High-purity sulfamic acid production equipment and sulfamic acid synthesis process

By using an annular partition and jacket heating unit in the sulfamic acid production equipment and combining the circulating flow method of the stirring unit, the problem of uneven temperature distribution in the sulfonation kettle is solved, the product purity and yield are improved, and the purification cost is reduced.

CN119909635AInactive Publication Date: 2025-05-02LAIZHOU GUANGCHENG CHEM CO LTD

Patent Information

Application Number
CN202510401542.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-01
Publication Date
2025-05-02
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

In the prior art, the temperature distribution in the sulfonation kettle is uneven, resulting in the decomposition of sulfamic acid in high temperature regions, reducing yields, and producing by-products, reducing product purity and increasing purification costs.

Method used

A high-purity sulfamic acid production equipment is designed, using an annular partition and a jacket heating unit. The inner cavity of the sulfonation kettle is divided into the inner and outer sides through the annular partition, and a jacket heating unit is set up in the outer shell. Combined with the circulating flow method of the stirring unit, it ensures uniform temperature distribution and uniform heat transfer.

Benefits of technology

It effectively avoids the decomposition of sulfamic acid and the generation of by-products caused by uneven temperature, improves the purity and yield of the product, and reduces the difficulty and cost of subsequent purification.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention belongs to the technical field of preparation of sulfamic acid, and particularly relates to high-purity sulfamic acid production equipment and a sulfamic acid synthesis process. Comprising a sulfonation kettle, a feeding pipe is fixedly connected to one side of the sulfonation kettle, an exhaust pipe is fixedly connected to the other side of the sulfonation kettle, a discharging pipe is fixedly connected to the bottom end of the sulfonation kettle, a motor is fixedly installed on one side of the top of the sulfonation kettle, and a first rotating shaft is rotationally connected to the center of the top of the sulfonation kettle; the first rotating shaft is in transmission connection with the output end of the motor through a belt, an annular partition plate is arranged in an inner cavity of the sulfonation kettle, and a plurality of supporting legs are arranged at the bottom end of the annular partition plate. The space in the sulfonation kettle can be divided into the inner side and the outer side through the annular heat conduction plate arranged in the sulfonation kettle, and the jacket heating unit arranged in the sulfonation kettle shell is matched, so that it is effectively ensured that heat is evenly transmitted to a reaction medium, and the local overheating or supercooling phenomenon is reduced.
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Description

Technical Field

[0001] The invention belongs to the technical field of aminosulfonic acid preparation, in particular to a high-purity aminosulfonic acid production device and an aminosulfonic acid synthesis process. Background Art

[0002] Aminosulfonic acid is an inorganic solid acid formed by replacing the hydroxyl group of sulfuric acid with an amino group. It has the chemical formula NH2SO3H and is generally white, odorless, rhombic flaky crystals. High-purity aminosulfonic acid refers to aminosulfonic acid products with higher purity specifications, and its purity usually reaches 99.5% or above. As a high-quality form of aminosulfonic acid, it has higher purity and more stable chemical properties. Therefore, it is widely used in medicine, food, pesticides, electrochemistry and other fields. There are usually two ways to prepare high-purity aminosulfonic acid, one is the liquid phase method and the other is the gas phase method. In actual production, since the liquid phase method has lower cost and simpler operation process than the gas phase method, most manufacturers use the liquid phase method to prepare high-purity aminosulfonic acid. When using the liquid phase method to prepare high-purity aminosulfonic acid, a sulfonation kettle is generally used for preparation.

[0003] In the prior art, because the internal space of the sulfonation kettle is relatively large, the heating component on the sulfonation kettle cannot ensure uniform temperature distribution in the sulfonation kettle during the preparation of aminosulfonic acid, which makes the temperature near the heating component in the sulfonation kettle higher, while the temperature far from the heating component is lower, which causes the higher temperature area to cause the generated aminosulfonic acid to decompose into raw materials again, thereby reducing the yield of the product. Secondly, the uneven temperature distribution will also lead to incomplete reaction or the generation of by-products, which will reduce the purity of the product and increase the difficulty and cost of subsequent purification.

[0004] To this end, the present invention provides a high-purity aminosulfonic acid production device and an aminosulfonic acid synthesis process. Summary of the invention

[0005] In order to make up for the deficiencies of the prior art and solve the problem in the prior art that, because the internal space of the sulfonating kettle is large, the heating component on the sulfonating kettle cannot ensure uniform temperature distribution in the sulfonating kettle during the preparation of aminosulfonic acid, which makes the temperature near the heating component in the sulfonating kettle higher, while the temperature far away from the heating component is lower, which causes the area with higher temperature to decompose the generated aminosulfonic acid into raw materials again, thereby reducing the yield of the product. Secondly, the uneven temperature distribution will also lead to incomplete reaction or the generation of by-products, which will reduce the purity of the product and increase the difficulty and cost of subsequent purification. The present invention provides a high-purity aminosulfonic acid production equipment and an aminosulfonic acid synthesis process.

