Kettle for dehydration and alcohol removal of dichloroethane

Abstract

The utility model provides a kettle for dehydration and alcohol removal of dichloroethane, which comprises a reaction kettle, the reaction kettle comprises a kettle body, a stirring mechanism is fixedly arranged at the top of the kettle body, a stirring shaft is fixedly connected with a transmission mechanism through a support rod, the bottom of the transmission mechanism is fixedly connected with a mixing mechanism, the mixing mechanism comprises a connecting seat, a stirring rod and a hydraulic cylinder, the connecting seat is fixedly connected with the bottom of the enclosure, the top end of the stirring rod is rotatably connected with the interior of the connecting seat, and a plurality of uniformly distributed rod bodies are arranged on the stirring rod. The stirring mechanism and the mixing mechanism are arranged in the kettle body and are matched to realize full mixing, and the mixing mechanism can be folded after stirring, so that the mixing efficiency can be improved, the subsequent standing layering cannot be influenced, the production period of dichloroethane can be effectively shortened, the production efficiency is improved, and the production cost is reduced. The dichloroethane recovery solvent is subjected to washing alcohol removal treatment, and the yield of acylation reaction is better stabilized and improved, so that the solvent scrap consumption and the production cost are reduced.

Description

Technical Field

[0001] This utility model relates to a reactor for dehydrating and removing alcohol from dichloroethane, belonging to the field of chemical production operation and synthesis process technology. Background Technology

[0002] Fine chemical synthesis processes utilize numerous solvents that meet the specific production requirements and are considered optimal. Dichloroethane is a key solvent for producing ethyl 2-hydroxy-2-(4-phenoxyphenyl)propionate. In the acylation reaction, dichloroethane is the primary solvent. However, after a certain reaction cycle, its content decreases while other alcohols accumulate, gradually reducing the acylation yield.

[0003] To ensure reaction yield, approximately 30% of the dichloroethane solvent needs to be replaced periodically, resulting in consistently high consumption. Furthermore, in the water washing and layering unit, emulsification frequently occurs due to the accumulation of fusel alcohols, causing difficulties in layering and extending the water washing production cycle. Secondly, in the post-treatment dichloroethane recovery and dehydration section, the influence of fusel alcohols gradually prolongs the distillation and dehydration time and cycle, leading to a gradual decrease in the recovery rate and efficiency of dichloroethane, and an increase in related energy consumption such as electricity, steam, circulating water, and cold salt. Utility Model Content

[0004] In order to solve the above-mentioned technical problems, this utility model provides a reactor for dehydrating and removing alcohol from dichloroethane.

[0005] This utility model solves the above-mentioned technical problems through the following technical solutions:

[0006] This utility model provides a reactor for dehydrating and removing alcohol from dichloroethane, including a reactor body. The reactor body has an outer shell fixedly installed on its surface. A stirring mechanism is fixedly installed on the top of the reactor body. The stirring mechanism includes a stirring shaft and a stirring paddle. The stirring shaft is rotatably connected to the top of the reactor body, and the stirring paddle is fixedly connected to the bottom of the stirring shaft. The stirring paddle has an arc-shaped structure and is located at the bottom of the reactor body. The stirring paddle has multiple evenly distributed through holes.

[0007] The stirring shaft is fixedly connected to the transmission mechanism via a support rod. A mixing mechanism is fixedly connected to the bottom of the transmission mechanism. The mixing mechanism includes a connecting seat, a stirring rod, and a hydraulic cylinder. The connecting seat is fixedly connected to the bottom of the ring and is located inside the limiting ring. The top of the stirring rod is rotatably connected to the connecting seat. The stirring rod has multiple evenly distributed rods.

[0008] In this technical solution, two sealed cavities are formed between the outer shell and the vessel body. A first heater and a second heater with a spiral structure are fixedly installed on the outer surface of the vessel body. The first heater and the second heater are respectively located in two separate cavities, and both the first heater and the second heater are located inside the outer shell.

