Fixed bed for hydrogenation reduction
By using fixed bed technology and glass ball-filled bed design in hydrogenation reaction, the problems of long reaction time and low efficiency of traditional hydrogenation kettles are solved, and the equipment volume reduction, accelerated reaction rate and improved production efficiency are achieved.
Patent Information
- Application Number
- CN202421834709.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-31
- Publication Date
- 2025-05-06
- Estimated Expiration
- 2034-07-31
AI Technical Summary
In the production of (1r,4r)-1-methyl-4-(nitromethyl)cyclohexane-1-ol, the single batch operation and reaction time are too long, resulting in low production efficiency.
Instead of the traditional reactor, the fixed bed technology is used to separate it into multiple beds by exchange columns and partitions. The raw materials and hydrogen are dispersed and mixed through the mesh, and the bed is filled with glass spheres to improve the gas-liquid mixing efficiency.
Continuous feeding and reaction are achieved, the equipment volume is reduced, the reaction rate is accelerated, the production efficiency is improved, and the equipment safety and operation convenience are improved through designs such as insulation layer and pressure relief valve.
Smart Images
Figure CN222829597U_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the field of chemical engineering, and in particular to a fixed bed for hydrogenation reduction. Background Art
[0002] Bcl-2 gene (i.e. B cell lymphoma / leukemia-2 gene) is an oncogene, which has a significant inhibitory effect on cell apoptosis and is one of the most important oncogenes in cell apoptosis research. The development of Bcl-2 (key protein in the cell apoptosis pathway) selective inhibitors is one of the key means to conquer cancer. (1r,4r)-1-methyl-4-(nitromethyl)cyclohexane-1-ol is a key intermediate for the preparation of Bcl-2 (key protein in the cell apoptosis pathway) selective inhibitors, and the high-pressure hydrogenation reactor one-pot reduction method is generally used.
[0003] A general hydrogenation kettle includes a kettle body, a feed port is welded through one side of the upper surface of the kettle body, a pressure relief pipe is welded through the other side of the upper surface of the kettle body, a control box for controlling the operation of the kettle body is installed on one side of the kettle body, a discharge hopper is welded through the lower surface of the kettle body, an air inlet pipe is welded through the lower surface of the kettle body near the discharge hopper, a stirring motor is installed on the upper surface of the kettle body, and the lower end of the stirring motor is connected to a stirring paddle extending into the interior of the tank body.
[0004] When using a hydrogenation reactor to produce (1r, 4r)-1-methyl-4-(nitromethyl)cyclohexane-1-ol, the operation and reaction time of a single batch is generally more than 10 hours, which is too time-consuming and has low production efficiency. Utility Model Content
[0005] In order to improve the efficiency of producing (1r, 4r)-1-methyl-4-(nitromethyl)cyclohexane-1-ol, the present application provides a fixed bed for hydrogenation reduction.
[0006] The fixed bed for hydrogenation reduction provided in the present application adopts the following technical solution:
[0007] A fixed bed for hydrogenation reduction comprises a frame, wherein a vertically arranged exchange column is arranged on the frame, and a plurality of horizontal partitions are arranged in the exchange column, wherein the plurality of partitions are evenly distributed and spaced along the vertical direction of the exchange column, and a fixed bed layer for mixing raw materials is formed between adjacent partitions, and a plurality of mesh holes are evenly distributed on the partitions and penetrate the partitions along the vertical direction, and a hydrogen storage tank and a feeding tank are arranged on the frame, wherein the hydrogen storage tank is connected to the upper end of the exchange column through an air outlet pipe, and the feeding tank is connected to the upper end of the exchange column through a feeding pipe, and the lower end of the exchange column is connected to a discharge pipe, wherein a first valve for controlling the discharge of feed liquid is provided on the discharge pipe, and a receiving barrel is provided at the lower end of the discharge pipe.