[0006] The technical solution applicable to the present invention for solving its technical problem is: a high-purity aminosulfonic acid production equipment described in the present invention comprises a sulfonation kettle, a feed pipe is fixedly connected to one side of the sulfonation kettle, an exhaust pipe is fixedly connected to the other side of the sulfonation kettle, a discharge pipe is fixedly connected to the bottom end of the sulfonation kettle, a motor is fixedly installed on one side of the top of the sulfonation kettle, a rotating shaft 1 is rotatably connected to the center of the top of the sulfonation kettle, the rotating shaft 1 is connected to the output end of the motor through a belt drive, an annular partition is provided in the inner cavity of the sulfonation kettle, a plurality of legs are provided at the bottom end of the annular partition, the legs of the annular partition are fixedly connected to the bottom of the inner cavity of the sulfonation kettle, a jacket heating unit is provided in the outer shell of the sulfonation kettle, a stirring unit is provided in the inner cavity of the sulfonation kettle, and the rotating shaft 1 is adapted to the stirring unit.

[0007] Preferably, the jacket heating unit comprises a second water inlet pipe, an annular water inlet plate, a heat conduction cavity and a first water outlet pipe; the bottom end of the sulfonation kettle is fixedly connected to an annular water inlet plate; the bottom end of the annular water inlet plate is fixedly connected to a second water inlet pipe; one end of the second water inlet pipe is externally connected to a water supply device; the other end of the second water inlet pipe is connected to an inner cavity of the annular water inlet plate; an annular cavity one, a heat conduction cavity and annular cavity two are arranged in sequence from bottom to top in the outer shell of the sulfonation kettle; there are multiple heat conduction cavities, all of which are serpentine; the multiple heat conduction cavities are evenly distributed between the first annular cavity and the second annular cavity, and are connected to each other; the inner cavity of the annular water inlet plate is connected to the first annular cavity; a first water outlet pipe is fixedly connected to the side wall of the sulfonation kettle; the first water outlet pipe is connected to the second annular cavity.

[0008] Preferably, a heat conducting pipe is embedded in the annular partition, one end of the heat conducting pipe is connected to the water inlet pipe three, the end of the water inlet pipe three away from the heat conducting pipe passes through the support leg of the annular partition and extends to the outside of the sulfonation kettle to be connected to the water inlet pipe two, the other end of the heat conducting pipe is connected to the water outlet pipe two, the end of the water outlet pipe two away from the heat conducting pipe passes through the support leg of the annular partition and extends to the outside of the sulfonation kettle, and the heat conducting pipes are distributed in a serpentine shape.

[0009] Preferably, the stirring unit includes an auger piece 1 and an auger piece 2, the bottom end of the rotating shaft 1 extends to the inner side of the annular partition and is fixedly connected to the auger piece 1, a mounting ring is fixedly connected to the inner cavity wall of the sulfonation kettle, a gear ring is fixedly connected to the bottom of the mounting ring, a gear 1 is fixedly connected to the rotating shaft 1, a plurality of gear 2s are meshingly connected to the outer side of the gear 1, a plurality of gear 2s are meshingly connected to the gear ring, a plurality of gear 2s are fixedly connected to the rotating shaft 2, a sealing rotating ring is rotatably connected to the bottom of the mounting ring, a plurality of rotating shafts 2 are fixedly connected to the sealing rotating ring, and the bottom end of the rotating shaft 2 extends to the outer side of the annular partition and is fixedly connected to the auger piece 2.

[0010] Preferably, the top end of the rotating shaft one is rotatably connected to a water inlet pipe one, and the end of the water inlet pipe one away from the rotating shaft one is externally connected to a water supply device, a water inlet chamber one is opened at the top of the rotating shaft one, and the water inlet pipe one is connected to the water inlet chamber one, and a water outlet chamber one is opened at the bottom of the rotating shaft one, and the bottom end of the rotating shaft one is rotatably connected to a water outlet pipe three, and the end of the water outlet pipe three away from the rotating shaft one passes through the discharge pipe and extends to the outside of the sulfonation kettle, the water outlet pipe three is L-shaped and fixedly connected to the discharge pipe, the water outlet pipe two is connected to the water outlet pipe three, the bottom of the water inlet chamber one is connected to the top of the inner cavity of the auger piece one, and the top of the water outlet chamber one is connected to the bottom of the inner cavity of the auger piece one.

[0011] Preferably, an annular fixed tube 1 is fixedly connected to the top of the inner cavity of the sulfonation kettle, the rotating shaft 1 is sealingly and rotatably connected to the annular fixed tube 1, through grooves are evenly opened on the rotating shaft 1, and the through grooves are connected to the water inlet cavity 1 and the annular fixed tube 1, a plurality of connecting tubes 1 are connected between the inner cavity of the mounting ring and the annular fixed tube 1, a water inlet cavity 2 is opened at the top of the rotating shaft 2, through holes are evenly opened on the sealing rotating ring, and the through holes are connected to the water inlet cavity 2 in a one-to-one correspondence, a water outlet cavity 2 is opened at the bottom of the rotating shaft 2, an annular fixed tube 2 is fixedly connected to the bottom of the outer wall of the annular partition, a sealing ring is rotatably connected to the annular fixed tube 2, a connecting tube 2 is fixedly connected to the bottom end of the rotating shaft 2, one end of the connecting tube 2 is connected to the water outlet cavity 2, one end of the plurality of connecting tubes 2 away from the rotating shaft 2 is fixedly connected to the sealing ring, the connecting tube 2 is connected to the annular fixed tube 2, and a plurality of connecting tubes 3 are connected between the annular fixed tube 2 and the water outlet pipe 3.

