A distillation column for bromine production and a method of using the same

CN118903849BActive Publication Date: 2026-11-03TANGSHAN SANYOU NEW MATERIALS CO LTD
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Patent Information

Application Number
CN202411117428.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-08-15
Publication Date
2026-11-03
Estimated Expiration
2044-08-15

AI Technical Summary

Technical Problem

In existing distillation towers used for bromine production, the reaction between chlorine and mother liquor is insufficient, leading to chlorine waste and reduced bromine purity.

Method used

The system employs a structure combining a ring-shaped spray pipe and a spiral heating steam pipe. The rotation of the ring-shaped spray pipe and the secondary preheating by the spiral heating steam pipe ensure uniform spraying and full reaction of the mother liquor. Combined with a sedimentation tank and baffle plate structure, impurities are filtered out and the purity of bromine gas is improved.

Benefits of technology

It improved the utilization rate of chlorine, enhanced the production efficiency of bromine, increased the purity of bromine, and reduced the impact of impurities.

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Abstract

The application belongs to the technical field of bromine production, and particularly relates to a distillation column for bromine production and a use method thereof. In view of the problems that existing chlorine cannot fully react with mother liquor, chlorine is wasted, the mother liquor is not uniformly preheated, a small amount of impurities may still be contained in bromine, and the purity of collected bromine in the later stage is affected, the following scheme is proposed. The scheme comprises a tower body and a filler layer fixed in the tower body, a ring-shaped spraying pipe above the filler layer is rotationally connected in the tower body, the ring-shaped spraying pipe is used for spraying the mother liquor to the filler layer, a conical partition below the filler layer is fixed in the tower body and is used for collecting the reacted liquid, and a waste liquid pipe penetrates through the bottom of the conical partition. In the application, the mother liquor can be heated twice, the heat energy carried in the steam is fully utilized, and when the mother liquor is sprayed, the ring-shaped spraying pipe is driven to rotate under the action of the booster pump, the nozzle and the arc-shaped plate, so that the mother liquor is uniformly sprayed on the filler layer, and the chlorine fully reacts with the mother liquor.
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Description

Technical Field

[0001] This invention relates to the field of bromine production technology, and in particular to a distillation column for bromine production and its usage method. Background Technology

[0002] Bromine is a brownish-red, volatile liquid with a strong, pungent odor. Its vapor is brownish-red, and its solid is yellowish-green with a metallic luster. It is an important chemical raw material. A utility model patent with patent number CN211004549U discloses a distillation tower for bromine production. However, this technical solution still faces some challenges in practical applications: 1. In this technical solution, the mother liquor is sprayed to contact chlorine gas, where it undergoes an exchange reaction with bromide ions to generate bromine gas. However, during the spraying process, the mother liquor continuously accumulates at a fixed position on the packing material, preventing the rising steam and chlorine gas from fully contacting the mother liquor. This affects the complete reaction between chlorine gas and the mother liquor, resulting in waste of chlorine gas and impacting the purity of the bromine gas. 2. During the bromine gas collection process, the bromine gas may still contain a small amount of impurities, which affects the purity of the collected bromine. In order to address the above problem, this invention proposes a distillation column for bromine production and its usage method. Summary of the Invention

[0003] The purpose of this invention is to solve the shortcomings of existing distillation towers for bromine production and their usage method, which are that chlorine cannot fully react with the mother liquor, resulting in chlorine waste and the bromine may still contain a small amount of impurities, affecting the purity of the bromine collected later.

[0004] To achieve the above objectives, the present invention adopts the following technical solution: A distillation column for bromine production includes a column body and a packing layer fixed inside the column body. An annular spray pipe located above the packing layer is rotatably connected inside the column body. The annular spray pipe is used to spray mother liquor onto the packing layer. The tower body is fixed with a conical baffle located below the packing layer for collecting the liquid after the reaction. A waste liquid pipe is fixedly inserted through the bottom of the conical baffle, and one end of the waste liquid pipe is fixedly extended to one side of the tower body for discharging the collected liquid to the outside. It also includes a condenser, which is set on one side of the tower body. A connecting pipe is fixed on one side of the condenser, and one end of the connecting pipe extends into the tower body. A liquid injection pipe is fixed on the side of the condenser away from the connecting pipe. A condenser tube is provided inside the condenser for the initial preheating of the mother liquor entering the condenser. It also includes a sedimentation tank, which is located below the condenser cylinder and is used to filter impurities contained in the liquid bromine after condensation in the condenser tube. The preheating structure, located inside the tower, is used for secondary preheating of the mother liquor after the initial preheating. The spray structure, located inside the tower, is used to uniformly spray the preheated mother liquor downwards onto the packing layer. The filter structure, located inside the sedimentation tank, is used to filter impurities in liquid bromine; Multiple stirring structures are arranged sequentially from top to bottom on the outer wall of the waste liquid pipe, with adjacent stirring structures arranged vertically. The waste liquid driving stirring structure inside the waste liquid pipe is used to stir the mother liquor located below the conical baffle in the tower body.