[0008] By adopting the above technical scheme, the hydrogen in the hydrogen storage tank flows into the exchange column from the upper end of the exchange column through the outlet pipe, the raw material 1-methyl-4-(nitromethyl)cyclohexyl-3-ene-1-ol and the Crabtree catalyst are dissolved in the feeding tank and flow into the exchange column from the upper end of the exchange column through the feeding pipe, the exchange column is divided into multiple beds by partitions, the raw materials and hydrogen are dispersed in the multiple beds through the mesh to mix and react, and the materials after the reaction are flowed into the receiving barrel through the discharge pipe at the lower end of the exchange column. Compared with traditional equipment, this technology adopts a fixed bed to replace the traditional reactor to achieve continuous feeding and reaction, so that the volume of the equipment is reduced and the reaction speed is increased.
[0009] Optionally, the fixed bed layer is filled with glass balls, the cross-sectional size of the glass balls is larger than the mesh size, and the diameter of the glass balls is smaller than or equal to the vertical distance between two adjacent partitions.
[0010] This reaction is a reaction between gaseous hydrogen and liquid materials, and mixing is relatively difficult. By adopting the above technical solution, the glass balls filled in the bed can improve the gas-liquid mixing efficiency and increase the reaction rate.
[0011] Optionally, the material receiving barrel includes a barrel body and an end cover, the end cover is threadedly connected to the upper end of the barrel body, the upper end of the end cover is connected to a vertically upward connecting pipe, the lower end of the discharge pipe is sleeved on the connecting pipe, and a pressure relief valve is provided on the side wall of the barrel body.
[0012] This reaction requires a high degree of cleanliness for the equipment. The reaction will be inactivated when the internal environment of the exchange column comes into contact with air. By adopting the above technical solution, the reacted liquid flows from the discharge pipe through the connecting pipe into the barrel body. The end cover and the barrel body are threadedly connected to play a sealing role, thereby reducing the entry of air and maintaining the reaction activity in the exchange column. The liquid entering the barrel body will increase the pressure in the receiving barrel, and the setting of the pressure relief valve can balance the air pressure.
[0013] Optionally, a fastening strip is provided at the lower end of the discharge pipe, and the fastening strip is in a circular ring shape and is sleeved on the discharge pipe. Fastening plates are provided at both ends of the fastening strip, and the two fastening plates are vertically arranged to the fastening strip. When the fastening strip is sleeved on the discharge pipe, the two fastening plates are located on the outer ring surface, and a fastening bolt is provided on the fastening plate. The part of the rod of the fastening bolt that passes through the two fastening plates and is exposed is threadedly connected with a fastening nut.
[0014] By adopting the above technical solution, after the discharge pipe is sleeved on the connecting pipe, the fastening strip is formed into a ring and sleeved on the connection between the discharge pipe and the connecting pipe. After the fastening strip forms a ring, the two fastening plates are close to each other, and the rod of the fastening bolt passes through the two fastening plates and is threadedly connected and fixed with the fastening bolt. After the fastening plate is fixed, it drives the fastening strip to tighten the discharge pipe, thereby making the connection between the discharge pipe and the connecting pipe more stable.
[0015] Optionally, a detection tube is provided on the side wall of the discharge tube, the first valve is located above the detection tube, and a second valve for controlling the opening and closing of the detection tube is provided on the detection tube.
[0016] During continuous reaction, regular sampling is required to detect the reaction results. By adopting the above technical solution, the operator opens the second valve, and the material flows out from the discharge pipe through the detection pipe, so that the operator does not need to open the end cover to take samples from the barrel, thereby achieving the effect of convenient operation.
[0017] Optionally, a one-way valve is provided on the detection tube, and the flow direction of the one-way valve is from the discharge pipe to the end of the detection tube away from the discharge pipe, and the one-way valve is located between the second valve and the discharge pipe.
