Deacidification kettle for preparing chloroformate
By designing a deacid kettle for uniform distribution and sufficient stirring of nitrogen during the preparation of chloroformate, the problems of uneven distribution of gas and low deacid efficiency are solved, and efficient deacid treatment and reduction of nitrogen consumption are achieved.
Patent Information
- Application Number
- CN202411496609.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-25
- Publication Date
- 2025-01-03
AI Technical Summary
There is uneven gas distribution in the deacidification treatment of isopropyl chloroformate, resulting in low deacidification efficiency and quality, large nitrogen consumption and long deacidification time.
A deacid kettle for chloroformate preparation is designed, using an air pump and a two-axis extension motor system to achieve uniform distribution of nitrogen through an annular tray and transverse tray, and fully stirred and mixed with multiple sets of stirring shafts and stirring rods. , improve the uniformity of gas distribution and material mixing.
The uniform distribution of nitrogen in the kettle body and the full mixing of reaction liquid are achieved, which significantly improves the deacidification efficiency and quality, shortens the deacidification time, and reduces nitrogen consumption.
Smart Images

Figure CN119236848A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of chloroformates, and particularly relates to a deacidification kettle for preparing chloroformates. Background Art
[0002] Chloroformate compounds mainly include methyl chloroformate, ethyl chloroformate, propyl chloroformate, isopropyl chloroformate, and n-butyl chloroformate. Among them, isopropyl chloroformate is an organic compound that is mainly used as a pesticide intermediate, ore flotation agent, and initiator for free radical polymerization reactions, and has a wide range of applications.
[0003] At present, isopropyl chloroformate is mainly synthesized by phosgene or methyl chloroformate and isopropyl alcohol, esterification occurs in reactor or esterification tower, a large amount of hydrogen chloride and excessive phosgene can be present in reaction solution, it is necessary to deviate from hydrogen chloride and phosgene by depickling process and obtain the product of high content, specifically reaction solution is sent in depickling still, by jacket hot water heating, improve reacting liquid temperature, then nitrogen bubbling depickling is passed into from the bottom of still, the gas deviated from is condensed by condenser but after, destroyed to tail gas destruction system, then discharged.But in actual depickling process, there is the situation of uneven gas distribution, depickling efficiency and quality are not high, cause a batch of material depickling required time longer, cause nitrogen consumption very high, urgently need to be solved. Summary of the Invention
[0004] In view of this, the object of the present invention is to provide a deacidification kettle for preparing chloroformate, which can achieve uniform distribution of nitrogen and sufficient stirring and mixing with materials to solve the above problems.
[0005] To achieve the above object, the technical solution adopted by the present invention is: a deacidification kettle for preparing chloroformate, comprising a base, a kettle body fixed on the base and an air pump, one end of the top of the kettle body is connected to a feed pipe with a feed valve, the other end of the top is connected to an exhaust pipe with an exhaust valve, an air inlet pipe is vertically penetrated and fixed in the center of the bottom, and one end of the bottom is connected to a discharge pipe with a discharge valve, the bottom end of the air inlet pipe is connected to the air outlet of the air pump, the top end is closed and a plurality of support rods are vertically fixed on the edge of the outer top end, the top ends of the support rods are fixedly connected to the same transmission box, and the upper inner portion of the transmission box is fixed The fixed frame is provided with a first double-axis extension motor, and a crankshaft is provided at the lower part horizontally and rotatably. A first driving bevel gear is fixedly sleeved on the output shaft of the lower part of the first double-axis extension motor, and a first driven bevel gear is fixedly sleeved on the crankshaft. The first driving bevel gear is vertically meshed with the first driven bevel gear, and a connecting rod is installed on the connecting rod journal of the crankshaft. The bottom end of the connecting rod is hinged with a lifting column, and the bottom end of the lifting column extends out of the transmission box and is fixedly connected to a lifting plate. The lifting plate is slidably sleeved with the support rod and its circumferential side is fixedly connected