[0005] In one possible design, the spray structure includes a liquid storage ring fixed inside the tower body, and the liquid storage ring is slidably and sealingly disposed at the top of the annular spray pipe. Multiple arc-shaped plates are fixed to the top of the annular spray pipe, and the arc-shaped plates are located inside the liquid storage ring. Multiple injection holes are provided at the top of the annular spray pipe, and the injection holes cooperate with the arc-shaped plates for injecting mother liquor into the annular spray pipe. Multiple guide pipes are fixed to the outer wall of the tower body, and the bottom ends of the guide pipes extend into the tower body and are located below the conical baffle. The top ends of the guide pipes extend into the tower body and are located above the liquid storage ring. An L-shaped pipe is fixed to one side of each guide pipe. Multiple liquid storage tubes are fixed inside the liquid ring. The bottom end of the L-shaped tube extends into the liquid storage ring and is connected to the liquid storage tubes. Multiple nozzles are fixed on one side of the liquid storage tubes, and the nozzles cooperate with the arc-shaped plate to drive the annular spray pipe to rotate. The mother liquor after secondary heating is sprayed towards the arc-shaped plate through the nozzles under the action of the guide pipe and the booster pump, which drives the annular spray pipe to rotate. The annular spray pipe rotates during the spraying of liquid bromine, thereby uniformly spraying the liquid bromine onto the packing layer. In the later stage, chlorine can fully react with the bromide ions in the mother liquor in the packing layer, improving the utilization rate of chlorine and the production efficiency of bromine.

[0006] In one possible design, the filtration structure includes a baffle plate detachably fixed inside a sedimentation tank. The bottom end of the condenser tube extends fixedly into the sedimentation tank, penetrating the baffle plate. Multiple filter holes are provided on the top side of the sedimentation tank away from the condenser tube for filtering impurities in the liquid bromine. Multiple blocking components are fixed to the bottom inner wall of the sedimentation tank to obstruct the flow of liquid bromine below the baffle plate. A collection pipe is fixed to one side of the sedimentation tank above the baffle plate. Liquid bromine flows below the baffle plate, and the flow rate is reduced by the multiple blocking components, allowing impurities carried in the liquid bromine to precipitate. As the liquid bromine gradually increases, impurities are filtered through the filter holes, and the collection pipe collects relatively pure liquid bromine.

[0007] In one possible design, the blocking member consists of a first partition and two second partitions, with the tops of both the first and second partitions abutting against the bottom of the blocking plate. The sides of the two second partitions that are far apart from each other are fixedly connected to one inner wall of the sedimentation tank. The two sides of the first partition form a first gap with the two inner walls of the sedimentation tank, and the sides of the two second partitions that are close to each other form a second gap. The cooperation between the first gap and the second gap can effectively reduce the flow rate of liquid bromine, allowing impurities carried in the liquid bromine to precipitate.

[0008] In one possible design, the preheating structure includes a spiral heating steam pipe disposed within the tower body, located below a conical baffle. A vent pipe is fixed to the bottom end of the spiral heating steam pipe, extending to the bottom of the tower body. Multiple columns are fixed to the top of the conical baffle, with the same annular exhaust pipe fixed to the top of each column. The top of the spiral heating steam pipe penetrates the conical baffle and connects to the annular exhaust pipe. An annular chlorine exhaust pipe is fixed within the tower body, with an injection pipe fixed to one side of the annular chlorine exhaust pipe, one end of which extends to the side of the tower body for injecting chlorine gas into the annular chlorine exhaust pipe. The annular chlorine exhaust pipe is located above the annular exhaust pipe. After heat exchange through a condenser, the mother liquor undergoes initial preheating. The mother liquor then enters the tower body through a connecting pipe, and steam is injected into the spiral heating steam pipe through the vent pipe. The steam and the spiral heating steam pipe then perform secondary preheating of the mother liquor, fully utilizing the thermal energy within the steam.

[0009] In one possible design, the stirring structure includes a rotating box fixed to the outer wall of the waste liquid pipe. A rotating shaft is rotatably connected inside the rotating box. Multiple arc-shaped liquid-gathering plates are fixed to the outer wall of the rotating shaft, with one side of each arc-shaped liquid-gathering plate extending into the waste liquid pipe. The arc-shaped liquid-gathering plates rotate under the action of the downstream liquid. Rotating rods are fixed to both ends of the rotating shaft, with one end of each rotating rod extending to one side of the rotating box. Multiple stirring blades are fixed to the outer wall of each rotating rod. The mother liquor after the reaction is discharged to the outside through the waste liquid pipe under the action of a conical baffle. As the liquid flows downward through the waste liquid pipe, it drives the arc-shaped liquid-gathering plates and the rotating shaft to rotate. The rotating shaft drives the rotating rods and stirring blades to rotate, thereby stirring the mother liquor inside the tower. This allows the mother liquor to be uniformly heated under the action of the spiral heating steam pipe, facilitating the subsequent exchange reaction between bromide ions and chlorine gas in the mother liquor.

[0010] In one possible design, the inner and outer walls of the annular exhaust pipe are both fixed with multiple exhaust holes, which are placed at an angle downwards to prevent liquid from entering the annular exhaust pipe through the exhaust holes. The guide pipe is equipped with a booster pump, which works in conjunction with the guide pipe to increase the flow rate of the mother liquor injected into the liquid storage ring through the guide pipe, so as to drive the annular spray pipe to rotate.

[0011] In one possible design, a gas collecting pipe and a liquid draining pipe are fixed at the top and bottom of the tower body, respectively. The liquid draining pipe is used to discharge the residual mother liquor in the tower body. One end of the gas collecting pipe extends into the condenser and is connected to the top of the condenser, so that the collected bromine gas is condensed in the condenser and the mother liquor in the condenser is preheated to improve the utilization rate of thermal energy. Both the annular chlorine gas discharge pipe and the annular spray pipe are equipped with cross pipes, and the two cross pipes are connected to the corresponding annular chlorine gas discharge pipe and the annular spray pipe. Multiple through holes are provided on the side of the two cross pipes that are close to each other to increase the efficiency and area of ​​spraying and exhaust.