[0018] When sampling from the detection tube, air is prone to reflux into the exchange column and affect the activity of the reaction. By adopting the above technical solution, the setting of the one-way valve allows the liquid to flow out of the detection tube only, reducing the reflux of the liquid and air, thereby maintaining the reaction activity.
[0019] Optionally, the hydrogen storage tank and the gas outlet pipe are both coated with a thermal insulation layer.
[0020] When hydrogen is released from a hydrogen storage tank, the gas pressure drops and it absorbs heat, causing the temperature of the hydrogen storage tank and the outlet pipe to drop. Operators are easily injured when they touch the hydrogen storage tank and the outlet pipe with lower temperatures. By adopting the above technical solution, the insulation layer can slow down the temperature transfer between the hydrogen storage tank and the outlet pipe and the outside world, thereby protecting the operators.
[0021] Optionally, the air outlet pipe and the feeding pipe are provided with flow meters for measuring the flow of materials in the air outlet pipe and the feeding pipe.
[0022] By adopting the above technical solution, the flow meter is used to detect the flow rate of hydrogen and raw materials, which is convenient for operators to control the reaction process.
[0023] In summary, the present application includes at least one of the following beneficial technical effects:
[0024] 1. By replacing the traditional reactor with fixed bed technology, the reaction can be carried out continuously, the equipment volume can be reduced, and the reaction rate can be accelerated;
[0025] 2. Filling the bed with glass balls can increase the mixing uniformity of hydrogen and raw materials;
[0026] 3. An insulation layer is provided on the hydrogen storage tank and the outlet pipe to protect the operators. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] Figure 1It is a schematic diagram of the structure of a fixed bed for hydrogenation reduction in an embodiment of the present application.
[0028] Figure 2 It is a cross-sectional view of a fixed bed exchange column for hydrogenation reduction according to an embodiment of the present application.
[0029] Figure 3 This is a cross-sectional view of a hydrogen storage tank and an outlet pipe of a fixed bed for hydrogenation reduction in an embodiment of the present application.
[0030] Figure 4 It is a schematic structural diagram of a fixed bed material receiving barrel for hydrogenation reduction according to an embodiment of the present application.
[0031] Explanation of the reference numerals: 1. rack; 2. exchange column; 21. partition; 22. bed layer; 23. glass ball; 24. discharge pipe; 25. first valve; 26. detection tube; 27. one-way valve; 28. second valve; 29. mesh; 3. hydrogen storage tank; 31. outlet pipe; 32. insulation layer; 4. feeding tank; 41. feeding pipe; 5. collecting barrel; 51. barrel body; 52. end cover; 53. connecting pipe; 54. pressure relief valve; 6. fastening strip; 61. fastening plate; 62. fastening bolt; 63. fastening nut; 7. flow meter. DETAILED DESCRIPTION
[0032] The following is combined with Figure 1-4 This application is described in further detail.
[0033] The present application embodiment discloses a fixed bed for hydrogenation reduction. Figure 1 A fixed bed for hydrogenation reduction includes a frame 1, on which a vertical exchange column 2, a hydrogen storage tank 3 and a feeding tank 4 are fixed, the upper end of the hydrogen storage tank 3 is connected with an outlet pipe 31, the end of the outlet pipe 31 away from the hydrogen storage tank 3 is connected to the upper end of the exchange column 2, the lower end of the feeding tank 4 is connected with a feeding pipe 41, the end of the feeding pipe 41 away from the feeding tank 4 is connected to the upper end of the exchange column 2, and flow meters 7 for measuring the flow rate in the pipes are installed on the feeding pipe 41 and the outlet pipe 31.
