Nitrogen replacement feeding device for adding triphenylphosphine
Through the nitrogen replacement feeding device, the problem of introduction of triphenylphosphine oxygen is solved, the activity and selectivity of the catalyst is maintained, and the efficiency and product quality of the carbonyl synthesis reaction are improved.
Patent Information
- Application Number
- CN202422790468.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-15
- Publication Date
- 2024-12-24
- Estimated Expiration
- 2034-11-15
AI Technical Summary
In the carbonyl synthesis reaction, the introduction of oxygen by triphenylphosphine will reduce the activity of the catalyst and affect the reaction efficiency, and it is difficult for the prior art to effectively reduce the amount of oxygen introduced.
A nitrogen replacement feeding device was designed to replace oxygen in the equipment through a nitrogen supply pipeline and an oxygen analyzer, ensuring the effective concentration of triphenylphosphine, and reducing the loss of triphenylphosphine through an aldehyde washing pipeline.
It effectively reduces the amount of oxygen introduced by triphenylphosphine during the supplementation process, maintains the activity and selectivity of the catalyst, and improves the efficiency of the reaction and product quality.
Smart Images
Figure CN222219537U_ABST
Abstract
Description
Technical Field
[0001] The utility model belongs to the technical field of chemical equipment, and in particular relates to a nitrogen replacement feeding device for adding triphenylphosphine. Background Art
[0002] In the carbonyl synthesis reaction process, triphenylphosphine, as a ligand of the catalyst, can combine with rhodium metal to form a stable complex, providing the required activity and selectivity for the reaction. As the reaction continues, the concentration of triphenylphosphine will gradually decrease, so it is necessary to add it regularly to maintain the effective concentration in the reaction system, ensure the continuation of the reaction, and maintain the high efficiency of the reaction.
[0003] However, in the operation process of adding triphenylphosphine, due to the influence of environmental factors or improper operation, a small amount of oxygen is often carried into the preparation tank among the triphenylphosphine powder. These oxygens react with triphenylphosphine to generate phosphine oxide, which not only significantly reduces the activity of the catalyst, but also has an adverse effect on the efficiency of subsequent reactions and the quality of the product. Therefore, reducing the amount of oxygen introduced into triphenylphosphine during the addition process is of great significance for ensuring the preparation quality of the catalyst. Utility Model Content
[0004] The utility model aims to provide a nitrogen replacement feeding device for adding triphenylphosphine, which reduces the amount of oxygen introduced into the triphenylphosphine during the addition process by nitrogen replacement, thereby maintaining the effective concentration of triphenylphosphine and ensuring the activity and selectivity of the catalyst in the carbonyl synthesis reaction.
[0005] To achieve the above purpose, the technical solution of the utility model is:
[0006] A nitrogen replacement feeding device for adding triphenylphosphine comprises a feeding port, a sealing cover is arranged at the top of the feeding port, a flushing pipeline is arranged at the upper side wall of the feeding port, an aldehyde washing pipeline and a nitrogen pipeline are arranged at one end of the flushing pipeline away from the feeding port, an oxygen analyzer is arranged at the lower side wall of the feeding port, a hopper is arranged at the bottom of the feeding port, a nitrogen supply pipeline and a vibrator are arranged on the side wall of the hopper, a flexible joint is arranged at the bottom opening of the hopper, an auger conveyor is connected below the flexible joint, a discharging pipeline is arranged at the bottom of one side of the auger conveyor away from the flexible joint, and a preparation tank is connected at one end of the discharging pipeline away from the auger conveyor.
[0007] in:
[0008] The top opening of the feeding port is arranged tilted.
[0009] The discharge pipeline is provided with a valve one, and the aldehyde washing pipeline is provided with a valve three.
[0010] The nitrogen pipeline is provided with a second valve, and the nitrogen supply pipeline is provided with a fourth valve.
[0011] The top of the auger conveyor is provided with an inspection port.
[0012] The material of the feeding port, the hopper and the preparation tank are all stainless steel.
