-shaped rack 231 and the inner arc-shaped rack 232 on the rotating shaft 23 is adjustable, this design allows for adjustment of the opening and closing cycle of the baffle 25 above the liquid supply cylinder 21. Figure 3 As shown, if the rotating shaft 23 rotates clockwise, when the angle between the outer arc-shaped rack 231 and the inner arc-shaped rack 232 on the rotating shaft 23 is small (less than 90°), then the baffle 25 above each liquid supply cylinder 21 will close for a shorter time and open for a longer time. In this case, the sulfonation reaction time of the normal amount in each reaction tube 14 will be longer. When the angle between the outer arc-shaped rack 231 and the inner arc-shaped rack 232 on the rotating shaft 23 is large (close to 180°), then the closing time of the baffle 25 above each liquid supply cylinder 21 will be equal to the opening time. In this case, the sulfonation reaction time of the normal amount in each reaction tube 14 will be about the same as the sulfonation reaction time of the low amount, allowing more time for the reaction tube to cool down.

[0030] In this embodiment, the top of the tank 1 is provided with an air inlet 17, the bottom of the tank 1 is provided with a discharge outlet 19, the bottom outer wall of the tank 1 is connected with multiple support legs 16, the inner wall of the tank 1 is connected with a liquid collection hopper 15 located directly below the bottom plate 13, and the outer wall of the tank 1 is provided with an air outlet 151 located below the liquid collection hopper 15.

[0031] In this embodiment, an inlet 18 is provided on the outer wall of the tank 1 between the top plate 11 and the partition plate 12, and an inlet 141 and an outlet 142 are provided on the outer wall of the tank 1 between the partition plate 12 and the bottom plate 13.

[0032] In this embodiment, a method for using an apparatus to improve the depth of sulfonation of active ingredients is also proposed, comprising the following steps:

[0033] S1. Prepare a sulfur trioxide-air mixture containing 4% to 7% sulfur trioxide as a sulfonating agent, and prepare a dodecylbenzene solution;

[0034] S2. The sulfonating agent is introduced into the tank 1 through the air inlet 17, and the dodecylbenzene solution is injected into the tank 1 through the liquid inlet 18. The dodecylbenzene solution forms a liquid film in the reaction tube 14 and reacts with the introduced sulfonating agent.

[0035] S3. During the production of dodecylbenzenesulfonic acid in the device, the regulating mechanism 2 is activated to periodically adjust the sulfonation reaction intensity in each reaction tube 14 to increase the content of active ingredients.

[0036] The working process and principle of this invention are as follows:

[0037] During use, sulfonating agent is introduced into the top of tank 1 through air inlet 17, and dodecylbenzene solution is injected into the space between the top plate 11 and the partition plate 12 of tank 1 through liquid inlet 18. The dodecylbenzene solution flows into the reaction tube 14 through the annular slit 211 on the liquid supply cylinder 21, forming a liquid film on the inner wall of the reaction tube 14. As gas is continuously injected into the top of tank 1, the sulfonating agent will flow downward. When passing through the reaction tube 14, sulfur trioxide gas reacts with the liquid film to generate dodecylbenzene sulfonic acid. The generated dodecylbenzene sulfonic acid flows down and is collected through the discharge port 19, while the sulfonating agent tail gas is discharged through the air outlet 151. Cooling water enters the space between the partition plate 12 and the bottom plate 13 of tank 1 through the water inlet 141 to absorb heat and cool the reaction tube 14.

[0038] During the production process, the motor 22 starts and drives the rotating shaft 23 to work. Through the meshing of the outer arc-shaped rack 231 and the inner arc-shaped rack 232 with the gear ring 264, the annular rotating plates 26 at different positions are driven to rotate. Assuming the rotating shaft 23 rotates clockwise, when the inner arc-shaped rack 232 meshes with and drives the annular rotating plate 26, it will drive the four baffles 25 to slide along the direction of the sliding groove 24 through the rotating limiting groove 263. This causes the originally open and dispersed four baffles 25 to slide and converge, reducing the amount of sulfonating agent gas entering at the opening of the liquid supply cylinder 21. At the same time, during the sliding process of the baffles 25, the lifting block 273 will be squeezed by the inclined block 28, causing the lifting ring 27 to descend, reducing the flow rate of dodecylbenzene solution in the annular slit 211. By simultaneously reducing the amount of sulfonating agent gas entering and the flow rate of dodecylbenzene solution, the amount of sulfonating agent gas entering the reaction tube 14 is reduced. The sulfonation reaction intensity is reduced, and the heat generated during the reaction is minimized. During this period, cooling water is used to lower the temperature of the reaction tube 14, preventing the tube wall temperature from exceeding the process threshold due to continuous high-intensity sulfonation reaction and inducing the formation of by-products. When the outer arc-shaped rack 231 engages and drives the annular rotating plate 26, the four polymer baffles 25 will slide outward and open, no longer blocking the opening of the liquid supply cylinder 21, restoring the original sulfonating agent supply. At the same time, after the inclined block 28 leaves, the lifting ring 27 slides upward under the action of the spring 274, restoring the original liquid flow rate of the annular slit 211, so that the reaction tube 14 returns to its original sulfonation reaction intensity. By periodically adjusting the sulfonation reaction intensity in the reaction tube 14, the temperature in the reaction tube 14 is always kept within a suitable threshold, avoiding the formation of by-products, thereby increasing the content of active ingredients.