[0012] Preferably, a spoiler is evenly fixed on the inner wall of the heat conduction cavity, the spoiler is in an I-shape, and a spoiler hole is formed on the spoiler.

[0013] Preferably, the spoiler hole is conical, and a spiral groove is provided on the inner wall of the spoiler hole.

[0014] Preferably, an air filter is fixedly connected to one end of the exhaust pipe away from the sulfonation kettle.

[0015] A high-purity aminosulfonic acid synthesis process, which is applicable to the high-purity aminosulfonic acid production equipment described above, comprises the following steps: S1: The staff first adds oleum into the sulfonation kettle through the feed pipe, starts the motor, and drives the rotating shaft to rotate through the motor and the belt, so that the stirring unit starts stirring; S2: When the temperature in the sulfonation kettle drops to 20-40°C, add the mixed sulfuric acid and urea into the sulfonation kettle through the feed pipe, stir for 8 hours, and then gradually raise the temperature to 70-90°C to evaporate sulfur trioxide; S3: After cooling and crystallization, crude aminosulfonic acid is obtained, and finally, high-purity aminosulfonic acid is obtained by recrystallization with water and dehydration and drying.

[0016] The beneficial effects of the present invention are as follows: 1. The high-purity aminosulfonic acid production equipment and aminosulfonic acid synthesis process described in the present invention can divide the space in the sulfonation kettle into inner and outer sides by means of an annular heat conduction plate arranged in the sulfonation kettle, and cooperate with the jacket heating unit arranged in the outer shell of the sulfonation kettle to effectively ensure that heat is evenly transferred to the reaction medium, reduce local overheating or overcooling, and design the heat conduction cavity into a snake shape, so that hot water can continuously change direction when flowing in the heat conduction cavity, thereby enhancing the degree of turbulence and improving the heat transfer efficiency.

[0017] 2. The high-purity aminosulfonic acid production equipment and aminosulfonic acid synthesis process described in the present invention use a stirring unit to allow the materials in the sulfonation kettle to form a circulating flow from the center to the outside and then back to the center, which not only ensures the uniform mixing of the materials in the kettle body, but also helps to evenly distribute the temperature. In addition, through the cooperation between the second gear and the gear ring, the auger piece 2 rotates while also revolving, further improving the stirring effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] The present invention will be further described below in conjunction with the accompanying drawings.

[0019] Figure 1 It is a stereogram of the present invention as a whole; Figure 2 is a cross-sectional view of a sulfonation kettle of the present invention; Figure 3 yes Figure 2 A partial enlarged view of the middle part; Figure 4 yes Figure 2 A partial enlarged view of point B in the middle; Figure 5 yes Figure 2 A partial enlarged view of point C in the middle; Figure 6 is an exploded view of the mounting ring of the present invention; Figure 7 It is an exploded view of the annular partition of the present invention; Figure 8 is a cross-sectional view of the heat conduction cavity of the present invention; Fig. 9 yes Figure 8 A partial enlarged view of point D in the middle; Fig.10 Schematic diagram of the spoiler of the present invention.

[0020] In the figure: 1, sulfonation kettle; 2, feed pipe; 3, discharge pipe; 4, exhaust pipe; 5, motor; 6, belt; 7, shaft 1; 8, water inlet pipe 1; 9, gear 1; 10, gear 2; 11, auger piece 1; 12, shaft 2; 13, auger piece 2; 14, mounting ring; 15, gear ring; 16, annular fixed pipe 1; 17, connecting pipe 1; 18, sealing rotating ring; 19, water inlet chamber 1; 20, through groove; 21, water inlet pipe 2; 22, annular water inlet plate ; 23. Annular cavity one; 24. Heat transfer cavity; 25. Annular cavity two; 26. Water outlet pipe one; 27. Water inlet pipe three; 28. Annular partition; 29. ​​Heat transfer pipe; 30. Water outlet pipe two; 31. Through hole; 32. Water outlet cavity one; 33. Water outlet pipe three; 34. Water inlet cavity two; 35. Water outlet cavity two; 36. Connecting pipe two; 37. Annular fixed pipe two; 38. Connecting pipe three; 39. Spoiler; 40. Spoiler hole; 41. Sealing ring; 42. Air filter. DETAILED DESCRIPTION

[0021] In order to make the technical means, creative features, objectives and effects achieved by the present invention easy to understand, the present invention is further explained below in conjunction with specific implementation methods.

