Reaction kettle for processing organic compound
By designing the push plate structure in the quantitative filling device of the reactor, the tetramethylguanidine in the barrel is crushed, which solves the problems of low production efficiency and conversion rate caused by its agglomeration, and achieves a more efficient reaction process.
Patent Information
- Application Number
- CN202411896755.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-23
- Publication Date
- 2025-03-04
AI Technical Summary
During the production process of 1,4-cyclohexanedimethylamine, tetramethylguanidine is prone to agglomeration, resulting in the difficulty in reacting with the mixed liquid in the reactor, reducing the production efficiency and conversion rate.
A reactor for processing organic compounds is designed, including a quantitative filling device and a push plate structure. By rotating the first push plate and the second push plate, the materials in the barrel are extruded, cut and stirred, and the agglomerated tetramethylguanidine is crushed to improve its contact efficiency with the reaction liquid.
By crushing the agglomerated tetramethylguanidine, its reaction efficiency in the reactor is improved, and the production efficiency and conversion rate of 1,4-cyclohexanedimethylamine are improved.
Smart Images
Figure CN119549065A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of organic compound processing, in particular to a reaction kettle for organic compound processing. Background Art
[0002] 1,4-cyclohexanedimethylamine is an industrially important compound used as a raw material for epoxy curing agents, polyamides, polyurethanes, and the like.
[0003] 1,4-cyclohexanedimethylamine exists in two isomeric forms, cis and trans, from the cyclohexane ring. The physical properties of polymers obtained by using different ratios of cis and trans cyclohexanedimethylamine vary greatly. For example, polyamide synthesized from 1,4-cyclohexanedimethylamine with a high trans content has the characteristics of high melting point and high heat resistance. Another example: polyamide synthesized from 1,3-cyclohexanedimethylamine with a high cis content has high crystallinity, while polyamide synthesized from 1,3-cyclohexanedimethylamine with a high trans content is amorphous. Therefore, it is extremely important to control the ratio of cis and trans isomers in cyclohexanedimethylamine according to different needs.
[0004] When producing 1,4-cyclohexanedimethylamine, add p-phenylenediamine, toluene, liquid ammonia, and ruthenium catalyst into the reactor. Under stirring conditions, control the temperature in the reactor to 100-105°C, maintain the hydrogen pressure in the reactor at 5.0Mpa, and perform internal standard detection on the reaction liquid in the reactor. When the internal standard content of p-phenylenediamine is 2.0%, add tetramethylguanidine to the reactor, continue the reaction for 6 hours, and perform gas chromatography detection on the reaction liquid. After the reaction, p-phenylenediamine was not detected, and the final raw material conversion rate was 100%. The content of trans-1,4-cyclohexanedimethylamine was 86.5%; the content of cis-1,4-cyclohexanedimethylamine was 11.6%; and the polymer content was 1.6%.
[0005] The reactor used for the production of 1,4-cyclohexanedimethylamine is equipped with a tetramethylguanidine quantitative filling device. However, since the tetramethylguanidine is pre-stored in the quantitative filling device, the tetramethylguanidine is prone to agglomeration. The agglomerated tetramethylguanidine is not easy to react with the mixed liquid in the reactor after being added into the reactor, so long-term stirring is required, which reduces the production efficiency and conversion rate of 1,4-cyclohexanedimethylamine. Summary of the invention
[0006] The main purpose of the present invention is to provide a reactor for processing organic compounds, which can crush agglomerated tetramethylguanidine and then add it into a reactor, thereby improving the production efficiency and conversion rate of 1,4-cyclohexanedimethylamine.