[0039] As is known from common technical knowledge, this invention can be implemented through other embodiments that do not depart from its spirit or essential characteristics. Therefore, the disclosed embodiments described above are merely illustrative in all respects and are not the only ones. All modifications within the scope of this invention or its equivalents are included in this invention.

Claims

1. An apparatus for improving the deep sulfonation of active ingredients, characterized in that: The tank includes a tank body (1) and an adjusting mechanism (2). The inner wall of the tank body (1) is connected from top to bottom to a top plate (11), a partition plate (12), and a bottom plate (13). Multiple reaction tubes (14) are connected between the partition plate (12) and the bottom plate (13) in a ring array. The upper end of each reaction tube (14) passes through the partition plate (12) and is coaxially connected to a liquid supply cylinder (21). The lower end of each reaction tube (14) passes through the bottom plate (13). The upper end of the liquid supply cylinder (21) passes through the top plate (11). Each liquid supply cylinder (21) is provided with an annular slit (211). The adjusting mechanism (2) is installed inside the tank body (1) and is used to adjust the sulfonation reaction intensity on the inner wall of the reaction tubes (14).

2. The apparatus for improving the depth of sulfonation of active ingredients according to claim 1, characterized in that: The adjusting mechanism (2) includes a motor (22) and multiple annular rotating plates (26). The motor (22) is mounted on the top outer wall of the tank (1). A rotating shaft (23) is rotatably connected to the center of the top of the tank (1). The output shaft of the motor (22) is coaxially connected to the rotating shaft (23). The lower end of the rotating shaft (23) is connected to an outer arc-shaped rack (231) and an inner arc-shaped rack (232) respectively through two connecting rods. Four sliding grooves (24) are provided on the top plate (11) around each supply cylinder (21). A slider (241) is slidably connected in each of the sliding grooves (24). A 90° fan-shaped baffle (25) is connected to the top of the slider (241). The liquid cylinder (21) is connected to four guide blocks (261). Each of the annular rotating plates (26) has four guide grooves (262). The four guide blocks (261) are slidably connected to the four guide grooves (262) on the annular rotating plate (26), so that the annular rotating plate (26) rotates slightly. The annular rotating plate (26) is coaxially arranged with the liquid supply cylinder (21). Each baffle (25) is connected to a limit rod (251). Each of the annular rotating plates (26) has four arc-shaped limit grooves (263). The four limit rods (251) are slidably connected to the four limit grooves (263) on the annular rotating plate (26). The outer ring surface of each annular rotating plate (26) is coaxially connected to a toothed ring (264).

3. The apparatus for improving the depth of sulfonation of active ingredients according to claim 2, characterized in that: Each of the liquid supply cylinders (21) has an annular groove (271) communicating with an annular slit (211). A lifting ring (27) is slidably connected in the annular groove (271). Two symmetrically distributed lifting grooves (272) are opened at the top of the liquid supply cylinder (21) communicating with the annular groove (271). Two symmetrical lifting blocks (273) are connected to the top of the lifting ring (27). The two lifting blocks (273) are slidably connected to the two lifting grooves (272) respectively. Multiple springs (274) are connected to the top of the lifting ring (27). The upper end of each spring (274) is connected to the top wall of the annular groove (271). Two baffles (25) near the lifting grooves (272) are connected to the bottom of the baffles (28).

4. The apparatus for improving the depth of sulfonation of active ingredients according to claim 2, characterized in that: The outer arc-shaped rack (231) and the inner arc-shaped rack (232) have the same number of teeth, and both the outer arc-shaped rack (231) and the inner arc-shaped rack (232) mesh with the gear ring (264) when they rotate. The angle between the outer arc-shaped rack (231) and the inner arc-shaped rack (232) on the rotating shaft (23) can be adjusted.

5. The apparatus for improving the depth of sulfonation of active ingredients according to claim 1, characterized in that: The tank (1) has an air inlet (17) at the top and a discharge port (19) at the bottom. The tank (1) has multiple support legs (16) connected to the bottom outer wall. The tank (1) has a liquid collection hopper (15) connected to the inner wall of the tank (1) and located directly below the bottom plate (13). The tank (1) has an air outlet (151) located on the outer wall of the tank (1) and below the liquid collection hopper (15).

6. The apparatus for improving the depth of sulfonation of active ingredients according to claim 1, characterized in that: The tank (1) has an inlet (18) on its outer wall between the top plate (11) and the partition plate (12), and a water inlet (141) and a water outlet (142) on its outer wall between the partition plate (12) and the bottom plate (13).

7. A method of using the apparatus for enhancing the depth of sulfonation of active ingredients according to any one of claims 1-6, characterized in that: Includes the following steps: S1. Prepare a sulfur trioxide-air mixture containing 4% to 7% sulfur trioxide as a sulfonating agent, and prepare a dodecylbenzene solution; S2. The sulfonating agent is introduced into the tank (1) through the air inlet (17), and the dodecylbenzene solution is injected into the tank (1) through the liquid inlet (18). The dodecylbenzene solution forms a liquid film in the reaction tube (14) and reacts with the introduced sulfonating agent. S3. During the production of dodecylbenzenesulfonic acid in the device, the regulating mechanism (2) is turned on to periodically adjust the sulfonation reaction intensity in each reaction tube (14) to increase the content of active ingredients.

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