[0022] like Figure 1-Figure 10As shown, a high-purity aminosulfonic acid production equipment described in an embodiment of the present invention includes a sulfonation kettle 1, a feed pipe 2 is fixedly connected to one side of the sulfonation kettle 1, an exhaust pipe 4 is fixedly connected to the other side of the sulfonation kettle 1, a discharge pipe 3 is fixedly connected to the bottom end of the sulfonation kettle 1, a motor 5 is fixedly installed on one side of the top of the sulfonation kettle 1, a rotating shaft 7 is rotatably connected to the center of the top of the sulfonation kettle 1, and the rotating shaft 7 is connected to the output end of the motor 5 through a belt 6. An annular partition 28 is provided in the inner cavity of the sulfonation kettle 1, and a plurality of support plates are provided at the bottom end of the annular partition 28. The legs of the annular partition 28 are fixedly connected to the bottom of the inner cavity of the sulfonating kettle 1. The outer shell of the sulfonating kettle 1 is provided with a jacket heating unit, and the inner cavity of the sulfonating kettle 1 is provided with a stirring unit. The rotating shaft 7 is adapted to the stirring unit. When working, the staff first adds fuming sulfuric acid into the sulfonating kettle 1 through the feeding pipe 2, starts the motor 5, and drives the rotating shaft 7 to rotate through the motor 5 and the belt 6, so that the stirring unit starts the stirring operation. When the temperature drops to 20-40°C, the mixed sulfuric acid and urea are added into the sulfonating kettle 1 through the feeding pipe 2. After stirring for 8 hours, the temperature is gradually raised to 70-90° C., sulfur trioxide is evaporated, and crude aminosulfonic acid is obtained after cooling and crystallization. When the stirring unit mixes and stirs the mixture in the sulfonation kettle 1, the space in the sulfonation kettle 1 can be divided into inner and outer sides by the annular partition 28 arranged in the sulfonation kettle 1, and the jacket heating unit arranged in the outer shell of the sulfonation kettle 1 can be used to achieve uniform heating of the mixture in the sulfonation kettle 1, which effectively avoids the problem in the prior art that, because the internal space of the sulfonation kettle 1 is large, the heating component on the sulfonation kettle 1 cannot ensure uniform temperature distribution in the sulfonation kettle 1 during the preparation of aminosulfonic acid, which makes the temperature near the heating component in the sulfonation kettle 1 higher, while the temperature far away from the heating component is lower, which causes the higher temperature area to cause the generated aminosulfonic acid to be re-decomposed into raw materials, thereby reducing the yield of the product. Secondly, the uneven temperature distribution will also lead to incomplete reaction or the generation of by-products, which will reduce the purity of the product and increase the difficulty and cost of subsequent purification.

[0023] The jacket heating unit comprises a water inlet pipe 21, an annular water inlet plate 22, a heat conduction cavity 24 and a water outlet pipe 1 26. The bottom end of the sulfonation kettle 1 is fixedly connected with an annular water inlet plate 22, and the bottom end of the annular water inlet plate 22 is fixedly connected with a water inlet pipe 21. One end of the water inlet pipe 21 is externally connected to a water supply device, and the other end of the water inlet pipe 21 is connected to the inner cavity of the annular water inlet plate 22. The outer shell of the sulfonation kettle 1 is provided with an annular cavity 1 23, a heat conduction cavity 24 and an annular cavity 25 from bottom to top. There are multiple heat conduction cavities 24, and they are all serpentine. The multiple heat conduction cavities 24 are evenly distributed between the annular cavity 1 23 and the annular cavity 25, and are connected to each other. The inner cavity of the annular water inlet plate 22 is connected to the annular cavity 1 23. The sulfonation kettle 1 A water outlet pipe 26 is fixedly connected to the side wall, and the water outlet pipe 26 is connected to the annular cavity 25; when working, hot water can be continuously sent into the annular water inlet plate 22 through the water inlet pipe 21, and the hot water then enters into multiple heat transfer cavities 24 through the annular cavity 23 from the annular water inlet plate 22. Finally, the hot water is collected from the heat transfer cavity 24 to the annular cavity 25 and discharged from the water outlet pipe 26. This jacket heating method can effectively ensure that heat is evenly transferred to the reaction medium and reduce local overheating or supercooling. At the same time, by designing the heat transfer cavity 24 to be serpentine, the hot water can continuously change direction when flowing in the heat transfer cavity 24, thereby enhancing the degree of turbulence and improving the heat transfer efficiency.

[0024] A heat conducting pipe 29 is embedded in the annular partition 28, one end of the heat conducting pipe 29 is connected to the water inlet pipe 3 27, the end of the water inlet pipe 3 27 away from the heat conducting pipe 29 passes through the foot of the annular partition 28 and extends to the outside of the sulfonation kettle 1 and is connected to the water inlet pipe 21, the other end of the heat conducting pipe 29 is connected to the water outlet pipe 2 30, the end of the water outlet pipe 2 30 away from the heat conducting pipe 29 passes through the foot of the annular partition 28 and extends to the outside of the sulfonation kettle 1, and the heat conducting pipe 29 is distributed in a serpentine shape; when working, the heat conducting pipe 29 is connected to the water outlet pipe 2 30 through the annular partition 28. The inner cavity of the sulfonation kettle 1 is divided into two spaces, and a heat conducting pipe 29 is embedded in the annular partition 28, so that hot water can flow out from the water outlet pipe 2 30 along the heat conducting pipe 29 after entering from the water inlet pipe 3 27, and so on and so forth, so that the annular partition 28 can dissipate heat to the inner cavity of the sulfonation kettle 1 on both sides, thereby avoiding the inability to effectively heat the central part of the inner cavity of the sulfonation kettle 1 by heating close to the jacket, thereby causing a temperature gradient difference between the inner cavity center and the outer side of the sulfonation kettle 1.