[0034] Reference Figure 1 as well as Figure 2A plurality of horizontal partitions 21 are installed inside the exchange column 2. The plurality of partitions 21 are evenly distributed in the exchange column 2 along the vertical direction. A fixed bed layer 22 for mixing and reacting raw materials is formed between two adjacent partitions 21. A plurality of mesh holes 29 are evenly opened on the partition 21 and penetrate the partition 21 along the vertical direction to facilitate the flow of materials. The fixed bed layer 22 is filled with glass balls 23. The cross-sectional size of the glass balls 23 is larger than the size of the mesh holes 29, thereby reducing the occurrence of the glass balls 23 sliding off the partition 21. The setting of the glass balls 23 can improve the uniformity of mixing of the raw materials and play a role in increasing the reaction rate.
[0035] Reference Figure 3 The outlet pipe 31 and the hydrogen storage tank 3 are both wrapped with a heat-insulating layer 32, thereby reducing the possibility of operators being injured due to temperature drop when hydrogen is discharged.
[0036] Reference Figure 1 as well as Figure 4 The lower end of the exchange column 2 is connected with a downward discharge pipe 24, and a receiving barrel 5 is provided below the discharge pipe 24. The receiving barrel 5 includes a barrel body 51 and an end cover 52. The end cover 52 is threadedly connected to the upper end of the barrel body 51, and a vertical upward connecting pipe 53 is installed on the upper end of the end cover 52. The lower end of the discharge pipe 24 is sleeved on the connecting pipe 53, so that the feed liquid in the exchange column 2 can smoothly flow into the receiving barrel 5 for collection. A pressure relief valve 54 is installed on the outer wall of the barrel body 51 to maintain the pressure balance in the receiving barrel 5.
[0037] Reference Figure 4 A fastening strip 6 is provided at the connection between the discharge pipe 24 and the connecting pipe 53. The fastening strip 6 is annularly sleeved on the discharge pipe 24. Both ends of the fastening strip 6 are fixedly connected with fastening plates 61 perpendicular to the fastening strip 6. When the fastening strip 6 is sleeved on the discharge pipe 24, the two fastening plates 61 are located on the outer ring surface of the fastening strip 6. A fastening bolt 62 is provided on the fastening plate 61. The rod of the fastening bolt 62 passes through the two fastening plates 61 in sequence, and the exposed part is threadedly connected with a fastening nut 63. After the fastening plate 61 is fixed by the fastening bolt 62 and the fastening nut 63, the fastening strip 6 is driven to tighten the discharge pipe 24, so that the connection between the discharge pipe 24 and the connecting pipe 53 is more stable.
[0038] Reference Figure 4 A horizontal detection tube 26 is connected to the side wall of the discharge pipe 24, and a one-way valve 27 and a second valve 28 are installed in sequence on the detection tube 26 in the direction away from the discharge pipe 24. The flow direction of the one-way valve 27 is from the discharge pipe 24 to the end of the detection tube 26 away from the discharge pipe 24. The setting of the one-way valve 27 allows the liquid to flow out only from the detection tube 26, reducing the backflow of the liquid and air.
[0039] The implementation principle of a fixed bed for hydrogenation reduction in an embodiment of the present application is as follows: the hydrogen in the hydrogen storage tank 3 flows into the exchange column 2 from the upper end of the exchange column 2 through the outlet pipe 31, the raw material 1-methyl-4-(nitromethyl)cyclohexyl-3-ene-1-ol and the Crabtree catalyst are dissolved in the feeding tank 4 and flow into the exchange column 2 from the upper end of the exchange column 2 through the feeding pipe 41, the exchange column 2 is divided into a plurality of beds 22 by the partition 21, the raw material and the hydrogen are dispersed in the plurality of beds 22 through the mesh 29 to mix and react, the glass balls 23 filled in the bed 22 can improve the gas-liquid mixing efficiency, and the materials after the reaction are flowed into the receiving barrel 5 through the discharge pipe 24 at the lower end of the exchange column 2 for collection.
[0040] When sampling is required for testing, the operator opens the second valve 28. The one-way valve 27 on the test tube 26 allows the liquid to flow out of the test tube 26 only, thereby reducing the backflow of the liquid and air.