[0012] In one possible design, an annular inclined plate is fixed inside the tower body, and multiple ceramic columns are fixed at the bottom of the annular inclined plate. The bottom ends of the multiple ceramic columns are fixedly extended into the liquid storage ring, and the annular inclined plate is made of ceramic. Under the action of the ceramic columns, the annular inclined plate can transfer the heat energy of the mother liquor in the liquid storage ring to the annular inclined plate, preventing bromine gas from condensing at the bottom of the annular inclined plate. A reflux pipe is fixedly inserted through the tower body, and one end of the reflux pipe extends to the outside of the tower body and is connected to the gas collecting pipe. A one-way valve is installed in the reflux pipe. The reflux pipe and the one-way valve are used to guide the liquid bromine condensed at the top of the tower body into the gas collecting pipe. When the bromine gas and vapor rise and enter the condenser pipe through the gas collecting pipe, the bromine gas condenses on the inner wall of the top of the tower body. At this time, the condensed liquid bromine falls onto the annular inclined plate along the inner wall of the tower body. The condensed liquid bromine can be poured into the gas collecting pipe through the reflux pipe, avoiding the liquid bromine from flowing back into the tower body and wasting liquid bromine.

[0013] This application discloses a method of using a distillation column for bromine production, comprising the following steps: S1. The mother liquor is injected into the condenser through the injection pipe, preheated through the condenser, and then enters the tower body. Inside the tower, steam is preheated a second time through the spiral heating steam pipe and sprayed evenly by the annular spray pipe. At the same time, chlorine gas is injected through the annular chlorine gas discharge pipe and rises with the steam into the packing layer, where it reacts with bromide ions in the mother liquor to generate bromine gas. S2. Bromine gas mixes with water vapor and rises, then flows back to the condenser tube through the gas collecting pipe. In the condenser tube, it is condensed into liquid bromine by the action of the mother liquid. The liquid bromine passes below the baffle plate and is slowed down by multiple blocking components to promote the precipitation of impurities. After being filtered through the filter holes, the pure bromine liquid is collected by the collecting pipe. S3. The preheated mother liquor is sprayed onto the arc plate through the nozzle, driving the annular spray pipe to rotate, so as to achieve uniform spraying of bromine liquid onto the packing layer, enhance the reaction efficiency of chlorine and bromide ions, and improve the utilization rate of chlorine and the production of bromine. S4. The mother liquor after the reaction is guided to the waste liquid pipe through the conical baffle and discharged at the same time. At the same time, the arc-shaped liquid collection plate and the rotating shaft are driven to rotate, which drives the stirring blade to rotate, ensuring that the mother liquor is heated evenly in the tower and promoting the full reaction of bromide ions and chlorine gas. S5. After the bromine gas and vapor condense at the top of the tower, they slide down the annular inclined plate to the reflux pipe and are then introduced into the gas collecting pipe, which effectively prevents the condensed bromine liquid from flowing back into the tower and reduces waste.

[0014] Beneficial effects: In this invention, the liquid storage ring is slidably and sealed at the top of the annular spray pipe. Multiple arc-shaped plates are fixed to the top of the annular spray pipe, and multiple injection holes are provided at the top of the annular spray pipe. Multiple guide pipes are fixed to the outer wall of the tower body. The bottom end of the L-shaped pipe extends into the liquid storage ring and connects to the liquid storage pipe. Multiple nozzles are fixed to one side of the liquid storage pipe. Under the action of the guide pipe and the booster pump, the mother liquor is sprayed through the nozzles towards the arc-shaped plates, driving the annular spray pipe to rotate. This allows liquid bromine to be evenly sprayed onto the packing layer. Later, chlorine gas can fully react with bromide ions in the mother liquor within the packing layer, improving the utilization rate of chlorine gas and the production efficiency of bromine gas. In this invention, the condenser cylinder is equipped with a condenser tube, and the bottom end of the gas collecting pipe extends into the condenser cylinder and is connected to the condenser tube. The tower body is equipped with a spiral heating steam pipe. After the mother liquor enters the condenser cylinder, it undergoes heat exchange through the condenser tube to complete the initial preheating of the mother liquor. Then, the mother liquor enters the tower body through the connecting pipe, and steam is injected into the spiral heating steam pipe through the vent pipe. The mother liquor is preheated a second time through the steam and the spiral heating steam pipe, making full use of the heat energy in the steam to preheat the mother liquor entering the condenser cylinder and fully utilizing the heat energy carried by the steam. In this invention, a rotating shaft is rotatably connected inside the rotating box. Multiple arc-shaped liquid-gathering plates are fixed to the outer wall of the rotating shaft. Rotating rods are fixed to both ends of the rotating shaft, and multiple stirring blades are fixed to the outer wall of the rotating rods. After the reaction, the mother liquor is discharged to the outside through the waste liquid pipe under the action of the conical baffle. When the liquid flows downward through the waste liquid pipe, the liquid drives the arc-shaped liquid-gathering plates and the rotating shaft to rotate. The rotating shaft drives the rotating rods and stirring blades to rotate, which is used to stir the mother liquor in the tower, so that the mother liquor can be uniformly heated under the action of the spiral heating steam pipe, so as to facilitate the exchange reaction between bromide ions and chlorine gas in the mother liquor in the later stage. In this invention, a baffle plate is fixed inside the sedimentation tank, and the bottom end of the condenser tube penetrates the baffle plate. Multiple filter holes are provided on the top side of the sedimentation tank away from the condenser tube, and multiple blocking components are fixed on the bottom inner wall of the sedimentation tank. Liquid bromine flows into the area below the baffle plate, and the flow rate of liquid bromine can be reduced by the action of multiple blocking components, so as to allow impurities carried in the liquid bromine to precipitate. As the liquid bromine gradually increases, the impurities are filtered through the filter holes, and then the collection tube can collect relatively pure liquid bromine.