[0013] The upper part of the hopper is a cylindrical barrel structure, and the lower part of the hopper is an inverted truncated cone funnel structure.
[0014] The nitrogen supply pipeline is arranged on the side wall of the cylinder at the upper part of the hopper, and the vibrator is arranged on the side wall of the funnel at the lower part of the hopper.
[0015] Both sides of the cylinder on the upper part of the hopper are equipped with supporting structures, and the supporting structures are located below the nitrogen supply pipeline.
[0016] A motor is arranged at one end of the auger conveyor, and a screw shaft is connected to the output end of the motor, and the screw shaft is arranged inside the auger conveyor.
[0017] The beneficial effects of the utility model are:
[0018] By setting up a nitrogen supply pipeline, nitrogen can be used to replace oxygen in the equipment, reducing the amount of oxygen introduced into triphenylphosphine during the addition process; by setting up an oxygen analyzer, the oxygen content of the equipment before and during the addition process can be detected at any time; by setting up an aldehyde washing pipeline, the residual triphenylphosphine can be flushed into the preparation tank to reduce the loss of triphenylphosphine. The device has a simple structure and is easy to operate. It can avoid the interference of oxygen, thereby maintaining the effective concentration of triphenylphosphine and ensuring the activity and selectivity of the catalyst in the carbonyl synthesis reaction. BRIEF DESCRIPTION OF THE DRAWINGS
[0019] Figure 1 It is a schematic diagram of the structure of the utility model;
[0020] In the figure:
[0021] 1. Feeding port; 2. Sealing cover; 3. Flushing pipeline; 4. Aldehyde washing pipeline; 5. Nitrogen pipeline; 6. Oxygen analyzer; 7. Hopper; 8. Nitrogen supply pipeline; 9. Vibrator; 10. Flexible joint; 11. Auger conveyor; 12. Discharge pipeline; 13. Preparation tank; 14. Valve one; 15. Valve three; 16. Valve two; 17. Valve four; 18. Inspection port; 19. Support structure. DETAILED DESCRIPTION
[0022] The present invention will be specifically described and illustrated below in conjunction with the embodiments.
[0023] Example 1
[0024] like Figure 1 As shown, the nitrogen displacement feeding device for adding triphenylphosphine described in the utility model comprises a feeding port 1, a sealing cover 2 is arranged on the top of the feeding port 1, a flushing pipeline 3 is arranged on the upper side wall of the feeding port 1, an aldehyde washing pipeline 4 and a nitrogen pipeline 5 are arranged on the end of the flushing pipeline 3 away from the feeding port 1, an oxygen analyzer 6 is arranged on the lower side wall of the feeding port 1, a hopper 7 is arranged at the bottom of the feeding port 1, a nitrogen supply pipeline 8 and a vibrator 9 are arranged on the side wall of the hopper 7, a flexible joint 10 is arranged at the bottom opening of the hopper 7, an auger conveyor 11 is connected below the flexible joint 10, a discharge pipeline 12 is arranged on the bottom of the side of the auger conveyor 11 away from the flexible joint 10, and a preparation tank 13 is connected to the end of the discharge pipeline 12 away from the auger conveyor 11.
[0025] The preparation tank 13 is used to store and prepare the catalyst in the carbonyl synthesis reaction; the feeding port 1 and the hopper 7 provide a passage for triphenylphosphine to enter the preparation tank 13; the nitrogen supply pipeline 8 is connected to a nitrogen source for providing high-purity nitrogen and blowing out oxygen through the feeding port 1 to replace the oxygen carried during the addition of triphenylphosphine; the oxygen analyzer 6 is used to detect the oxygen content of the equipment before and during the addition of triphenylphosphine; the aldehyde washing pipeline 4 is used to flush the residual triphenylphosphine powder into the preparation tank 13, and the nitrogen pipeline 5 is used to flush the residual aldehyde into the preparation tank 13; the flexible joint 10 is used to compensate for the displacement and deformation of the hopper 7 caused by the vibration of the vibrator 9, so as to ensure the stability and reliability of the connection; the auger conveyor 11 can realize the continuous and closed transportation of the triphenylphosphine powder from the hopper 7 to the preparation tank 13; the vibrator 9 can promote the transportation of the triphenylphosphine powder and avoid the hopper 7 from being blocked; the sealing cover 2 can be tightly covered on the feeding port 1 to prevent the outside air from entering the feeding port 1.