to an annular air distribution pipe, and a plurality of first air distribution pipes are provided on the upper and lower sides of the annular air distribution pipe. The air outlet hole and its lower side are connected with the top of the air inlet pipe through a hose. A plurality of protective boxes distributed at circumferential intervals are fixed on the lifting plate. A second double-axis extension motor is fixed in the middle of the protective box, and solid stirring shafts are provided horizontally and rotatably in the upper and lower parts. A second driving bevel gear is fixed on the upper and lower conveying shafts of the second double-axis extension motor. A second driven bevel gear is fixed on the two solid stirring shafts. The second driving bevel gear is vertically meshed with the second driven bevel gear on the same side. The end of the solid stirring shaft away from the lifting column extends out of the protective box and is radially fixed on it. A plurality of solid stirring rods are provided, and the output shaft of the upper part of the first double-shaft extension motor extends out of the transmission box and is fixedly connected to a rotating plate. A hollow stirring shaft is vertically fixed on the left and right sides of the bottom of the rotating plate, and a plurality of hollow stirring rods are radially connected on the lower part of the hollow stirring shaft. A plurality of through holes are provided on the upper circumferential side of the air inlet pipe, and a conveying box is rotatably sleeved thereon. The left and right sides of the conveying box are fixedly connected with transverse air distribution pipes, and the tail end of the transverse air distribution pipe is fixedly connected to the bottom end of the hollow stirring shaft on the same side. A plurality of second air outlet holes are provided on the circumferential sides of the transverse air distribution pipe and the hollow stirring rod.
[0006] Preferably, the outer fixed sleeve of the kettle body is provided with an insulation jacket, a medium input ring pipe is fixedly provided in the lower part of the insulation jacket, and a medium output ring pipe is fixedly provided in the upper part, the medium input ring pipe is connected to the medium input pipe extending out of the insulation jacket, and the medium output ring pipe is connected to the medium output pipe extending out of the insulation jacket, and a plurality of S-shaped heat exchange tubes are distributed between the medium input ring pipe and the medium output ring pipe, the bottom end of the S-shaped heat exchange tube is connected to the medium input ring pipe, and the top end is connected to the medium output ring pipe.
[0007] Preferably, the kettle body is fixedly mounted on the base by a plurality of legs.
[0008] Preferably, the legs and the base are both made of foam aluminum.
[0009] Preferably, a rubber anti-slip pad is fixed on the bottom of the base.
[0010] The beneficial effect of the present invention is that when in use, the air inlet of the air pump is connected to the existing nitrogen source, and the exhaust pipe is connected to the subsequent treatment process. During deacidification treatment, the feed valve can be opened first, and the reaction liquid to be treated can be fed into the kettle through the feed pipe. After the feeding is completed, the feed valve is closed, the exhaust valve is opened, and then the air pump and the first double-shaft motor and the second double-shaft motor are started to realize deacidification treatment. Specifically, under the pumping of the air pump, the nitrogen in the nitrogen source can be first transported to the air inlet pipe, and then the nitrogen is diverted to the annular air distribution pipe and the conveying box through the hose and the through hole. The nitrogen entering the annular air distribution pipe can be sprayed upward and downward into the middle part of the kettle body through the first air outlet holes on the upper and lower sides thereof. The nitrogen entering the conveying box can continue to be diverted to the two horizontal air distribution pipes. Part of the nitrogen can be directly sprayed into the lower part of the kettle body in a divergent shape through the second air outlet holes on the horizontal air distribution pipe, and part of the nitrogen can continue to be transported to the hollow stirring shaft, and diverted to each hollow stirring rod through the hollow stirring shaft, and sprayed into the edge of the kettle body in a divergent shape through the second air outlet holes on the hollow stirring rod. At the same time, the operation of the first dual-extension motor drives both the crankshaft via a gear transmission and the rotating plate. The crankshaft's rotation is converted into the overall lifting and lowering motion of the lifting column, lifting