[0015] In this invention, the mother liquor can be reheated to make full use of the heat energy carried by the steam. When spraying the mother liquor, the booster pump, nozzle and arc plate can drive the annular spray pipe to rotate, so that the mother liquor is evenly sprayed on the packing layer, so that chlorine gas reacts fully with the mother liquor, improve the utilization rate of chlorine gas and improve the production efficiency of bromine gas. In addition, the condensed bromine liquid can be filtered to avoid impurities affecting the purity of the bromine liquid. Attached Figure Description

[0016] Figure 1 This is a three-dimensional structural schematic diagram of a distillation column for bromine production provided in Embodiment 1 of the present invention; Figure 2 This is a schematic diagram of the main cross-sectional structure of a distillation tower for bromine production provided in Embodiment 1 of the present invention; Figure 3 for Figure 2 Enlarged structural diagram at point A in the middle; Figure 4 This is a three-dimensional cross-sectional view of the condenser and sedimentation tank of a distillation tower for bromine production provided in Embodiment 1 of the present invention. Figure 5 A three-dimensional cross-sectional view of the liquid storage ring and annular spray pipe of a distillation tower for bromine production provided in Embodiment 1 of the present invention; Figure 6 for Figure 5 Enlarged structural diagram at point B; Figure 7 This is a three-dimensional cross-sectional view of the waste liquid pipe of a distillation tower for bromine production provided in Embodiment 1 of the present invention. Figure 8 This is a three-dimensional exploded structural diagram of the baffle plate, the first baffle plate, and the second baffle plate of a distillation tower for bromine production provided in Embodiment 1 of the present invention. Figure 9 This is a partial front view sectional view of the structure of a distillation column for bromine production provided in Embodiment 1 of the present invention.

[0017] In the diagram: 1. Tower body; 2. Conical baffle; 3. Spiral heating steam pipe; 4. Guide pipe; 5. Booster pump; 6. Annular spray pipe; 7. Packing layer; 8. Annular chlorine emission pipe; 9. Gas injection pipe; 10. Annular exhaust pipe; 11. Liquid storage ring; 12. L-shaped pipe; 13. Liquid storage pipe; 14. Spray head; 15. Arc-shaped plate; 16. Liquid injection hole; 17. Condenser; 18. Gas collecting pipe; 19. Condenser; 20. Liquid injection pipe; 21. 21. Connecting pipe; 22. Sedimentation tank; 23. Baffle plate; 24. Blocking component; 25. Collection pipe; 26. Filter hole; 27. First partition plate; 28. Second partition plate; 29. ​​Waste liquid pipe; 30. Rotating box; 31. Rotating shaft; 32. Arc-shaped liquid collection plate; 33. Rotating rod; 34. Stirring blade; 35. Drain pipe; 36. Annular inclined plate; 37. Ceramic column; 38. Return pipe; 39. Column; 40. Vent pipe; 41. Steam vent. Detailed Implementation

[0018] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments.

[0019] Example 1

[0020] Reference Figure 1 and Figure 2 A distillation column, used in bromine production, includes a column body 1 and a packing layer 7 fixed within the column body 1. An annular spray pipe 6 is rotatably connected within the column body 1, located above the packing layer 7, for spraying mother liquor onto the packing layer 7. A conical baffle 2 is fixed within the column body 1, located below the packing layer 7, for collecting the liquid after the reaction. A waste liquid pipe 29 is fixedly inserted through the bottom of the conical baffle 2, with one end of the waste liquid pipe 29 extending to one side of the column body 1 for discharging the collected liquid to the outside.

[0021] Reference Figure 1 , Figure 2 and Figure 4 The distillation column also includes a condenser 17, which is located on one side of the column body 1. A connecting pipe 21 is fixed to one side of the condenser 17, with one end of the connecting pipe 21 extending into the column body 1. A liquid injection pipe 20 is fixed to the side of the condenser 17 away from the connecting pipe 21. A condenser pipe 19 is provided inside the condenser 17 for initial preheating of the mother liquor entering the condenser 17.

[0022] Reference Figure 1 , Figure 2 and Figure 4 The distillation column also includes a settling tank 22, which is located below the condenser cylinder 17 and is used to filter impurities contained in the liquid bromine condensed in the condenser tube 19.

[0023] Reference Figure 1 and Figure 2 The distillation column also includes a preheating structure located within column body 1, used for secondary preheating of the mother liquor after the initial preheating. A spraying structure is also provided within column body 1 to evenly spray the secondary preheated mother liquor downwards onto the packing layer 7. A filtration structure is installed in the settling tank 22 to filter impurities from the liquid bromine. The distillation column also features multiple stirring structures, arranged sequentially from top to bottom on the outer wall of the waste liquid pipe 29, with adjacent stirring structures arranged vertically. The waste liquid-driven stirring structure within the waste liquid pipe 29 is used to stir the mother liquor located below the conical baffle 2 within column body 1.