[0009] In this technical solution, a plurality of evenly distributed support legs are fixedly installed on the outer wall of the outer shell, and the surface of the vessel body and the outer shell are both fixedly fitted with a heat insulation layer, and the support legs penetrate the heat insulation layer.

[0010] In this technical solution, the top of the vessel is fixedly connected to the exhaust pipe and the input pipe, the bottom of the vessel is fixedly connected to the output pipe, and a conveying pipe is fixedly installed on the side wall of the vessel. The exhaust pipe, the input pipe, the output pipe and the conveying pipe are all connected through the insulation layer.

[0011] In this technical solution, a sleeve is fixedly installed on the top of the vessel body, the top of the sleeve is fixedly connected to the drive motor, and the output end of the drive motor is fixedly connected to the stirring shaft through a coupling.

[0012] In this technical solution, the transmission mechanism includes a surrounding ring and a limiting ring. The inner wall of the surrounding ring is fixedly connected to the stirring shaft through two support rods. There are two limiting rings, which are correspondingly arranged at the upper and lower ends of the surrounding ring. The limiting ring is fixedly connected to the inner wall of the vessel, and the surrounding ring is rotatably connected to the inside of the vessel.

[0013] In this technical solution, a mixing mechanism is fixedly installed at the bottom of the ring, and the stirring rod has a bent structure.

[0014] In this technical solution, the hydraulic cylinder is fixedly connected to the bottom of the limiting ring, the telescopic end of the hydraulic cylinder is fixedly connected to the end head, the end head has a convex structure, the bottom of the limiting ring is provided with a movable ring, the movable ring has a T-shaped guide groove, the end head is slidably connected to the guide groove of the movable ring, and the inner side of the movable ring is movably connected to the stirring rod through a connecting rod.

[0015] In this technical solution, the connecting seats are arranged on both sides of the top of the stirring rod.

[0016] In this technical solution, there are multiple hydraulic cylinders, which are evenly distributed at the bottom of the limiting ring.

[0017] Based on common knowledge in the field, the above-mentioned preferred conditions can be combined arbitrarily to obtain various preferred embodiments of this utility model.

[0018] The positive and progressive effects of this utility model are as follows:

[0019] The aforementioned reactor for dehydrating and removing alcohol from dichloroethane improves solvent recovery quality and stabilizes and increases the yield of the acylation reaction by washing the dichloroethane recovery solvent with water to remove alcohol. This reduces solvent waste and production costs. By washing dichloroethane with water to remove alcohol before distillation and dehydration, the main content of recovered dichloroethane is increased or guaranteed, and enriched fusel alcohols are removed. This achieves a high and stable yield of the acylation reaction and solves the emulsification problem caused by fusel alcohol enrichment in the water washing unit, as well as the low recovery rate and efficiency of distillation and dehydration of dichloroethane. This significantly reduces the solvent consumption per unit and the consumption of related energy sources such as electricity, steam, circulating water, and cold salt, while also shortening the production cycle and ensuring production stability of related units.

[0020] Furthermore, by combining a stirring mechanism and a mixing mechanism within the reactor, dichloroethane can be fully mixed during water washing to remove alcohol, effectively reducing the stirring time required. Simultaneously, the mixing mechanism can be retracted after stirring, preventing the solvent from adhering to the aqueous phase on the stirring rod and affecting the stratification effect. This ensures that the stratification during settling is not affected by the stirring rod. The multiple rods on the stirring rod not only improve mixing efficiency but also do not affect subsequent settling, effectively shortening the dichloroethane production cycle and improving production efficiency. Attached Figure Description

[0021] Figure 1 This is a schematic diagram of the overall three-dimensional structure of this utility model.

[0022] Figure 2 This is a schematic diagram of the internal structure of the vessel body of this utility model.

[0023] Figure 3 This is a schematic diagram of the internal structure of the enclosure of this utility model.

[0024] Figure 4 This utility model Figure 3 A magnified schematic diagram of the structure at point A in the middle.

[0025] Figure 5 This is a schematic diagram of the internal front view of the present invention.

[0026] Figure 6 This is a schematic diagram of the process for dehydrating and removing alcohol from dichloroethane according to this utility model.