[0025] The stirring unit includes an auger piece 11 and an auger piece 2 13. The bottom end of the rotating shaft 7 extends to the inner side of the annular partition 28 and is fixedly connected to the auger piece 11. A mounting ring 14 is fixedly connected to the inner wall of the sulfonation kettle 1. A gear ring 15 is fixedly connected to the bottom of the mounting ring 14. A gear 9 is fixedly connected to the rotating shaft 7. A plurality of gears 2 10 are meshedly connected to the outer side of the gear 9. The plurality of gears 2 10 are meshedly connected to the gear ring 15. A rotating shaft 2 12 is fixedly connected to the plurality of gears 2 10. A sealing rotating ring 18 is rotatably connected to the bottom of the mounting ring 14. The plurality of rotating shafts 2 12 are fixedly connected to the sealing rotating ring 18. The bottom end of the rotating shaft 2 12 extends to the outer side of the annular partition 28 and is fixedly connected to the auger piece 11. When working, through the cooperation between gear 19 and gear 210, the auger piece 11 on the rotating shaft 7 rotates forward, and drives the material in the center of the inner cavity of the sulfonating kettle 1 to flow upward, and the auger piece 13 on the rotating shaft 12 rotates reversely, driving the material outside the inner cavity of the sulfonating kettle 1 to flow downward, and so on, so that the material in the sulfonating kettle 1 forms a circulating flow from the center to the outside and then back to the center, which not only ensures the uniform mixing of the material in the kettle body, but also contributes to the uniform distribution of temperature. In addition, through the cooperation between gear 210 and the gear ring 15, the auger piece 213 rotates on itself and revolves at the same time, further improving the stirring effect.

[0026] The top of the rotating shaft 7 is rotatably connected with a water inlet pipe 8, and the end of the water inlet pipe 8 away from the rotating shaft 7 is connected to an external water supply device. A water inlet cavity 19 is provided at the top of the rotating shaft 7, and the water inlet pipe 8 is connected to the water inlet cavity 19. A water outlet cavity 32 is provided at the bottom of the rotating shaft 7, and a water outlet pipe 33 is rotatably connected to the bottom end of the rotating shaft 7. The end of the water outlet pipe 33 away from the rotating shaft 7 passes through the discharge pipe 3 and extends to the outside of the sulfonation kettle 1. The water outlet pipe 33 is L-shaped and fixedly connected to the discharge pipe 3. The water outlet pipe 2 30 is connected to the water outlet pipe 33. The bottom of the water inlet cavity 19 is connected to the top of the inner cavity of the auger piece 11. The water outlet The top of the cavity 32 is connected with the bottom of the inner cavity of the auger piece 11; when working, hot water is sent into the water inlet cavity 19 through the water inlet pipe 8, so that the hot water enters the inner cavity of the auger piece 11 through the bottom of the water inlet cavity 19, and flows downward along the auger piece 11 until it flows out from the water outlet cavity 32, and then enters the water outlet pipe 33, and finally, is discharged from the sulfonation kettle 1 through the water outlet pipe 33. By flowing hot water in the auger piece 11, not only can the temperature at the center of the inner cavity of the sulfonation kettle 1 be supplemented, but also a multi-stage jacket heating design is further realized, so that the temperature in the sulfonation kettle 1 can be evenly distributed.

[0027] The top of the inner cavity of the sulfonation kettle 1 is fixedly connected with an annular fixed pipe 16, and the rotating shaft 17 is sealed and rotatably connected with the annular fixed pipe 16. The rotating shaft 17 is evenly provided with through grooves 20, and the through grooves 20 are connected with the water inlet cavity 19 and the annular fixed pipe 16. A plurality of connecting pipes 17 are connected between the inner cavity of the mounting ring 14 and the annular fixed pipe 16. The top of the rotating shaft 12 is provided with a water inlet cavity 24, and the sealing rotating ring 18 is evenly provided with through holes 31, and the through holes 31 are connected with the water inlet cavity 24. Correspondingly connected, a water outlet cavity 35 is provided at the bottom of the second rotating shaft 12, a second annular fixed pipe 37 is fixedly connected to the bottom of the outer wall of the annular partition 28, a sealing ring 41 is rotatably connected to the second annular fixed pipe 37, a connecting pipe 36 is fixedly connected to the bottom end of the second rotating shaft 12, one end of the connecting pipe 36 is connected to the second water outlet cavity 35, and one end of the plurality of connecting pipes 36 away from the second rotating shaft 12 is fixedly connected to the sealing ring 41, the connecting pipe 36 is connected to the second annular fixed pipe 37, and the second annular fixed pipe 37 is connected to the water outlet cavity 35. There are multiple connecting pipes 38 connected between the three 33; when working, after the hot water enters the water inlet chamber 19, part of the hot water enters the auger piece 11, and the other part of the hot water enters the annular fixed pipe 16 through the through groove 20, and then enters the water inlet chamber 2 34 through the connecting pipe 17 and the mounting ring 14, and enters the inner cavity of the auger piece 2 13 from the bottom of the water inlet chamber 2 34, flows downward along the auger piece 2 13 until it flows out from the water outlet chamber 2 35, enters the annular fixed pipe 2 37 after passing through the connecting pipe 2 36, and is then sent into the water outlet pipe 3 33 through the connecting pipe 3 38, and finally discharged from the sulfonation kettle 1 through the water outlet pipe 3 33. By flowing hot water in the auger piece 2 13, not only can the temperature of the area between the outer shell of the sulfonation kettle 1 and the annular partition 28 be supplemented, but also the downward flow of hot water in the auger piece 11 is complementary to the upward flow of hot water in the heat conduction chamber 24 and the heat conduction pipe 29, further ensuring that the temperature in the sulfonation kettle 1 can be evenly distributed.