[0024] Reference Figure 2 , Figure 5 and Figure 6 Specifically, the spray structure includes a liquid storage ring 11 fixed inside the tower body 1, which is slidably and sealed at the top of the annular spray pipe 6. Multiple arc-shaped plates 15 are fixed to the top of the annular spray pipe 6, located within the liquid storage ring 11. Multiple injection holes 16 are provided at the top of the annular spray pipe 6, cooperating with the arc-shaped plates 15 to inject mother liquor into the annular spray pipe 6. Multiple guide pipes 4 are fixed to the outer wall of the tower body 1, with their bottom ends extending into the tower body 1 and located below the conical baffle 2, and their top ends extending into the tower body 1 and located above the liquid storage ring 11. An L-shaped pipe 12 is fixed to one side of the guide pipe 4, and multiple liquid storage pipes 13 are fixed inside the liquid storage ring 11. The bottom ends of the L-shaped pipes 12 extend into the liquid storage ring 11 and are connected to the liquid storage pipes 13. Multiple nozzles 14 are fixed to one side of the liquid storage pipe 13. These nozzles 14 cooperate with the arc-shaped plate 15 to drive the rotation of the annular spray pipe 6. The mother liquor, after secondary heating, is sprayed towards the arc-shaped plate 15 through the nozzles 14 under the action of the guide pipe 4 and the booster pump 5, driving the annular spray pipe 6 to rotate. The annular spray pipe 6 rotates during the spraying of liquid bromine, thus uniformly spraying the liquid bromine onto the packing layer 7. This allows chlorine gas to fully react with bromide ions in the mother liquor within the packing layer 7, improving the utilization rate of chlorine gas and the production efficiency of bromine gas.

[0025] Reference Figure 2 , Figure 4 and Figure 8The filtration structure includes a baffle plate 23 detachably fixed inside the settling tank 22. The bottom end of the condenser tube 19 extends fixedly into the settling tank 22 and passes through the baffle plate 23. Multiple filter holes 26 are provided on the top side of the settling tank 22 away from the condenser tube 19 for filtering impurities in the liquid bromine. Multiple blocking members 24 are fixed to the bottom inner wall of the settling tank 22 to obstruct the flow of liquid bromine below the baffle plate 23. A collection tube 25 is fixed to one side of the settling tank 22 above the baffle plate 23. As liquid bromine flows below the baffle plate 23, the flow rate of the liquid bromine is reduced by the multiple blocking members 24, causing impurities carried in the liquid bromine to precipitate. As the amount of liquid bromine gradually increases, impurities are filtered through the filter holes 26, and then the collection tube 25 collects relatively pure liquid bromine.

[0026] Reference Figures 1-8 In actual operation, the mother liquor first enters the condenser tube 19 inside the condenser cylinder 17 for initial preheating, and then enters the tower body 1 through the connecting pipe 21. Inside the tower body 1, the mother liquor undergoes secondary preheating through the preheating structure before entering the spray structure. Specifically, the mother liquor enters the storage tube 13 inside the storage ring 11 through the guide pipe 4 and the L-shaped pipe 12, and then is sprayed onto the arc plate 15 through the nozzle 14, driving the annular spray pipe 6 to rotate, thereby uniformly spraying the mother liquor onto the packing layer 7. Chlorine gas enters the tower body 1 from the annular chlorine gas discharge pipe 8 and reacts with bromide ions in the mother liquor on the packing layer 7 to generate bromine gas. The reacted liquid is collected through the conical baffle 2 and discharged through the waste liquid pipe 29. At the same time, the waste liquid in the waste liquid pipe 29 drives the stirring structure to stir the mother liquor in the tower body 1, improving the reaction efficiency. The generated bromine gas is condensed by the condenser tube 19 and then enters the sedimentation tank 22 for filtration, finally obtaining relatively pure liquid bromine.

[0027] Reference Figure 4 and Figure 8 The specific design of the barrier component: The barrier component 24 in the distillation column consists of a first partition 27 and two second partitions 28. The tops of the first partition 27 and the two second partitions 28 are in close contact with the bottom of the barrier plate 23. The two second partitions 28 are respectively fixed to the inner walls of both sides of the settling tank 22. A first gap is formed between the two sides of the first partition 27 and the inner walls of both sides of the settling tank 22. A second gap is formed on the side of the two second partitions 28 that are close to each other. When liquid bromine flows through these gaps, its flow rate is effectively reduced, thereby allowing impurities carried in the liquid bromine to precipitate.

[0028] Reference Figures 1-3The specific design of the preheating structure includes a spiral heating steam pipe 3 inside the tower body 1, located below the conical baffle 2. A vent pipe 40 is connected to the bottom end of the spiral heating steam pipe 3, extending to the bottom of the tower body 1. Multiple columns 39 are fixed to the top of the conical baffle 2, and the tops of these columns collectively support an annular exhaust pipe 10. The top of the spiral heating steam pipe 3 passes through the conical baffle 2 and connects to the annular exhaust pipe 10. An annular chlorine exhaust pipe 8 is also fixed inside the tower body 1, with an injection pipe 9 connected to one side. One end of the injection pipe 9 extends to one side of the tower body 1 for injecting chlorine gas into the annular chlorine exhaust pipe 8. The annular chlorine exhaust pipe 8 is located above the annular exhaust pipe 10. The mother liquor is first preheated through the condenser pipe 19, and then enters the tower body 1 through the connecting pipe 21. Steam is injected into the spiral heating steam pipe 3 through the vent pipe 40 to preheat the mother liquor a second time, thereby making full use of the heat energy in the steam.

[0029] Reference Figure 2 and Figure 7 The specific design of the stirring structure includes a rotating box 30 fixed to the outer wall of the waste liquid pipe 29. A rotating shaft 31 is rotatably connected inside the rotating box 30. Multiple arc-shaped liquid-gathering plates 32 are fixed to the outer wall of the rotating shaft 31, with one side of each plate extending into the waste liquid pipe 29. When the liquid flows downwards through the waste liquid pipe 29, it drives the arc-shaped liquid-gathering plates 32 and the rotating shaft 31 to rotate. Rotating rods 33 are fixed to both ends of the rotating shaft 31, with one end extending into the rotating box 30. Multiple stirring blades 34 are fixed to the outer wall of the rotating rods 33. When the mother liquor after reaction is discharged to the outside through the waste liquid pipe 29 under the action of the conical baffle 2, the liquid drives the arc-shaped liquid-gathering plates 32 and the rotating shaft 31 to rotate, which in turn drives the rotating rods 33 and the stirring blades 34 to rotate, thus stirring the mother liquor inside the tower body 1. This allows the mother liquor to be uniformly heated under the action of the spiral heating steam pipe 3, facilitating the subsequent exchange reaction between bromide ions and chlorine in the mother liquor.