plate, and annular gas distribution pipe, thereby more evenly distributing nitrogen throughout the center of the kettle. Furthermore, the operation of the second dual-extension motor within each protective box drives the corresponding solid stirring shaft via corresponding gear transmissions. Multiple sets of rotating solid stirring shafts and their attached solid stirring rods can be used to thoroughly stir and mix the reaction liquid and nitrogen from both the upper and lower sides of the annular gas distribution pipe. The rotation of the rotating plate drives the overall rotation of the two sets of hollow stirring shafts. With the rotational connection between the delivery box and the air inlet pipe and the fixed connection between the transverse gas distribution pipe and the hollow stirring shafts, the delivery box, transverse gas distribution pipe, hollow stirring shaft, and the multiple sets of hollow stirring rods attached to the hollow stirring shafts can rotate as a whole, thus more evenly distributing nitrogen throughout the bottom and sides of the kettle and thoroughly stirring and mixing the reaction liquid and nitrogen from both the bottom and sides of the kettle. In this way, nitrogen can be injected at multiple locations in the middle, bottom, and sides of the kettle body, coordinated with lifting and rotation. This can distribute the nitrogen more evenly and completely, and can also help the reaction liquid and nitrogen to be stirred and mixed more evenly, which is more conducive to bubbling deacidification, and can greatly improve the efficiency and quality of deacidification. Compared with existing technologies, it can effectively shorten the time required for deacidification of a batch of materials and reduce nitrogen consumption. The deacidified gas can be discharged through the exhaust pipe to subsequent processing steps. After deacidification is completed, the discharge valve is opened and the material can be discharged through the discharge pipe. BRIEF DESCRIPTION OF THE DRAWINGS
[0011] Figure 1 It is a schematic diagram of the main structure of the present invention; Figure 2 It is a schematic diagram of the main cross-sectional structure of the present invention; Figure 3 This is a schematic diagram of the main structure of the air intake pipe and the structure above it according to the present invention; Figure 4 yes Figure 3 Schematic diagram of the enlarged structure at A in the middle; Figure 5 yes Figure 3 Schematic diagram of the enlarged structure at B in the middle; Figure 6 1 is a schematic diagram of the top view of the lifting plate of the present invention; Figure 7 It is a schematic diagram of the main cross-sectional structure of the thermal insulation jacket of the present invention.
[0012] In the figure, the numbers are: 1 for the base, 2 for the kettle body, 3 for the air pump, 4 for the feed valve, 5 for the feed pipe, 6 for the exhaust valve, 7 for the exhaust pipe, 8 for the air intake pipe, 9 for the discharge valve, 10 for the discharge pipe, 11 for the support rod, 12 for the transmission box, 13 for the first double-axis extension motor, 14 for the crankshaft, 15 for the first active bevel gear, 16 for the first driven bevel gear, 17 for the connecting rod, 18 for the lifting column, 19 for the lifting plate, 20 for the annular air distribution pipe, 21 for the first air outlet, 22 for the hose, 23 for the protective box, 24 for the second Double-axle extension motor, 25 is a solid stirring shaft, 26 is the second active bevel gear, 27 is the second driven bevel gear, 28 is a solid stirring rod, 29 is a rotating plate, 30 is a hollow stirring shaft, 31 is a hollow stirring rod, 32 is a through hole, 33 is a conveying box, 34 is a transverse air distribution pipe, 35 is a second air outlet, 36 is a thermal insulation jacket, 37 is a medium input ring pipe, 38 is a medium output ring pipe, 39 is a medium input pipe, 40 is a medium output pipe, 41 is an S-shaped heat exchange pipe, 42 is a support leg, and 43 is a rubber anti-slip pad. DETAILED DESCRIPTION
[0013] The present invention is further described in detail below with reference to the accompanying drawings and specific embodiments: like Figures 1 to 7As shown, a deacidification kettle for preparing chloroformate comprises a base 1, a kettle body 2 fixed to the base 1, and an air pump 3. A feed pipe 5 with a feed valve 4 is connected to one end of the top of the kettle body 2, an exhaust pipe 7 with an exhaust valve 6 is connected to the other end of the top, an air inlet pipe 8 is vertically fixedly provided through the center of the bottom, and a discharge pipe 10 with a discharge valve 9 is connected to one end of the bottom. The bottom end of the air inlet pipe 8 is connected to the air outlet of the air pump 3, the top end is closed, and a plurality of support rods 11 are