[0007] In order to achieve the above object, the technical solution provided by the present invention is: A reaction kettle for processing organic compounds, comprising a kettle body, an upper cover fixed at the upper end of the kettle body, a hydrogenation pipe and a liquid inlet pipe fixed on the upper cover, a discharge pipe fixedly connected to the lower end of the kettle body, and a quantitative filling device connected to the kettle body fixed at the upper end of the upper cover; the quantitative filling device comprises a barrel connected to the inside of the kettle body at the lower end, a filter screen fixed in the barrel, a rotating tube arranged in the barrel, a rotating rod concentrically rotating and sealingly connected in the rotating tube, the upper ends of the rotating tube and the rotating rod both extending above the barrel, the rotating tube and the upper end of the barrel being movably sealed, and the upper ends of the rotating tube and the rotating rod being connected to the upper end of the barrel. The drive unit is connected, and the drive unit can make the rotating rod and the rotating tube rotate synchronously and the rotation directions of the rotating rod and the rotating tube are opposite. A first push plate is fixed on the rotating tube in the barrel, and a second push plate is fixed on the rotating rod in the barrel. The lower end of the first push plate and the lower end of the second push plate are in sliding contact with the upper end of the filter screen, and the first push plate and the second push plate are in sliding contact with the inner edge of the side wall of the barrel. The upper end of the drive unit is fixedly connected to the lower end of the telescopic rod, and the upper end of the telescopic rod is concentrically fixedly connected to the output shaft of the first motor. A bracket is fixed on the upper end of the barrel, and the first motor is fixed on the bracket.
[0008] Specifically, the upper end of the barrel is fixedly connected with a feeding pipe, the lower end of the barrel is fixed on the upper cover and connected with the interior of the kettle body, and a quantitative valve is installed in the lower pipe.
[0009] Specifically, a stirring rod is rotatably arranged in the kettle body, and a second motor capable of driving the stirring rod to rotate is fixed on the upper cover.
[0010] Specifically, the diameter of the lower part of the rotating rod is equal to the outer diameter of the rotating tube, the upper part of the rotating rod passes through the rotating tube, the upper end of the lower part of the rotating rod is rotatably sealed and connected to the lower end of the rotating tube, the lower end of the rotating rod is rotatably contacted with the upper end of the filter screen, the first push plate is rotatably contacted with the outer edge of the lower part of the rotating rod, and the second push plate is rotatably contacted with the outer edge of the rotating tube.
[0011] Specifically, the driving unit includes an inverted U-shaped frame, the lower end of the telescopic rod is fixedly connected to the upper end of the frame, the upper end of the rotating tube is rotatably connected to the lower end of the frame, the upper end of the rotating rod is rotatably connected to the upper end of the frame, a first bevel gear is concentrically fixed to the upper end of the rotating rod, a second bevel gear is concentrically fixed to the upper end of the rotating tube, the first bevel gear and the second bevel gear are arranged opposite to each other up and down, a third motor is fixed on the frame, a third bevel gear is concentrically fixed on the output shaft of the third motor, the third bevel gear is located between the first bevel gear and the second bevel gear, and the third bevel gear is meshed with the first bevel gear and the second bevel gear.
[0012] Specifically, a heating plate is fixed inside the side wall of the kettle body.
[0013] Specifically, valves are installed on the feeding pipe and the discharging pipe.
[0014] Compared with the prior art, the present invention has the following beneficial effects: 1. The first push plate and the second push plate can squeeze the material between them when rotating, and can break the agglomerated material in the barrel to facilitate the material to pass through the filter.
[0015] 2. When the material in the barrel is severely agglomerated, the first push plate and the second push plate move upward, rotate and then move downward. The first push plate and the second push plate can cut the agglomerated material in the barrel, and can pre-cut and crush the severely agglomerated material in the barrel, thereby improving the crushing efficiency of the agglomerated material in the barrel.
[0016] 3. When the first push plate and the second push plate rotate, the material in the barrel can be stirred, which can facilitate the material in the barrel to pass through the filter.
[0017] 4. During the rotation of the first push plate and the second push plate, the material adhering to the inner edge of the barrel side wall can be scraped off. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] Figure 1 This is a schematic diagram of the reactor.
[0019] Figure 2 Schematic diagram of the barrel.
[0020] Figure 3 A cross-sectional view of the barrel.
[0021] Figure 4 for Figure 3 Magnified view of area A.
[0022] Figure 5 for Figure 3 Magnified view of area B.
[0023] Figure 6 Schematic diagram of the rotating rod.
[0024] Figure 7 It is a schematic diagram of the connection between the rotating rod, the rotating tube, the first push plate and the second push plate.
[0025] Figure 8 It is a schematic diagram of the cross-sectional structure of the first push plate and the second push plate in the barrel.
[0026] Fig. 9 It is a schematic diagram of the first push plate and the second push plate squeezing the material in the barrel after rotating.