[0027] Explanation of reference numerals in the attached figures:

[0028] 100. Reactor; 11. Reactor body; 111. Outer shell; 112. First heater; 113. Second heater; 114. Support leg; 115. Insulation layer; 116. Exhaust pipe; 117. Input pipe; 118. Output pipe; 119. Conveying pipe; 21. Sleeve; 211. Drive motor; 212. Stirring shaft; 213. Stirring paddle; 214. Through hole; 215. Support rod; 31. Enclosure ring ; 311, Limiting ring; 312, Connecting seat; 313, Stirring rod; 314, Hydraulic cylinder; 315, End; 316, Moving ring; 317, Connecting rod; 200, Primary condenser; 300, Secondary collector; 400, Tank for dichloroethane to be recovered; 500, Qualified dichloroethane tank; 600, Water separator; 700, Dichloroethane receiving tank; 800, Water receiving tank; 900, Water washing phase tank. Detailed Implementation

[0029] The present invention will be further illustrated by way of embodiments below, but the present invention is not limited to the scope of the embodiments described herein.

[0030] like Figure 1-6 As shown, the reactor for dehydrating and removing alcohol from dichloroethane includes a reactor 100. The reactor 100 includes a reactor body 11, and a shell 111 is fixedly installed on the surface of the reactor body 11. Two sealed cavities are formed between the shell 111 and the reactor body 11. A first heater 112 and a second heater 113 with a spiral structure are fixedly installed on the outer surface of the reactor body 11. The first heater 112 and the second heater 113 are respectively located in the two separated cavities. Both the first heater 112 and the second heater 113 are located inside the shell 111. Therefore, a cavity is formed between the vessel body 11 and the outer shell 111 through the outer shell 111. The middle part of the outer shell 111 is fixedly connected to the vessel body 11 through a spacer ring. The spacer ring forms two cavities inside the outer shell 111, so that the first heater 112 and the second heater 113 do not affect each other. The first heater 112 can heat the bottom of the vessel body 11, so that the dichloroethane can reach the boiling point and achieve dehydration treatment. The second heater 113 can realize auxiliary temperature control. It can be used in parallel or alone as needed to ensure the temperature is uniform when heating dichloroethane.

[0031] Multiple evenly distributed support legs 114 are fixedly installed on the outer wall of the outer shell 111. The support legs 114 are fixed to the ground, and the part of the vessel body 11 located below the support legs 114 penetrates the ground and is installed to the next layer, which can ensure the stable installation of the reactor 100. Both the vessel body 11 and the outer shell 111 are fixedly fitted with a heat insulation layer 115. The support legs 114 penetrate the heat insulation layer 115 and are located on the outside of the heat insulation layer 115. By setting the heat insulation layer 115, heat preservation can be achieved, so that the heat during heating will not be dissipated too quickly, thus improving the energy saving effect.

[0032] The top of the vessel body 11 is fixedly connected to the exhaust pipe 116 and the input pipe 117, respectively. The bottom of the vessel body 11 is fixedly connected to the output pipe 118. A conveying pipe 119 is fixedly installed on the side wall of the vessel body 11. The exhaust pipe 116, the input pipe 117, the output pipe 118, and the conveying pipe 119 are all connected through the insulation layer 115. The exhaust pipe 116 is used for the discharge of azeotropic steam. The input pipe 117 can be used for the conveying of dichloroethane or water. The top of the vessel body 11 is provided with at least two input pipes 117. The output pipe 118 is used for the output of dichloroethane waiting to be recovered after stratification.

[0033] A stirring mechanism is fixedly installed on the top of the vessel body 11. The stirring mechanism includes a stirring shaft 212 and a stirring paddle 213. A sleeve 21 is fixedly installed on the top of the vessel body 11. The top of the sleeve 21 is fixedly connected to a drive motor 211, and the output end of the drive motor 211 is fixedly connected to the stirring shaft 212 through a coupling. The stirring shaft 212 is rotatably connected to the top of the vessel body 11. The stirring paddle 213 is fixedly connected to the bottom of the stirring shaft 212. The stirring paddle 213 has an arc-shaped structure and is located at the bottom of the vessel body 11. The stirring paddle 213 has multiple evenly distributed through holes 214. By setting the through holes 214, the medium can be dispersed, so that dichloroethane can be quickly and efficiently mixed with the aqueous phase, ensuring the uniformity of the mixing of the aqueous phase and dichloroethane, and ensuring the efficiency of water washing to remove alcohol.