[0028] The inner wall of the heat conduction cavity 24 is evenly fixed with a spoiler 39, which is in an I-shape and has a spoiler hole 40. During operation, by arranging the spoiler 39 in the heat conduction cavity 24 and providing the spoiler hole 40 on the I-shaped spoiler 39, not only the passing rate of hot water is guaranteed, but also the flow velocity of hot water is accelerated when passing through the spoiler hole 40, further enhancing the degree of turbulence, greatly improving the heat transfer efficiency, and reducing heat loss and the occurrence of temperature gradient.

[0029] The spoiler hole 40 is conical, and a spiral groove is provided on the inner wall of the spoiler hole 40; when working, by designing the spoiler hole 40 to be conical and providing the spiral groove on the inner wall, the spoiler hole 40 has an increased spoiler effect on the hot water and the turbulence is enhanced.

[0030] An air filter 42 is fixedly connected to one end of the exhaust pipe 4 away from the sulfonation reactor 1; during operation, by installing the air filter 42 on the exhaust pipe 4, sulfur trioxide discharged during the reaction process can be purified to avoid direct discharge and pollution to the atmospheric environment.

[0031] A high-purity aminosulfonic acid synthesis process, which is applicable to the above-mentioned high-purity aminosulfonic acid production equipment, comprises the following steps: S1: The staff first adds fuming sulfuric acid into the sulfonation reactor 1 through the feed pipe 2, starts the motor 5, and drives the rotating shaft 7 to rotate through the motor 5 and the belt 6, so that the stirring unit starts the stirring operation; S2: When the temperature in the sulfonation kettle 1 drops to 20-40°C, add the mixed sulfuric acid and urea into the sulfonation kettle 1 through the feed pipe 2, stir for 8 hours, and then gradually raise the temperature to 70-90°C to evaporate sulfur trioxide; S3: After cooling and crystallization, crude aminosulfonic acid is obtained, and finally, high-purity aminosulfonic acid is obtained by recrystallization with water and dehydration and drying.

[0032] Working principle: the staff first adds fuming sulfuric acid into the sulfonation kettle 1 through the feed pipe 2, starts the motor 5, and drives the rotating shaft 7 to rotate through the motor 5 and the belt 6, so that the stirring unit starts the stirring operation. When the temperature drops to 20-40°C, the mixed sulfuric acid and urea are added into the sulfonation kettle 1 through the feed pipe 2. After stirring for 8 hours, the temperature is gradually raised to 70-90°C, sulfur trioxide is evaporated, and crude aminosulfonic acid is obtained after cooling and crystallization. When the stirring unit mixes and stirs the mixture in the sulfonation kettle 1, the annular partition 28 arranged in the sulfonation kettle 1 can divide the space in the sulfonation kettle 1 into inner and outer sides, and then cooperates with the jacket heating unit arranged in the outer shell of the sulfonation kettle 1 to achieve uniform heating of the mixture in the sulfonation kettle 1. Hot water can be continuously fed into the annular water inlet plate 22 through the water inlet pipe 21, and then the hot water enters multiple heat conduction chambers 24 through the annular cavity 1 23 from the annular water inlet plate 22. Finally, the hot water is collected from the heat conduction chamber 24 to the annular cavity 25 and discharged from the water outlet pipe 1 26. This jacket heating method can effectively ensure that heat is evenly transferred to the reaction medium and reduce local overheating or supercooling. At the same time, by designing the heat conduction chamber 24 to be serpentine, the hot water can continuously change direction when flowing in the heat conduction chamber 24, thereby enhancing the turbulence and improving the heat transfer efficiency. The inner cavity of the sulfonation reactor 1 is divided into two spaces by the annular partition 28, and a heat conduction pipe 29 is embedded in the annular partition 28, so that the hot water can flow along the annular cavity 25 after entering from the water inlet pipe 3 27. The heat conducting pipe 29 then flows out from the water outlet pipe 2 30, and the flow is repeated in this way, so that the annular partition 28 can radiate heat to the inner cavity of the sulfonating kettle 1 on both sides, thereby avoiding the inability to effectively heat the central part of the inner cavity of the sulfonating kettle 1 by heating close to the jacket, which leads to a temperature gradient difference between the inner cavity center and the outer side of the sulfonating kettle 1. Through the cooperation between the gear 1 9 and the gear 2 10, the auger piece 1 11 on the rotating shaft 1 7 rotates forward and drives the material in the center of the inner cavity of the sulfonating kettle 1 to flow upward, while the auger piece 2 13 on the rotating shaft 2 12 rotates in the opposite direction, driving the material on the outer side of the inner cavity of the sulfonating kettle 1 to flow downward, and so on, so that the material in the sulfonating kettle 1 forms a circulating flow from the center to the outside and then back to the center, which not only ensures that the material is The uniform mixing in the kettle body also contributes to the uniform distribution of temperature. In addition, through the cooperation between the gear 2 10 and the gear ring 15, the auger piece 2 13 can rotate while revolving, which further improves the stirring effect. The hot water is sent into the water inlet chamber 19 through the water inlet pipe 18, so that the hot water enters the inner cavity of the auger piece 11 through the bottom of the water inlet chamber 19, and flows downward along the auger piece 11 until it flows out of the water outlet chamber 32, and then enters the water outlet pipe 3 33, and finally, it is discharged from the sulfonation kettle 1 through the water outlet pipe 3 33. By flowing hot water in the auger piece 11, not only can the temperature at the center of the inner cavity of the sulfonation kettle 1 be supplemented, but also a multi-stage jacket heating design is further realized, so that the temperature in the sulfonation kettle 1 can be evenly distributed.After the hot water enters the water inlet chamber 19, part of the hot water enters the auger piece 11, and the other part of the hot water enters the annular fixed pipe 16 through the through groove 20, and then enters the water inlet chamber 2 34 through the connecting pipe 17 and the mounting ring 14, and enters the inner cavity of the auger piece 2 13 from the bottom of the water inlet chamber 2 34, flows downward along the auger piece 2 13 until it flows out from the water outlet chamber 2 35, passes through the connecting pipe 2 36, enters the annular fixed pipe 2 37, and is then sent to the water outlet pipe 3 33 through the connecting pipe 3 38, and finally discharged from the sulfonation kettle 1 through the water outlet pipe 3 33. By flowing hot water in the auger piece 2 13, not only can the temperature of the area between the outer shell of the sulfonation kettle 1 and the annular partition 28 be supplemented, but also The downward flow of hot water in the auger blade 11 complements the upward flow of hot water in the heat conduction cavity 24 and the heat conduction pipe 29, further ensuring that the temperature in the sulfonation kettle 1 can be evenly distributed. By arranging a spoiler 39 in the heat conduction cavity 24 and opening a spoiler hole 40 on the I-shaped spoiler 39, not only the passing rate of hot water is guaranteed, but also the flow rate of hot water is accelerated when passing through the spoiler hole 40, further enhancing the turbulence, greatly improving the heat transfer efficiency, reducing heat loss and the occurrence of temperature gradients, and installing an air filter 42 on the exhaust pipe 4, the sulfur trioxide discharged during the reaction process can be purified to avoid direct discharge and pollution to the atmospheric environment.