[0027] The names of the parts in the accompanying drawings are: 1. kettle body; 2. upper cover; 3. barrel; 4. bracket; 5. first motor; 6. second motor; 7. liquid inlet pipe; 8. hydrogenation pipe; 9. heating plate; 10. stirring rod; 11. discharge pipe; 12. first push plate; 13. filter screen; 14. feed pipe; 15. telescopic rod; 16. frame; 17. first bevel gear; 18. second bevel gear; 19. third bevel gear; 20. third motor; 21. rotating tube; 22. rotating rod; 23. second push plate; 24. feeding pipe; 25. quantitative valve. DETAILED DESCRIPTION
[0028] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.
[0029] like Figure 1-Figure 9 As shown, the reaction kettle for processing organic compounds comprises a kettle body 1 , and a heating plate 9 is fixed inside the side wall of the kettle body 1 .
[0030] An upper cover 2 is fixed to the upper end of the kettle body 1, a hydrogenation pipe 8 and a liquid inlet pipe 7 are fixed to the upper cover 2, a discharge pipe 11 is fixedly connected to the lower end of the kettle body 1, and valves are installed on the feed pipe 24 and the discharge pipe 11.
[0031] A stirring rod 10 is rotatably arranged in the kettle body 1 , and a second motor 6 capable of driving the stirring rod 10 to rotate is fixed on the upper cover 2 .
[0032] A quantitative filling device connected to the kettle body 1 is fixed on the upper end of the upper cover 2 .
[0033] The quantitative filling device includes a barrel 3 whose lower end is connected to the interior of the kettle body 1, and a feeding pipe 24 is fixedly connected to the upper end of the barrel 3. The discharge pipe 14 at the lower end of the barrel 3 is fixed on the upper cover 2 and connected to the interior of the kettle body 1, and a quantitative valve 25 is installed in the discharge pipe 14.
[0034] A filter screen 13 is fixed in the barrel 3. A rotating tube 21 is provided in the barrel 3. A rotating rod 22 is coaxially rotating and sealed in the rotating tube 21. The diameter of the lower part of the rotating rod 22 is equal to the outer diameter of the rotating tube 21. The upper part of the rotating rod 22 passes through the rotating tube 21. The upper end of the lower part of the rotating rod 22 is rotatably and sealedly connected to the lower end of the rotating tube 21. The lower end of the rotating rod 22 is in rotational contact with the upper end of the filter screen 13.
[0035] The upper ends of the rotating tube 21 and the rotating rod 22 extend above the barrel 3, and the rotating tube 21 is movably and sealedly connected to the upper end of the barrel 3. The upper ends of the rotating tube 21 and the rotating rod 22 are connected to a driving unit, and the driving unit can make the rotating rod 22 and the rotating tube 21 rotate synchronously and the rotation directions of the rotating rod 22 and the rotating tube 21 are opposite.
[0036] A first push plate 12 is fixed on the rotating tube 21 in the barrel 3, and a second push plate 23 is fixed on the rotating rod 22 in the barrel 3. The first push plate 12 is in rotational contact with the outer edge of the lower portion of the rotating rod 22, and the second push plate 23 is in rotational contact with the outer edge of the rotating tube 21. The lower end of the first push plate 12 and the lower end of the second push plate 23 are in sliding contact with the upper end of the filter screen 13, and the first push plate 12 and the second push plate 23 are in sliding contact with the inner edge of the side wall of the barrel 3.
[0037] The upper end of the driving unit is fixedly connected to the lower end of the telescopic rod 15 , the upper end of the telescopic rod 15 is fixedly connected to the output shaft of the first motor 5 concentrically, the upper end of the barrel 3 is fixed with a bracket 4 , and the first motor 5 is fixed on the bracket 4 .
[0038] The driving unit includes an inverted U-shaped frame 16, the lower end of the telescopic rod 15 is fixedly connected to the upper end of the frame 16, the upper end of the rotating tube 21 is rotatably connected to the lower end of the frame 16, the upper end of the rotating rod 22 is rotatably connected to the upper end of the frame 16, a first bevel gear 17 is concentrically fixed to the upper end of the rotating rod 22, a second bevel gear 18 is concentrically fixed to the upper end of the rotating tube 21, the first bevel gear 17 and the second bevel gear 18 are arranged opposite to each other up and down, a third motor 20 is fixed to the frame 16, a third bevel gear 19 is concentrically fixed to the output shaft of the third motor 20, the third bevel gear 19 is located between the first bevel gear 17 and the second bevel gear 18, and the third bevel gear 19 is meshed with the first bevel gear 17 and the second bevel gear 18.