[0041] The above are all preferred embodiments of the present application, and the protection scope of the present application is not limited thereto. Therefore, any equivalent changes made according to the structure, shape, and principle of the present application should be included in the protection scope of the present application.
Claims
1. A fixed bed for hydrogenation reduction, characterized in that: The invention comprises a frame (1), wherein a vertically arranged exchange column (2) is provided on the frame (1), wherein a plurality of horizontal partitions (21) are provided in the exchange column (2), wherein the plurality of partitions (21) are evenly distributed and arranged at intervals along the vertical direction of the exchange column (2), wherein a fixed bed layer (22) for mixing raw materials is formed between adjacent partitions (21), wherein a plurality of mesh holes (29) are evenly distributed on the partitions (21) and penetrate the partitions (21) in the vertical direction, wherein a hydrogen storage tank (3) and a feeding tank (4) are provided on the frame (1), wherein the hydrogen storage tank (3) is connected to the upper end of the exchange column (2) through an outlet pipe (31), wherein the feeding tank (4) is connected to the upper end of the exchange column (2) through a feeding pipe (41), wherein a discharge pipe (24) is connected to the lower end of the exchange column (2), wherein a first valve (25) for controlling the discharge of feed liquid is provided on the discharge pipe (24), and a receiving barrel (5) is provided at the lower end of the discharge pipe (24).
2. A fixed bed for hydrogenation reduction according to claim 1, characterized in that: The fixed bed layer (22) is filled with glass balls (23), the cross-section of the glass balls (23) is larger than the mesh size (29), and the diameter of the glass balls (23) is smaller than or equal to the vertical distance between two adjacent partitions (21).
3. A fixed bed for hydrogenation reduction according to claim 1, characterized in that: The material receiving barrel (5) comprises a barrel body (51) and an end cover (52), wherein the end cover (52) is threadedly connected to the upper end of the barrel body (51), the upper end of the end cover (52) is connected to a connecting pipe (53) extending vertically upward, the lower end of the material discharging pipe (24) is sleeved on the connecting pipe (53), and a pressure relief valve (54) is provided on the side wall of the barrel body (51).
4. A fixed bed for hydrogenation reduction according to claim 3, characterized in that: A fastening strip (6) is provided at the lower end of the discharge pipe (24). The fastening strip (6) is annularly sleeved on the discharge pipe (24). Fastening plates (61) are provided at both ends of the fastening strip (6). The two fastening plates (61) are arranged perpendicular to the fastening strip (6). When the fastening strip (6) is sleeved on the discharge pipe (24), the two fastening plates (61) are located on the outer annular surface. A fastening bolt (62) is provided on the fastening plate (61). The exposed portion of the rod of the fastening bolt (62) passing through the two fastening plates (61) is threadedly connected with a fastening nut (63).
5. A fixed bed for hydrogenation reduction according to claim 1, characterized in that: A detection tube (26) is provided on the side wall of the discharge tube (24), the first valve (25) is located above the detection tube (26), and a second valve (28) for controlling the opening and closing of the detection tube (26) is provided on the detection tube (26).
6. A fixed bed for hydrogenation reduction according to claim 5, characterized in that: The detection tube (26) is provided with a one-way valve (27), the flow direction of the one-way valve (27) is from the discharge tube (24) to the end of the detection tube (26) away from the discharge tube (24), and the one-way valve (27) is located between the second valve (28) and the discharge tube (24).
7. A fixed bed for hydrogenation reduction according to claim 1, characterized in that: The hydrogen storage tank (3) and the gas outlet pipe (31) are both covered with a thermal insulation layer (32).
8. A fixed bed for hydrogenation reduction according to claim 1, characterized in that: The air outlet pipe (31) and the feeding pipe (41) are provided with a flow meter (7) for measuring the flow rate of the material in the air outlet pipe (31) and the feeding pipe (41).