[0026] The top opening of the feeding port 1 is arranged to be inclined.
[0027] The discharge pipeline 12 is provided with a valve 14 , and the aldehyde washing pipeline 4 is provided with a valve 3 15 .
[0028] A valve two 16 is provided on the nitrogen pipeline 5, and a valve four 17 is provided on the nitrogen supply pipeline 8.
[0029] An inspection port 18 is provided at the top of the auger conveyor 11. The inspection port 18 is used to observe the flow of triphenylphosphine powder inside the auger conveyor 11 to avoid blockage and stagnation.
[0030] The materials of the feed port 1, the hopper 7 and the preparation tank 13 are all stainless steel.
[0031] The upper part of the hopper 7 is provided with a cylindrical barrel structure, and the lower part of the hopper 7 is provided with an inverted truncated cone-shaped funnel structure.
[0032] The nitrogen supply pipeline 8 is arranged on the side wall of the cylinder at the upper part of the hopper 7 , and the vibrator 9 is arranged on the side wall of the funnel at the lower part of the hopper 7 .
[0033] Support structures 19 are provided on both sides of the cylinder at the top of the hopper 7 , and the support structure 19 is located below the nitrogen supply pipeline 8 .
[0034] A motor is disposed at one end of the auger conveyor 11 , and a screw shaft is connected to an output end of the motor. The screw shaft is disposed inside the auger conveyor 11 .
[0035] Working process and principle:
[0036] 1. Preparation
[0037] Before the device is put into use, the mass of triphenylphosphine and aldehyde to be added is determined according to the concentration of triphenylphosphine in the preparation tank 13. Ensure that valve 1 14, valve 2 16, valve 3 15 and valve 4 17 are in a closed state, add the aldehyde to be added into the preparation tank 13 in advance, and maintain a slight positive pressure of nitrogen in the preparation tank 13 while adding aldehyde.
[0038] 2. Nitrogen replacement stage
[0039] Turn on the oxygen analyzer 6, open the sealing cover 2 and the valve 17 on the nitrogen supply pipeline 8, and continuously introduce nitrogen into the hopper 7 and the auger conveyor 11 to replace the oxygen inside the hopper 7 and the auger conveyor 11 with nitrogen.
[0040] 3. Triphenylphosphine addition stage
[0041] When the oxygen content value displayed by the oxygen analyzer 6 is lower than the specified value, the valve 14 on the discharge pipeline 12 is opened, the auger conveyor 11 and the vibrator 9 are started, the triphenylphosphine powder is slowly poured down from the feed port 1, the feed flow rate of the triphenylphosphine powder is controlled, and the opening of the valve 29 17 on the nitrogen supply pipeline 8 is adjusted at the same time, on the one hand, to avoid excessive nitrogen volume hindering the normal fall of the triphenylphosphine powder, and on the other hand, to avoid too little nitrogen volume leading to the inability to completely replace the oxygen carried by the triphenylphosphine powder. During the addition of the triphenylphosphine powder, it is ensured that a trace amount of nitrogen continues to flow at the top of the feed port 1, and at the same time, it is ensured that the oxygen content value displayed by the oxygen analyzer 6 is lower than the specified value.
[0042] During the process of adding triphenylphosphine to the preparation tank 13, the conveying of the triphenylphosphine powder can be observed through the inspection port 18 on the upper part of the auger conveyor 11. When there is too much triphenylphosphine powder adhering to the auger conveyor 11, the vibration frequency of the vibrator 9 can be increased or the feed amount of the triphenylphosphine powder from the feeding port 1 can be reduced.