[0039] When 1,4-cyclohexanedimethylamine is produced, tetramethylguanidine is added to the barrel 3 through the feeding pipe 24, and then the feeding pipe 24 is blocked. Paraphenylenediamine, toluene, liquid ammonia, and ruthenium catalyst are added to the kettle body 1 through the liquid inlet pipe 7. The second motor 6 is started, and the second motor 6 drives the stirring rod 10 to rotate, and the heating plate 9 is started to keep the temperature in the kettle body 1 between 100°C and 105°C. Hydrogen is added to the kettle body 1 through the hydrogenation pipe 8, and the pressure in the kettle body 1 is 5.0Mpa. Then the reaction liquid in the kettle body 1 is detected by the internal standard method.
[0040] When the internal standard content of p-phenylenediamine in the kettle body 1 is 2.0%, the first motor 5 is started and the quantitative valve 25 is opened, and the quantitative valve 25 can be opened to allow the tetramethylguanidine in the barrel 3 to be quantitatively discharged into the kettle body 1. Then the reaction is continued for 6 hours, and the reaction liquid is detected by gas chromatography.
[0041] When the tetramethylguanidine in the barrel 3 is agglomerated, the third motor 20 is started to make the third motor 20 rotate forward, and the third motor 20 rotates the first bevel gear 17 and the second bevel gear 18 through the third bevel gear 19. The rotating tube 21 and the rotating rod 22 rotate at the same time and in opposite directions, then the first push plate 12 and the second push plate 23 rotate in opposite directions. When the first push plate 12 and the second push plate 23 rotate in the barrel 3, the first push plate 12 and the second push plate 23 are close to each other, and the first push plate 12 and the second push plate 23 can squeeze the tetramethylguanidine between them, thereby squeezing and crushing the agglomerated tetramethylguanidine.
[0042] Then the third motor 20 is reversed, the first push plate 12 and the second push plate 23 move away from each other and then move closer to each other, and the first push plate 12 and the second push plate 23 can still squeeze the tetramethylguanidine between them. The third motor 20 is rotated forward and then reversed, and the first push plate 12 and the second push plate 23 can squeeze all the tetramethylguanidine in the barrel 3, so that the agglomerated tetramethylguanidine can be broken.
[0043] Then start the first motor 5, which causes the driving unit, the rotating rod 22, the rotating tube 21, the first push plate 12 and the second push plate 23 to rotate simultaneously through the telescopic rod 15. When the first push plate 12 and the second push plate 23 rotate in the barrel 3, the tetramethylguanidine in the barrel 3 can be stirred, so that the tetramethylguanidine can quickly pass through the filter 13 and enter the discharge pipe 14.
[0044] When the tetramethylguanidine in the barrel 3 is severely agglomerated, the telescopic rod 15 is started to make the driving unit, the rotating rod 22, the rotating tube 21, the first push plate 12 and the second push plate 23 move upward. When the lower ends of the first push plate 12 and the second push plate 23 are located above the tetramethylguanidine in the barrel 3, the first motor 5 is started to make the first motor 5 drive the telescopic rod 15, the driving unit, the rotating rod 22, the rotating tube 21, the first push plate 12 and the second push plate 23 to rotate a certain angle. Then the telescopic rod 15 is started to make the driving unit, the rotating rod 22, the rotating tube 21, the first push plate 12 and the second push plate 23 move downward. When the driving unit, the rotating rod 22, the rotating tube 21, the first push plate 12 and the second push plate 23 move downward, the first push plate 12 and the second push plate 23 can cut the tetramethylguanidine agglomerated in the barrel 3, thereby realizing pre-crushing of the tetramethylguanidine that is severely agglomerated in the barrel 3.
[0045] During the pre-crushing process of the severely agglomerated tetramethylguanidine in the barrel 3 , the first push plate 12 and the second push plate 23 can be moved upward, rotated and then moved downward for multiple times, thereby ensuring the pre-crushing effect of the agglomerated tetramethylguanidine in the barrel 3 .
[0046] During the rotation of the first push plate 12 and the second push plate 23 , tetramethylguanidine adhering to the inner edge of the side wall of the barrel 3 can be scraped off.