vertically fixed to the edges of the outer top end. The top ends of the support rods 11 are fixedly connected to a common transmission box 12. A first dual-axis motor 13 is fixedly mounted in the upper portion of the transmission box 12, and a crankshaft 14 is horizontally and rotatably mounted in the lower portion. A first driving bevel gear 15 is fixedly sleeved on the output shaft of the lower portion of the first dual-axis motor 13, and a first driven bevel gear 16 is fixedly sleeved on the crankshaft 14. The first driving bevel gear 15 is vertically meshed with the first driven bevel gear 16. A connecting rod 17 is mounted on the connecting rod journal of the crankshaft 14. A lifting column 18 is hinged at the bottom end of the connecting rod 17. The bottom end of the lifting column 18 extends out of the transmission case 12 and is fixedly connected to a lifting plate 19. The lifting plate 19 is slidably sleeved with the support rod 11 and a ring-shaped air distribution pipe 20 is fixedly connected to its circumferential side. A plurality of first air outlet holes 21 are provided on the upper and lower sides of the ring-shaped air distribution pipe 20, and its lower side is connected to the top end of the air inlet pipe 8 through a hose 22. Several circumferentially spaced protective boxes 23 are fixedly mounted on the lifting plate 19. A second dual-extension motor 24 is fixedly mounted in the middle of the protective box 23. Solid stirring shafts 25 are mounted horizontally and rotatably in both the upper and lower sections. Second driving bevel gears 26 are fixedly mounted on the upper and lower conveyor shafts of the second dual-extension motor 24. Second driven bevel gears 27 are fixedly mounted on both solid stirring shafts 25. The second driving bevel gears 26 are vertically meshed with the second driven bevel gears 27 on the same side. The solid stirring shafts 25 extend out of the protective box 23 at the end away from the lifting column 18 and are radially fixed with several solid stirring rods 28. The output shaft of the first dual-extension motor 13 extends out of the transmission case 12 and is fixedly connected to a rotating plate 29. Hollow stirring shafts 30 are vertically fixed to the left and right sides of the bottom of the rotating plate 29. Several hollow stirring rods 31 are radially connected to the lower portion of the hollow stirring shafts 30. A plurality of through holes 32 are formed on the circumference of the upper portion of the air inlet pipe 8, to which a delivery box 33 is rotatably sleeved. Transverse air distribution pipes 34 are fixedly connected to the left and right sides of the delivery box 33. The tail ends of the transverse air distribution pipes 34 are fixedly connected to the bottom end of the hollow stirring shaft 30 on the same side. A plurality of second air outlet holes 35 are formed on the circumference of the transverse air distribution pipes 34 and the hollow stirring rod 31. When in use, the air inlet of the air pump 3 is connected to the existing nitrogen source, and the exhaust pipe 7 is connected to the subsequent processing steps. During the deacidification treatment, the feed valve 4 can be opened first, and the reaction liquid to be treated is fed into the kettle body 2 through the feed pipe 5. After the feeding is completed, the feed valve 4 is closed, the exhaust valve 6 is opened, and then the air pump 3 and the first double-axis motor 13 and the second double-axis motor 24 are started to realize the deacidification treatment. Specifically: under the pumping of the air pump 3, the nitrogen in the nitrogen source can be first transported to the air inlet pipe 8, and then the nitrogen can be diverted to the annular air distribution pipe 20 and the conveying box 33 through the hose 22 and the through hole 32. The nitrogen entering the annular air distribution pipe 20 can be directed upward and downward through the first air outlet 21 on the upper and lower sides thereof. The nitrogen gas ejected into the middle part of the kettle body 2 and entering the delivery box 33 can be further diverted into the two horizontal air distribution pipes 34. Part of the nitrogen gas can be directly ejected into the lower part of the kettle body 2 in a divergent manner through the second air outlet holes 35 on the horizontal air distribution pipes 34, and part of the nitrogen gas can be continuously transported to the hollow stirring shaft 30, diverted into each hollow stirring rod 31 through the hollow stirring shaft 30, and diverged into the edge of the kettle body 2 through the second air outlet holes 35 on the hollow stirring rod 31. At the same time, the operation of the first double-axis extension motor 13 can not only drive the crankshaft 14 to rotate through gear transmission, but also directly drive the rotation of the turntable 29. The