[0030] Reference Figures 1-3 The specific design of the annular exhaust pipe and the guide pipe: Multiple exhaust holes 41 are fixed on both the inner and outer walls of the annular exhaust pipe 10. These exhaust holes 41 are placed at an angle downwards to prevent liquid from entering the annular exhaust pipe 10 through the exhaust holes 41. A booster pump 5 is installed on the guide pipe 4. The booster pump 5 cooperates with the guide pipe 4 to increase the flow rate of the mother liquor injected into the liquid storage ring 11 through the guide pipe 4, thereby driving the annular spray pipe 6 to rotate.

[0031] Reference Figure 1 , Figure 2 and Figure 4The design of the gas collecting pipe and the liquid drain pipe: A gas collecting pipe 18 is fixed at the top of the distillation column, and a liquid drain pipe 35 is fixed at the bottom. The main function of the liquid drain pipe 35 is to discharge the residual mother liquor inside the column body 1. One end of the gas collecting pipe 18 extends into the condenser 17 and connects to the top of the condenser 19. This design allows the collected bromine gas to be condensed in the condenser 19, while simultaneously preheating the mother liquor in the condenser 17, thereby improving the utilization rate of thermal energy.

[0032] Reference Figure 2 and Figure 5 The cross-shaped tube design: Both the annular chlorine exhaust pipe 8 and the annular spray pipe 6 are equipped with cross-shaped tubes, and these two cross-shaped tubes are connected to the corresponding annular chlorine exhaust pipe 8 and annular spray pipe 6, respectively. Multiple through holes are provided on the side of the two cross-shaped tubes that are close to each other. This design can increase the efficiency and area of ​​spraying and exhaust.

[0033] Example 2

[0034] refer to Figure 9 Improvements based on Example 1: Design of the annular inclined plate and ceramic columns: An annular inclined plate 36 is fixed inside the tower body 1, and multiple ceramic columns 37 are fixed to the bottom of the plate. The bottom ends of these ceramic columns 37 are all fixedly extended into the liquid storage ring 11. The annular inclined plate 36 is made of ceramic material, which can transfer the heat energy of the mother liquor in the liquid storage ring 11 to the annular inclined plate 36 under the action of the ceramic columns 37, thereby preventing bromine gas from condensing at the bottom of the annular inclined plate 36.

[0035] Reflux pipe design: A reflux pipe 38 is fixedly installed inside the tower body 1, with one end extending to the outside of the tower body 1 and connecting to the gas collecting pipe 18. A one-way valve is installed inside the reflux pipe 38. When bromine gas and vapor rise and enter the condenser pipe 19 through the gas collecting pipe 18, the bromine gas will condense on the inner wall of the top of the tower body 1. At this time, the condensed liquid bromine will fall onto the annular inclined plate 36 along the inner wall of the tower body 1. Through the reflux pipe 38, the condensed liquid bromine can be guided into the gas collecting pipe 18, avoiding the waste caused by the liquid bromine flowing back into the tower body 1.

[0036] A method of using a distillation column for bromine production includes the following steps: S1. Mother liquor is injected into condenser cylinder 17 through injection pipe 20. Heat exchange occurs through condenser pipe 19, completing the initial preheating of mother liquor. Then, mother liquor enters tower body 1 through connecting pipe 21. Steam is injected into spiral heating steam pipe 3 through vent pipe 40. The mother liquor is preheated a second time through steam and spiral heating steam pipe 3. The preheated mother liquor is sprayed downward through annular spray pipe 6 under the action of guide pipe 4 and booster pump 5. Chlorine gas is injected into annular chlorine gas discharge pipe 8 through gas injection pipe 9. Chlorine gas and steam in annular exhaust pipe 10 move upward into packing layer 7, allowing mother liquor and chlorine gas to contact in packing layer 7. Chlorine gas and bromide ions exchange to generate bromine gas. S2. Bromine gas is heated together with water vapor and rises along the inner wall of tower 1. Finally, it flows back to condenser 19 under the action of gas collecting pipe 18. Under the action of mother liquor in condenser cylinder 17, it is condensed into liquid bromine, making full use of the heat energy in the steam. The liquid bromine flows into the lower part of baffle plate 23. Under the action of multiple baffle components 24, the flow rate of liquid bromine can be reduced, so that impurities carried in the liquid bromine can be precipitated. As the liquid bromine gradually increases, the impurities are filtered through filter hole 26. Then, the collection pipe 25 can collect relatively pure liquid bromine. S3. After secondary heating, the mother liquor is sprayed towards the arc plate 15 through the nozzle 14 under the action of the guide pipe 4 and the booster pump 5. This drives the annular spray pipe 6 to rotate. The annular spray pipe 6 rotates during the spraying of liquid bromine, which in turn can spray the liquid bromine evenly onto the packing layer 7. Later, chlorine can fully react with the bromide ions in the mother liquor in the packing layer 7, thereby improving the utilization rate of chlorine and the production efficiency of bromine. S4. After the reaction, the mother liquor is discharged to the outside through the waste liquid pipe 29 under the action of the conical baffle 2. When the liquid flows downward through the waste liquid pipe 29, the liquid drives the arc-shaped liquid collection plate 32 and the rotating shaft 31 to rotate. The rotating shaft 31 drives the rotating rod 33 and the stirring blade 34 to rotate, which is used to stir the mother liquor in the tower body 1, so that the mother liquor can be heated evenly under the action of the spiral heating steam pipe 3, so as to facilitate the exchange reaction between bromide ions and chlorine gas in the mother liquor in the later stage. S5. When bromine gas and vapor rise and enter the condenser 19 through the gas collecting pipe 18, bromine gas condenses on the inner wall of the top of the tower body 1. At this time, the condensed liquid bromine falls onto the annular inclined plate 36 along the inner wall of the tower body 1. The condensed liquid bromine can be poured into the gas collecting pipe 18 through the return pipe 38 to avoid the liquid bromine flowing back into the tower body 1 and causing waste of liquid bromine.