[0043] 4. Flushing and purging stage
[0044] After all the triphenylphosphine powder is added to the preparation tank 13, the sealing cover 2 and the valve 4 17 are closed in sequence, and then the valve 3 15 on the aldehyde washing pipeline 4 is opened to flush the triphenylphosphine powder remaining in the hopper 7 and the auger conveyor 11 into the preparation tank 13 through the aldehyde.
[0045] After confirming that there is no residual triphenylphosphine in the auger conveyor 11 by observing through the inspection port 18, close the valve three 15 on the aldehyde washing pipeline 4, open the valve two 16 on the nitrogen pipeline 5, and use nitrogen to blow the aldehyde remaining in the hopper 7 and the auger conveyor 11 into the preparation tank 13. After the blowing is completed, close the valve one 14 and the valve two 16, and the addition of triphenylphosphine powder is completed.
Claims
1. A nitrogen displacement feeding device for adding triphenylphosphine, comprising a feeding port (1), characterized in that: A sealing cover (2) is provided at the top of the feeding port (1); a flushing pipeline (3) is provided at the upper side wall of the feeding port (1); an aldehyde washing pipeline (4) and a nitrogen pipeline (5) are provided at one end of the flushing pipeline (3) away from the feeding port (1); an oxygen analyzer (6) is provided at the lower side wall of the feeding port (1); a hopper (7) is provided at the bottom of the feeding port (1); a nitrogen supply pipeline (8) and a vibrator (9) are provided at the side wall of the hopper (7); a flexible joint (10) is provided at the bottom opening of the hopper (7); an auger conveyor (11) is connected below the flexible joint (10); a discharge pipeline (12) is provided at the bottom of the auger conveyor (11) away from the flexible joint (10); and a preparation tank (13) is connected at one end of the discharge pipeline (12) away from the auger conveyor (11).
2. The nitrogen replacement feeding device for adding triphenylphosphine according to claim 1, characterized in that: The top opening of the feeding port (1) is arranged to be inclined.
3. The nitrogen replacement feeding device for adding triphenylphosphine according to claim 1, characterized in that: The discharge pipeline (12) is provided with a valve one (14), and the aldehyde washing pipeline (4) is provided with a valve three (15).
4. The nitrogen replacement feeding device for adding triphenylphosphine according to claim 1, characterized in that: A second valve (16) is provided on the nitrogen pipeline (5), and a fourth valve (17) is provided on the nitrogen supply pipeline (8).
5. The nitrogen replacement feeding device for adding triphenylphosphine according to claim 1, characterized in that: An inspection port (18) is provided on the top of the auger conveyor (11).
6. The nitrogen replacement feeding device for adding triphenylphosphine according to claim 1, characterized in that: The material of the feeding port (1), the hopper (7) and the preparation tank (13) are all stainless steel.
7. The nitrogen replacement feeding device for adding triphenylphosphine according to claim 1, characterized in that: The upper part of the hopper (7) is provided with a cylindrical barrel structure, and the lower part of the hopper (7) is provided with an inverted truncated cone-shaped funnel structure.
8. The nitrogen displacement feeding device for adding triphenylphosphine according to claim 7, characterized in that: The nitrogen supply pipeline (8) is arranged on the side wall of the cylinder at the upper part of the hopper (7), and the vibrator (9) is arranged on the side wall of the funnel at the lower part of the hopper (7).
9. The nitrogen displacement feeding device for adding triphenylphosphine according to claim 8, characterized in that: Support structures (19) are provided on both sides of the cylinder at the top of the hopper (7), and the support structure (19) is located below the nitrogen supply pipeline (8).
10. The nitrogen replacement feeding device for adding triphenylphosphine according to claim 1, characterized in that: A motor is arranged at one end of the auger conveyor (11), and a screw shaft is connected to the output end of the motor. The screw shaft is arranged inside the auger conveyor (11).