rotation of the crankshaft 14 can be converted into the overall lifting movement of the lifting column 18, the lifting plate 19 and the annular gas distribution pipe 20, so that the nitrogen is distributed more evenly in the middle part of the kettle body 2. The operation of the second double-axis extension motor 24 in each protective box 23 can drive the corresponding solid stirring shaft 25 to rotate through the corresponding gear transmission. The reaction liquid and nitrogen can be fully stirred and mixed from the upper and lower sides of the annular gas distribution pipe 20 by using multiple groups of rotating solid stirring shafts 25 and the solid stirring rods 28 thereon. The rotation of the rotating plate 29 drives the two sets of hollow stirring shafts 30 to rotate as a whole. With the rotational connection between the conveying box 33 and the air inlet pipe 8 and the fixed connection between the transverse air distribution pipe 34 and the hollow stirring shaft 30, the conveying box 33, the transverse air distribution pipe 34, the hollow stirring shaft 30, and the multiple sets of hollow stirring rods 31 on the hollow stirring shaft 30 can rotate as a whole, thereby more evenly distributing nitrogen gas at the bottom and sides of the kettle body 2 and thoroughly stirring and mixing the reaction liquid and nitrogen gas from the bottom and sides of the kettle body 2. In this way, nitrogen gas can be injected from multiple locations in the middle, bottom, and sides of the kettle body 2, coordinated with the lifting and rotation. This achieves more uniform and complete distribution of nitrogen gas and more uniform stirring and mixing of the reaction liquid and nitrogen gas, further facilitating bubbling deacidification and significantly improving the efficiency and quality of deacidification. Compared with existing technologies, it can effectively shorten the deacidification time of a batch of materials and reduce nitrogen consumption. The deacidified gas can be discharged to the subsequent processing step through the exhaust pipe 7. After the deacidification is completed, the discharge valve 9 is opened and the material can be discharged through the discharge pipe 10.
[0014] In this embodiment, an insulating jacket 36 is fixedly provided on the outer side of the kettle body 2, a medium input loop 37 is fixedly provided in the lower part of the insulating jacket 36, and a medium output loop 38 is fixedly provided in the upper part. The medium input loop 37 is connected to a medium input pipe 39 extending out of the insulating jacket 36, and the medium output loop 38 is connected to a medium output pipe 40 extending out of the insulating jacket 36. Several S-shaped heat exchange tubes 41 are distributed between the medium input loop 37 and the medium output loop 38, and the bottom end of the S-shaped heat exchange tube 41 is connected to the medium input loop 37, and the top end is connected to the medium output loop 38. In actual use, the medium input pipe 39 and the medium output pipe 40 are both connected to a medium conveying pipeline, and the medium can be hot water, so that during the deacidification operation, the hot water can be sent to the medium input ring pipe 37 through the medium input ring pipe 37, and then diverted to each S-shaped heat exchange tube 41 through the medium input ring pipe 37, so that the hot water flows in an S shape through the S-shaped heat exchange tube 41 and then gathers into the medium output ring pipe 38, and then flows out through the medium output pipe 40, thereby achieving effective heating of the kettle body 2 and providing the temperature required for deacidification. The structural design of the S-shaped heat exchange tube 41 can effectively extend the residence time of hot water and make the hot water more evenly distributed, so that the heating of the kettle body 2 is more uniform and effective, which is more conducive to ensuring the efficiency and quality of deacidification and shortening the time required for deacidification.
[0015] In this embodiment, the kettle body 2 is fixedly mounted on the base 1 by a plurality of legs 42 for easy fixation in use.
[0016] In this embodiment, the legs 42 and the base 1 are both made of foam aluminum. Foam aluminum is an existing material with excellent properties such as high specific stiffness, high damping, shock absorption and energy absorption. It can play a good role in buffering, shock absorption and protection, and is more conducive to the smooth progress of the deacidification operation.
[0017] In this embodiment, a rubber anti-skid pad 43 is fixed to the bottom of the base 1, which can effectively enhance the friction between the base 1 and the ground, making the entire deacidification device more stable and reliable, and ensuring the smooth progress of the deacidification operation.