[0037] However, the working principle and wiring method of the booster pump 5 are commonplace and are all conventional methods or common knowledge, so they will not be described in detail here. Those skilled in the art can make any selections according to their needs or convenience.

[0038] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A distillation column for bromine production, characterized in that, It includes a tower body (1) and a packing layer (7) fixed inside the tower body (1). An annular spray pipe (6) located above the packing layer (7) is rotatably connected inside the tower body (1). The annular spray pipe (6) is used to spray mother liquor onto the packing layer (7). The tower body (1) is fixed with a conical baffle (2) located below the packing layer (7) for collecting the liquid after the reaction. A waste liquid pipe (29) is fixedly inserted through the bottom of the conical baffle (2), and one end of the waste liquid pipe (29) is fixedly extended to one side of the tower body (1) for discharging the collected liquid to the outside. It also includes a condenser (17), which is set on one side of the tower body (1). A connecting pipe (21) is fixed on one side of the condenser (17), and one end of the connecting pipe (21) extends into the tower body (1). A liquid injection pipe (20) is fixed on the side of the condenser (17) away from the connecting pipe (21). A condenser (19) is provided inside the condenser (17) for the initial preheating of the mother liquor entering the condenser (17). It also includes a sedimentation tank (22), which is located below the condenser (17) and is used to filter impurities contained in the liquid bromine after condensation in the condenser tube (19); The preheating structure is set inside the tower body (1) and is used to preheat the mother liquor after the initial preheating. The spray structure is set inside the tower body (1) and is used to spray the mother liquor after secondary preheating evenly downwards onto the packing layer (7); The filter structure is set inside the sedimentation tank (22) for filtering impurities in liquid bromine; Multiple stirring structures are arranged sequentially from top to bottom on the outer wall of the waste liquid pipe (29), and two adjacent stirring structures are arranged vertically. The waste liquid driving stirring structure in the waste liquid pipe (29) is used to stir the mother liquor located below the conical baffle (2) in the tower body (1). The preheating structure includes a spiral heating steam pipe (3) installed inside the tower body (1), and the spiral heating steam pipe (3) is located below the conical partition (2). The bottom end of the spiral heating steam pipe (3) is fixed with a vent pipe (40), and the bottom end of the vent pipe (40) extends to the bottom of the tower body (1). The top of the conical partition (2) is fixed with multiple columns (39), and the top of the multiple columns (39) is fixed with the same annular exhaust pipe (10). The top end of the spiral heating steam pipe (3) passes through the conical partition (2) and is connected to the annular exhaust pipe (10). An annular chlorine exhaust pipe (8) is fixed inside the tower body (1). An injection pipe (9) is fixed on one side of the annular chlorine exhaust pipe (8), and one end of the injection pipe (9) extends to one side of the tower body (1) for injecting chlorine into the annular chlorine exhaust pipe (8). The annular chlorine exhaust pipe (8) is located above the annular exhaust pipe (10).

2. The distillation column for bromine production according to claim 1, characterized in that, The spray structure includes a liquid storage ring (11) fixed inside the tower body (1), and the liquid storage ring (11) is slidably and sealed at the top of the annular spray pipe (6). The top of the annular spray pipe (6) is fixed with multiple arc-shaped plates (15), and the arc-shaped plates (15) are located inside the liquid storage ring (11). The top of the annular spray pipe (6) is provided with multiple injection holes (16), and the injection holes (16) cooperate with the arc-shaped plates (15) to inject the mother liquor into the annular spray pipe (6). The outer wall of the tower body (1) is fixed with multiple guide pipes (4), and the bottom end of the guide pipes (4) extends... The top end of the guide pipe (4) extends into the tower body (1) and is located below the conical partition (2). An L-shaped pipe (12) is fixed on one side of the guide pipe (4). Multiple liquid storage pipes (13) are fixed inside the liquid storage ring (11). The bottom end of the L-shaped pipe (12) extends into the liquid storage ring (11) and is connected to the liquid storage pipe (13). Multiple nozzles (14) are fixed on one side of the liquid storage pipe (13). The nozzles (14) cooperate with the arc plate (15) to drive the annular spray pipe (6) to rotate.

3. A distillation column for bromine production according to claim 2, characterized in that, The filtration structure includes a baffle plate (23) that is detachably and fixedly installed in the sedimentation tank (22). The bottom end of the condenser tube (19) is fixedly extended into the sedimentation tank (22). The bottom end of the condenser tube (19) penetrates the baffle plate (23). The top of the sedimentation tank (22) away from the condenser tube (19) is provided with multiple filter holes (26) for filtering impurities in the liquid bromine. The bottom inner wall of the sedimentation tank (22) is fixed with multiple blocking components (24). The blocking components (24) are used to obstruct the flow of liquid bromine below the baffle plate (23). A collection tube (25) located above the baffle plate (23) is fixed on one side of the sedimentation tank (22).