[0047] 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 and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.
Claims
1. A reaction kettle for processing organic compounds, comprising a kettle body (1), an upper cover (2) fixed to the upper end of the kettle body (1), a hydrogenation pipe (8) and a liquid inlet pipe (7) fixed to the upper cover (2), and a discharge pipe (11) fixedly connected to the lower end of the kettle body (1), characterized in that: A quantitative filling device connected to the kettle body (1) is fixed at the upper end of the upper cover (2); the quantitative filling device comprises a barrel (3) whose lower end is connected to the inside of the kettle body (1); a filter screen (13) is fixed in the barrel (3); a rotating tube (21) is arranged in the barrel (3); a rotating rod (22) is coaxially rotatably sealed in the rotating tube (21); the upper ends of the rotating tube (21) and the rotating rod (22) both extend above the barrel (3); the rotating tube (21) is movably sealed to the upper end of the barrel (3); the upper ends of the rotating tube (21) and the rotating rod (22) are connected to a driving unit; the driving unit can make the rotating rod (22) and the rotating tube (21) rotate synchronously and the rotating rod (22) rotate synchronously. In a direction opposite to the rotation direction of the rotating tube (21), a first push plate (12) is fixed on the rotating tube (21) in the barrel (3), a second push plate (23) is fixed on the rotating rod (22) in the barrel (3), the lower end of the first push plate (12) and the lower end of the second push plate (23) are in sliding contact with the upper end of the filter screen (13), the first push plate (12) and the second push plate (23) are in sliding contact with the inner edge of the side wall of the barrel (3), the upper end of the driving unit is fixedly connected to the lower end of the telescopic rod (15), the upper end of the telescopic rod (15) is fixedly connected to the output shaft of the first motor (5) concentrically, the upper end of the barrel (3) is fixedly connected to the bracket (4), and the first motor (5) is fixed on the bracket (4).
2. The organic compound processing reactor according to claim 1, characterized in that: The upper end of the barrel (3) is fixedly connected to a feeding pipe (24), the lower end of the barrel (3) is fixed to the upper cover (2) and connected to the interior of the kettle body (1), and a quantitative valve (25) is installed in the lower end of the barrel (14).
3. The organic compound processing reactor according to claim 1, characterized in that: A stirring rod (10) is rotatably arranged in the kettle body (1), and a second motor (6) capable of driving the stirring rod (10) to rotate is fixed on the upper cover (2).
4. The organic compound processing reactor according to claim 1, characterized in that: The diameter of the lower portion of the rotating rod (22) is equal to the outer diameter of the rotating tube (21), the upper portion of the rotating rod (22) penetrates the rotating tube (21), the upper end of the lower portion of the rotating rod (22) is rotatably sealed and connected to the lower end of the rotating tube (21), the lower end of the rotating rod (22) is in rotatable contact with the upper end of the filter screen (13), the first push plate (12) is in rotatable contact with the outer edge of the lower portion of the rotating rod (22), and the second push plate (23) is in rotatable contact with the outer edge of the rotating tube (21).
5. The organic compound processing reactor according to claim 1, characterized in that: The driving unit comprises an inverted U-shaped frame (16), the lower end of the telescopic rod (15) is fixedly connected to the upper end of the frame (16), the upper end of the rotating tube (21) is rotatably connected to the lower end of the frame (16), the upper end of the rotating rod (22) is rotatably connected to the upper end of the frame (16), the upper end of the rotating rod (22) is concentrically fixed with a first bevel gear (17), the upper end of the rotating tube (21) is concentrically fixed with a second bevel gear (18), the first bevel gear (17) and the second bevel gear (18) are arranged opposite to each other up and down, a third motor (20) is fixed on the frame (16), a third bevel gear (19) is concentrically fixed on the output shaft of the third motor (20), the third bevel gear (19) is located between the first bevel gear (17) and the second bevel gear (18), and the third bevel gear (19) is meshed with the first bevel gear (17) and the second bevel gear (18).
6. The organic compound processing reactor according to claim 1, characterized in that: A heating plate (9) is fixed inside the side wall of the kettle body (1).
7. The organic compound processing reactor according to claim 1, characterized in that: Valves are installed on the feeding pipe (24) and the discharging pipe (11).