[0018] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.
Claims
1. A deacidification kettle for preparing chloroformate, comprising a base, a kettle body fixed on the base and an air pump, characterized in that: One end of the top of the kettle body is connected to a feed pipe with a feed valve, the other end of the top is connected to an exhaust pipe with an exhaust valve, an air intake pipe is vertically penetrated through the center of the bottom, and one end of the bottom is connected to a discharge pipe with a discharge valve, the bottom end of the air intake pipe is connected to the air outlet of the air pump, the top end is closed, and a plurality of support rods are vertically fixed on the edge of the outer top end, the top ends of the support rods are fixedly connected to the same transmission box, the upper inner part of the transmission box is fixedly provided with a first double-axis extension motor, the lower part is horizontally and rotatably provided with a crankshaft, and the output shaft at the lower part of the first double-axis extension motor The upper fixed sleeve is provided with a first active bevel gear, the upper fixed sleeve of the crankshaft is provided with a first driven bevel gear, the first active bevel gear is vertically meshed with the first driven bevel gear, a connecting rod is installed on the connecting rod journal of the crankshaft, the bottom end of the connecting rod is hinged with a lifting column, the bottom end of the lifting column extends out of the transmission box and is fixedly connected with a lifting plate, the lifting plate is slidably sleeved with the support rod and a ring-shaped air distribution pipe is fixedly connected to the circumference thereof, a plurality of first air outlet holes are opened on the upper and lower sides of the ring-shaped air distribution pipe, and the lower side thereof is connected with the top end of the air inlet pipe through a hose, and the lifting plate A plurality of protective boxes are fixedly provided at intervals in a circumference, a second double-axle extension motor is fixedly provided in the middle of the protective box, solid stirring shafts are horizontally and rotatably provided in the upper and lower parts, second driving bevel gears are fixedly provided on the conveying shafts of the upper and lower parts of the second double-axle extension motor, second driven bevel gears are fixedly provided on the two solid stirring shafts, the second driving bevel gear is vertically meshed with the second driven bevel gear on the same side, one end of the solid stirring shaft away from the lifting column extends out of the protective box and a plurality of solid stirring rods are radially fixed thereon, the first The output shaft of a double-axle extension motor extends out of the transmission box and is fixedly connected to a rotating plate. Hollow stirring shafts are vertically fixed on the left and right sides of the bottom of the rotating plate. A plurality of hollow stirring rods are radially connected to the lower part of the hollow stirring shaft. A plurality of through holes are provided on the upper circumferential side of the air inlet pipe, and a conveying box is rotatably sleeved thereon. The left and right sides of the conveying box are fixedly connected to transverse air distribution pipes, and the tail end of the transverse air distribution pipe is fixedly connected to the bottom end of the hollow stirring shaft on the same side. A plurality of second air outlet holes are provided on the circumferential sides of the transverse air distribution pipe and the hollow stirring rods.
2. The deacidification kettle for preparing chloroformate according to claim 1, characterized in that: An outer fixed sleeve of the kettle body is provided with an insulation jacket, a medium input ring pipe is fixedly provided in the lower part of the insulation jacket, and a medium output ring pipe is fixedly provided in the upper part, the medium input ring pipe is connected to the medium input pipe extending out of the insulation jacket, and the medium output ring pipe is connected to the medium output pipe extending out of the insulation jacket, and a plurality of S-shaped heat exchange tubes are distributed between the medium input ring pipe and the medium output ring pipe, the bottom end of the S-shaped heat exchange tube is connected to the medium input ring pipe, and the top end is connected to the medium output ring pipe.
3. The deacidification kettle for preparing chloroformate according to claim 1, characterized in that: The kettle body is fixedly mounted on the base through a plurality of supporting legs.
4. The deacidification kettle for preparing chloroformate according to claim 3, characterized in that: The legs and the base are both made of foam aluminum.
5. The deacidification kettle for preparing chloroformate according to claim 1, characterized in that: A rubber anti-skid pad is fixedly arranged at the bottom of the base.