[0034] The stirring shaft 212 is fixedly connected to the transmission mechanism via a support rod 215. A mixing mechanism is fixedly connected to the bottom of the transmission mechanism. The transmission mechanism includes a surrounding ring 31 and a limiting ring 311. The inner wall of the surrounding ring 31 is fixedly connected to the stirring shaft 212 via two support rods 215. There are two limiting rings 311, which are correspondingly arranged at the upper and lower ends of the surrounding ring 31. The limiting rings 311 are fixedly connected to the inner wall of the vessel body 11, and the surrounding ring 31 is rotatably connected to the inside of the vessel body 11. The stirring shaft 212 drives the support rod 215 and the surrounding ring 31 to rotate synchronously. The limiting rings 311 can limit the surrounding ring 31 and ensure the stable rotation of the surrounding ring 31.

[0035] A mixing mechanism is fixedly installed at the bottom of the enclosure 31. The mixing mechanism includes a connecting seat 312, a stirring rod 313, and a hydraulic cylinder 314. The connecting seat 312 is fixedly connected to the bottom of the enclosure 31 and is located inside the limiting ring 311. The top end of the stirring rod 313 is rotatably connected to the connecting seat 312. The stirring rod 313 has multiple evenly distributed rods. The mixing effect is amplified by the cooperation of the stirring rod 313 and the rods, so that dichloroethane and the water phase are fully mixed during stirring. The stirring rod 313 has a bent structure. The structure of the stirring rod 313 allows it to avoid interference with the stirring shaft 212 and the support rod 215 when rotating around the connecting seat 312.

[0036] The hydraulic cylinder 314 is fixedly connected to the bottom of the limiting ring 311. The telescopic end of the hydraulic cylinder 314 is fixedly connected to the end head 315. The end head 315 has a convex structure. The bottom of the limiting ring 311 is provided with a movable ring 316. A T-shaped guide groove is opened in the movable ring 316. The end head 315 is slidably connected to the guide groove of the movable ring 316. The inner side of the movable ring 316 is movably connected to the stirring rod 313 through the connecting rod 317. Thus, when the stirring shaft 212 drives the ring 31 to rotate, the ring 31 drives the connecting seat 312 and the stirring rod 313 to rotate synchronously. The stirring rod 313 drives the movable ring 316 to rotate synchronously through the connecting rod 317, so that the movable ring 316 rotates on the surface of the end head 315, thereby realizing the synchronous rotation of the stirring rod 313 and the stirring paddle 213. The stirring paddle 213, the stirring rod 313, and the support rod 215 on the stirring rod 313 achieve efficient mixing.

[0037] The connecting seats 312 are located on both sides of the top of the stirring rod 313. When the stirring rod 313 is rotated by the surrounding ring 31, the resistance formed by the stirring rod 313 when it is inserted into dichloroethane can be absorbed by the connecting seats 312. That is, the connecting seats 312 drive the stirring rod 313 to rotate around the vessel body 11 to overcome the resistance of the stirring rod 313. When the stirring rod 313 rotates, the connecting rod 317 only drives the movable ring 316 to rotate, and will not generate too much resistance to affect its smooth rotation.

[0038] The hydraulic cylinders 314 are multiple and evenly distributed at the bottom of the limiting ring 311. The movable ring 316 is limited by the end 315 at the bottom of the hydraulic cylinder 314, so that it can rotate stably. The telescopic end of the hydraulic cylinder 314 is provided with a limiting rib, which is engaged and slids with the bottom of the cylinder body of the hydraulic cylinder 314. By providing a limiting rib on the telescopic end of the hydraulic cylinder 314, it can be ensured that the cylinder body and the telescopic end of the hydraulic cylinder 314 can extend and retract normally without relative rotation.