4. A distillation column for bromine production according to claim 3, characterized in that, The blocking member (24) is composed of a first partition (27) and two second partitions (28). The tops of the first partition (27) and the second partitions (28) are in contact with the bottom of the blocking plate (23). The two second partitions (28) are fixedly connected to the inner wall of one side of the sedimentation tank (22) on opposite sides. The two sides of the first partition (27) form a first gap with the inner walls of the two sides of the sedimentation tank (22). The two second partitions (28) are close to each other on opposite sides, forming a second gap. The cooperation of the first gap and the second gap can effectively reduce the flow rate of liquid bromine, so that the impurities carried in the liquid bromine can be precipitated.

5. A distillation column for bromine production according to claim 4, characterized in that, The stirring structure includes a rotating box (30) fixed to the outer wall of the waste liquid pipe (29). A rotating shaft (31) is rotatably connected inside the rotating box (30). Multiple arc-shaped liquid-gathering plates (32) are fixed to the outer wall of the rotating shaft (31), and one side of the arc-shaped liquid-gathering plates (32) extends into the waste liquid pipe (29). The arc-shaped liquid-gathering plates (32) rotate under the action of the downstream liquid. Rotating rods (33) are fixed to both ends of the rotating shaft (31), and one end of the rotating rods (33) extends to one side of the rotating box (30). Multiple stirring blades (34) are fixed to the outer wall of the rotating rods (33).

6. A distillation column for bromine production according to claim 5, characterized in that, The inner and outer walls of the annular vent pipe (10) are fixed with multiple vent holes (41), and the vent holes (41) are placed obliquely downward to prevent liquid from entering the annular vent pipe (10) through the vent holes (41). The guide pipe (4) is equipped with a booster pump (5), and the booster pump (5) cooperates with the guide pipe (4) to increase the flow rate of the mother liquid injected into the liquid storage ring (11) by the guide pipe (4).

7. A distillation column for bromine production according to claim 6, characterized in that, The top and bottom of the tower body (1) are respectively fixed with a gas collecting pipe (18) and a liquid draining pipe (35). The liquid draining pipe (35) is used to discharge the mother liquor remaining in the tower body (1). One end of the gas collecting pipe (18) extends into the condenser cylinder (17) and is connected to the top of the condenser pipe (19). This is used to condense the collected bromine gas in the condenser pipe (19) and preheat the mother liquor in the condenser cylinder (17) to improve the utilization rate of thermal energy. The annular chlorine gas discharge pipe (8) and the annular spray pipe (6) are both equipped with cross pipes. The two cross pipes are connected to the corresponding annular chlorine gas discharge pipe (8) and annular spray pipe (6). The two cross pipes are provided with multiple through holes on the side that is close to each other to increase the efficiency and area of ​​spraying and exhaust.

8. A distillation column for bromine production according to claim 7, characterized in that, An annular inclined plate (36) is fixed inside the tower body (1). Multiple ceramic columns (37) are fixed at the bottom of the annular inclined plate (36). The bottom ends of the multiple ceramic columns (37) are fixedly extended into the liquid storage ring (11). The annular inclined plate (36) is made of ceramic material. Under the action of the ceramic columns (37), the annular inclined plate (36) can introduce the heat energy of the mother liquor in the liquid storage ring (11) into the annular inclined plate (36), so as to avoid condensation of bromine gas at the bottom of the annular inclined plate (36). A reflux pipe (38) is fixedly inserted inside the tower body (1). One end of the reflux pipe (38) extends to the outside of the tower body (1) and is connected to the gas collecting pipe (18). A one-way valve is provided in the reflux pipe (38). The reflux pipe (38) and the one-way valve are used to introduce the liquid bromine condensed at the top of the tower body (1) into the gas collecting pipe (18).

9. The method of using a distillation column for bromine production according to claim 8, characterized in that, Includes the following steps: S1. The mother liquor is injected into the condenser (17) through the injection pipe (20), preheated by the condenser (19) first, and then enters the tower body (1). Inside the tower, the steam preheats the mother liquor a second time through the spiral heating steam pipe (3) and is evenly sprayed by the annular spray pipe (6). At the same time, chlorine gas is injected through the annular chlorine gas discharge pipe (8) and rises with the steam into the packing layer (7), where it reacts with the bromide ions in the mother liquor to generate bromine gas. S2. Bromine gas and water vapor mix and rise, and flow back to the condenser tube (19) through the gas collecting tube (18). Under the action of the mother liquid in the condenser tube (17), the liquid bromine is condensed into liquid bromine. The liquid bromine passes below the baffle plate (23) and passes through multiple blocking components (24) to slow down the flow rate to promote the precipitation of impurities. After being filtered through the filter hole (26), the pure bromine liquid is collected by the collecting tube (25). S3. The preheated mother liquor is sprayed onto the arc plate (15) through the nozzle (14), driving the annular spray pipe (6) to rotate, so as to achieve uniform spraying of bromine liquid onto the packing layer (7), enhance the reaction efficiency of chlorine and bromide ions, and improve the utilization rate of chlorine and the production of bromine. S4. The mother liquor after the reaction is guided to the waste liquid pipe (29) through the conical baffle (2) and discharged. At the same time, the arc-shaped liquid collection plate (32) and the rotating shaft (31) are driven to rotate, which drives the stirring blade (34) to rotate, ensuring that the mother liquor is heated evenly in the tower and promoting the full reaction of bromide ions and chlorine gas. S5. After the bromine gas and vapor condense at the top of the tower, they slide down along the annular inclined plate (36) to the return pipe (38) and then into the gas collecting pipe (18), which effectively prevents the condensed bromine liquid from flowing back into the tower and reduces waste.

Citation Information

Patent Citations

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