[0033] The above-mentioned front, back, left, right, top and bottom are all based on the figures in the specification. Figure 1 As a benchmark, according to the person's observation perspective, the side of the device facing the observer is defined as the front, the left side of the observer is defined as the left, and so on.

[0034] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the scope of protection of the present invention.

[0035] The above shows and describes the basic principles, main features and advantages of the present invention. It should be understood by those skilled in the art that the present invention is not limited to the above embodiments. The above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention. The scope of protection of the present invention is defined by the attached claims and their equivalents.

Claims

1. A high-purity aminosulfonic acid production device, comprising a sulfonation kettle (1), a feed pipe (2) is fixedly connected to one side of the sulfonation kettle (1), an exhaust pipe (4) is fixedly connected to the other side of the sulfonation kettle (1), a discharge pipe (3) is fixedly connected to the bottom end of the sulfonation kettle (1), a motor (5) is fixedly installed on one side of the top of the sulfonation kettle (1), a rotating shaft (7) is rotatably connected to the center of the top of the sulfonation kettle (1), and the rotating shaft (7) is connected to the output end of the motor (5) through a belt (6), characterized in that: An annular partition (28) is provided in the inner cavity of the sulfonation kettle (1), a plurality of legs are provided at the bottom end of the annular partition (28), the legs of the annular partition (28) are fixedly connected to the bottom of the inner cavity of the sulfonation kettle (1), a jacket heating unit is provided in the outer shell of the sulfonation kettle (1), a stirring unit is provided in the inner cavity of the sulfonation kettle (1), and the rotating shaft 1 (7) is adapted to the stirring unit.

2. A high-purity aminosulfonic acid production equipment according to claim 1, characterized in that: The jacket heating unit comprises a second water inlet pipe (21), an annular water inlet plate (22), a heat conduction cavity (24) and a first water outlet pipe (26); the bottom end of the sulfonation kettle (1) is fixedly connected to the annular water inlet plate (22); the bottom end of the annular water inlet plate (22) is fixedly connected to the second water inlet pipe (21); one end of the second water inlet pipe (21) is externally connected to a water supply device; the other end of the second water inlet pipe (21) is in communication with the inner cavity of the annular water inlet plate (22); the outer shell of the sulfonation kettle (1) is provided with a heat conduction cavity (24) from bottom to top in accordance with the heat conduction cavity (24) and the heat conduction cavity (24). An annular cavity (23), a heat-conducting cavity (24) and an annular cavity (25) are provided. There are a plurality of heat-conducting cavities (24), all of which are serpentine. The plurality of heat-conducting cavities (24) are evenly distributed between the annular cavity (23) and the annular cavity (25), and are interconnected. The inner cavity of the annular water inlet plate (22) is connected to the annular cavity (23). A water outlet pipe (26) is fixedly connected to the side wall of the sulfonation kettle (1), and the water outlet pipe (26) is connected to the annular cavity (25).

3. A high-purity aminosulfonic acid production equipment according to claim 2, characterized in that: A heat conducting pipe (29) is embedded in the annular partition (28); one end of the heat conducting pipe (29) is connected to the water inlet pipe three (27); one end of the water inlet pipe three (27) away from the heat conducting pipe (29) passes through the support leg of the annular partition (28) and extends to the outside of the sulfonation kettle (1) and is connected to the water inlet pipe two (21); the other end of the heat conducting pipe (29) is connected to the water outlet pipe two (30); one end of the water outlet pipe two (30) away from the heat conducting pipe (29) passes through the support leg of the annular partition (28) and extends to the outside of the sulfonation kettle (1); the heat conducting pipes (29) are distributed in a serpentine shape.