[0039] In specific operation, the stirring shaft 212 drives the stirring rod 313 to rotate synchronously to achieve efficient stirring and mixing. After the operation is completed, the hydraulic cylinder 314 shortens to drive the end 315 to move upward. The end 315 pushes the movable ring 316 upward, and the connecting rod 317 pushes the stirring rod 313 to rotate and retract, so that the stirring rod 313 is separated from the mixture of dichloroethane and water phase. At this time, the static stratification operation is carried out to avoid the water phase adhering to the stirring rod 313 and its surface rod body, which would affect the stratification effect. This can achieve rapid stratification, improve stirring and mixing efficiency, and shorten the dichloroethane production cycle.

[0040] Specifically, such as Figure 6 As shown, the specific steps for removing alcohol from dichloroethane are as follows:

[0041] 1. Preparation of materials in reactor 100: Open the vent valve of reactor 100, open the feed valve of reactor 100, and start the pump to pump 5500 kg of dichloroethane containing fusel oil to be recovered from tank 400 into the reactor.

[0042] 2. Water washing to remove alcohol: Add 550 kg of fresh water to reactor 100, start stirring and wash for 30 minutes, stop stirring and let stand to separate the layers. The lower layer of dichloroethane to be recovered is sent to the dichloroethane recovery tank 400, and the upper aqueous phase is sent to the water washing aqueous phase tank 900.

[0043] The specific steps for dehydrating dichloroethane are as follows:

[0044] 3. Distillation and dehydration of dichloroethane:

[0045] 3.1. The dichloroethane to be recovered, after being washed with water to remove alcohol, is added to the reactor at 100°C and stirred.

[0046] 3.2 Open the circulating water supply and return valve of the first-stage condenser 200 and the cold salt supply and return valve of the second-stage trap 300.

[0047] 3.3 Open the steam trap of reactor 100 and the steam regulating valve of reactor 100. Control the steam pressure by adjusting the opening degree. Heat the mixture until liquid appears in the glass separator below the condenser. Collect the water layer collected in the early stage in the water receiving tank 800. After dehydration, put it into the water washing phase tank 900 for wastewater recycling treatment. A small amount of water-containing dichloroethane in the lower layer of the separator is returned to the reactor, and the rest is collected into the dichloroethane receiving tank 700.

[0048] 3.4 After the water volume in the separator 600 decreases, a small amount of water-containing dichloroethane in the lower layer of the separator is returned to the reactor, while the rest is collected in the dichloroethane receiving tank 700 and then stored in the dichloroethane recovery tank 400 for further dehydration treatment in the next batch.

[0049] 3.5 When the glass separator becomes clear, take a sample from the reflux line to measure the water content. If the water content is <0.05%, stop the 100°C steam extraction from the reactor; otherwise, continue extraction until the water content is within acceptable limits.

[0050] 3.6. Close the 100-degree steam trap of the reactor, open the circulating water supply and return valve, and circulate the circulating water to cool down to 30-35℃. Transfer the dichloroethane in the reactor to a qualified dichloroethane tank 500 for later use in the reaction.

[0051] This utility model is not limited to the above-described embodiments. Any changes in its shape or structure fall within the protection scope of this utility model. The protection scope of this utility model is defined by the appended claims. Those skilled in the art can make various changes or modifications to these embodiments without departing from the principles and essence of this utility model, but all such changes and modifications fall within the protection scope of this utility model.

Claims

1. A vessel for dehydrating and removing alcohol from dichloroethane, comprising a reaction vessel (100), said reaction vessel (100) comprising a vessel body (11), wherein a shell (111) is fixedly mounted on the surface of said vessel body (11), characterized in that, A stirring mechanism is fixedly installed on the top of the vessel body (11). The stirring mechanism includes a stirring shaft (212) and a stirring paddle (213). The stirring shaft (212) is rotatably connected to the top of the vessel body (11), and the stirring paddle (213) is fixedly connected to the bottom of the stirring shaft (212). The stirring paddle (213) has an arc-shaped structure and is located at the bottom of the vessel body (11). The stirring paddle (213) has multiple evenly distributed through holes (214). The stirring shaft (212) is fixedly connected to the transmission mechanism via a support rod (215). A mixing mechanism is fixedly connected to the bottom of the transmission mechanism. The mixing mechanism includes a connecting seat (312), a stirring rod (313), and a hydraulic cylinder (314). The connecting seat (312) is fixedly connected to the bottom of the ring (31). The connecting seat (312) is located inside the limiting ring (311). The top of the stirring rod (313) is rotatably connected to the connecting seat (312). The stirring rod (313) has multiple evenly distributed rods.

2. The reactor for dehydration and alcohol removal of dichloroethane as described in claim 1, characterized in that: Two sealed cavities are formed between the outer shell (111) and the vessel body (11). A first heater (112) and a second heater (113) with a spiral structure are fixedly installed on the outer surface of the vessel body (11). The first heater (112) and the second heater (113) are located in two separate cavities respectively. The first heater (112) and the second heater (113) are both located inside the outer shell (111).

3. The reactor for dehydration and alcohol removal of dichloroethane as described in claim 1, characterized in that: The outer wall of the outer shell (111) is fixedly installed with a plurality of evenly distributed support legs (114), and the surfaces of the vessel body (11) and the outer shell (111) are both fixedly fitted with a heat insulation layer (115), and the support legs (114) penetrate the heat insulation layer (115).

4. The reactor for dehydration and alcohol removal of dichloroethane as described in claim 1, characterized in that: The top of the vessel body (11) is fixedly connected to the exhaust pipe (116) and the input pipe (117) respectively, the bottom of the vessel body (11) is fixedly connected to the output pipe (118), the side wall of the vessel body (11) is fixedly installed with a conveying pipe (119), and the exhaust pipe (116), the input pipe (117), the output pipe (118) and the conveying pipe (119) are all connected through the insulation layer (115).

5. The reactor for dehydration and alcohol removal of dichloroethane as described in claim 1, characterized in that: A sleeve (21) is fixedly installed on the top of the vessel body (11). The top of the sleeve (21) is fixedly connected to the drive motor (211), and the output end of the drive motor (211) is fixedly connected to the stirring shaft (212) through a coupling.

6. The reactor for dehydration and alcohol removal of dichloroethane as described in claim 1, characterized in that: The transmission mechanism includes a ring (31) and a limiting ring (311). The inner wall of the ring (31) is fixedly connected to the stirring shaft (212) by two support rods (215). There are two limiting rings (311), which are respectively set at the upper and lower ends of the ring (31). The limiting rings (311) are fixedly connected to the inner wall of the vessel body (11), and the ring (31) is rotatably connected to the inside of the vessel body (11).

7. The reactor for dehydration and alcohol removal of dichloroethane as described in claim 1, characterized in that: A mixing mechanism is fixedly installed at the bottom of the ring (31), and the stirring rod (313) has a bent structure.

8. The reactor for dehydration and alcohol removal of dichloroethane as described in claim 1, characterized in that: The hydraulic cylinder (314) is fixedly connected to the bottom of the limiting ring (311). The telescopic end of the hydraulic cylinder (314) is fixedly connected to the end head (315). The end head (315) has a convex structure. The bottom of the limiting ring (311) is provided with a movable ring (316). A T-shaped guide groove is opened in the movable ring (316). The end head (315) is slidably connected to the guide groove of the movable ring (316). The inner side of the movable ring (316) is movably connected to the stirring rod (313) through the connecting rod (317).

9. The reactor for dehydration and alcohol removal of dichloroethane as described in claim 1, characterized in that: The connecting seat (312) is located on both sides of the top of the stirring rod (313).

10. The reactor for dehydration and alcohol removal of dichloroethane as described in claim 1, characterized in that: The number of hydraulic cylinders (314) is multiple, and the multiple hydraulic cylinders (314) are evenly distributed at the bottom of the limiting ring (311).

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