4. A high-purity aminosulfonic acid production equipment according to claim 3, characterized in that: The stirring unit comprises an auger piece 1 (11) and an auger piece 2 (13); the bottom end of the rotating shaft 1 (7) extends to the inner side of the annular partition (28) and is fixedly connected to the auger piece 1 (11); a mounting ring (14) is fixedly connected to the inner wall of the sulfonation kettle (1); a gear ring (15) is fixedly connected to the bottom of the mounting ring (14); a gear 1 (9) is fixedly connected to the rotating shaft 1 (7); a plurality of gear 2s (10) are meshingly connected to the outer side of the gear 1 (9); the plurality of gear 2s (10) are meshingly connected to the gear ring (15); the plurality of gear 2s (10) are fixedly connected to the rotating shaft 2 (12); the bottom of the mounting ring (14) is rotatably connected to a sealing rotating ring (18); the plurality of rotating shafts (12) are fixedly connected to the sealing rotating ring (18); the bottom end of the rotating shaft 2 (12) extends to the outer side of the annular partition (28) and is fixedly connected to the auger piece 2 (13).

5. A high-purity aminosulfonic acid production equipment according to claim 4, characterized in that: The top of the rotating shaft (7) is rotatably connected to a water inlet pipe (8), and one end of the water inlet pipe (8) away from the rotating shaft (7) is externally connected to a water supply device. The top of the rotating shaft (7) is provided with a water inlet cavity (19), and the water inlet pipe (8) is connected to the water inlet cavity (19). The bottom of the rotating shaft (7) is provided with a water outlet cavity (32), and the bottom end of the rotating shaft (7) is rotatably connected to a water outlet pipe (33). One end of the water pipe three (33) away from the rotating shaft one (7) passes through the discharge pipe (3) and extends to the outside of the sulfonation kettle (1); the water pipe three (33) is L-shaped and is fixedly connected to the discharge pipe (3); the water pipe two (30) is connected to the water pipe three (33); the bottom of the water inlet chamber one (19) is connected to the top of the inner cavity of the auger piece one (11); and the top of the water outlet chamber one (32) is connected to the bottom of the inner cavity of the auger piece one (11).

6. A high-purity aminosulfonic acid production equipment according to claim 5, characterized in that: An annular fixed tube (16) is fixedly connected to the top of the inner cavity of the sulfonation kettle (1), the rotating shaft (7) is connected to the annular fixed tube (16) in a sealed and rotatable manner, through grooves (20) are evenly formed on the rotating shaft (7), the through grooves (20) are connected to the water inlet cavity (19) and the annular fixed tube (16), a plurality of connecting tubes (17) are connected between the inner cavity of the mounting ring (14) and the annular fixed tube (16), a water inlet cavity (34) is formed on the top of the rotating shaft (12), through holes (31) are evenly formed on the sealing rotating ring (18), the through holes (31) are connected to the water inlet cavity (34) in a one-to-one correspondence, and the rotating shaft A water outlet cavity 2 (35) is provided at the bottom of the second (12), an annular fixed pipe 2 (37) is fixedly connected to the bottom of the outer wall of the annular partition (28), a sealing ring (41) is rotatably connected to the annular fixed pipe 2 (37), a connecting pipe 2 (36) is fixedly connected to the bottom end of the second rotating shaft (12), one end of the connecting pipe 2 (36) is connected to the water outlet cavity 2 (35), one end of a plurality of connecting pipes 2 (36) away from the second rotating shaft (12) is fixedly connected to the sealing ring (41), the connecting pipe 2 (36) is connected to the annular fixed pipe 2 (37), and a plurality of connecting pipes 3 (38) are connected between the annular fixed pipe 2 (37) and the water outlet pipe 3 (33).

7. A high-purity aminosulfonic acid production equipment according to claim 6, characterized in that: A spoiler (39) is evenly fixedly connected to the inner wall of the heat conduction cavity (24); the spoiler (39) is in an I-shape, and a spoiler hole (40) is provided on the spoiler (39).

8. A high-purity aminosulfonic acid production equipment according to claim 7, characterized in that: The spoiler hole (40) is conical, and a spiral groove is provided on the inner wall of the spoiler hole (40).

9. A high-purity aminosulfonic acid production equipment according to claim 8, characterized in that: An air filter (42) is fixedly connected to one end of the exhaust pipe (4) away from the sulfonation kettle (1).

10. A high-purity aminosulfonic acid synthesis process, characterized in that: The synthesis process is applicable to a high-purity aminosulfonic acid production device as described in claim 9, and the synthesis process comprises the following steps: S1: The staff first adds fuming sulfuric acid into the sulfonation kettle (1) through the feed pipe (2), starts the motor (5), and drives the rotating shaft (7) to rotate through the motor (5) and the belt (6), so that the stirring unit starts stirring; S2: When the temperature in the sulfonation kettle (1) drops to 20-40°C, the mixed sulfuric acid and urea are added to the sulfonation kettle (1) through the feed pipe (2), stirred for 8 hours, and then gradually heated to 70-90°C to evaporate sulfur trioxide; S3: After cooling and crystallization, crude aminosulfonic acid is obtained, and finally, high-purity aminosulfonic acid is obtained by recrystallization with water and dehydration and drying.

Citation Information

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