A kind of methyl anthranilate production washing device
By introducing a neutralization tank, a centrifugal extractor, and a water washing tower into the production of methyl anthranilate, combined with stirring equipment and a packing layer, the problems of insufficient neutralization and poor water washing effect were solved, achieving efficient separation and purification.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- SHANDONG LISHUO PETROCHEMICAL CO LTD
- Filing Date
- 2025-08-07
- Publication Date
- 2026-07-03
AI Technical Summary
In the production process of methyl anthranilate, insufficient neutralization, long separation cycle, and poor water washing effect affect product purity.
The device, which includes a neutralization tank, a centrifugal extractor, and a water washing tower, combined with stirring equipment and a packing layer, achieves thorough mixing and separation of the reaction liquid and the sodium carbonate solution. The multi-stage centrifugal extractor and water distributor are used to increase the contact area between the two phases and improve the water washing efficiency.
It improves the efficiency and completeness of the neutralization reaction, shortens the separation cycle, and significantly enhances the washing effect and product purity.
Smart Images
Figure CN224443030U_ABST
Abstract
Description
Technical Field
[0001] This utility model belongs to the technical field of water washing equipment, specifically relating to a water washing device for the production of methyl anthranilate. Background Technology
[0002] In the production of methyl anthranilate, the product after esterification needs to be neutralized to remove residual acid and washed with water to remove salt and water-soluble impurities. The existing process has the following problems: the neutralized mixture mostly relies on natural sedimentation and stratification, resulting in insufficient neutralization and long separation cycles; the water washing process uses a stirred tank mixing method, which limits the contact area between the two phases, leading to poor washing effect and affecting the purity of subsequent products. Utility Model Content
[0003] Therefore, it is necessary to provide a washing apparatus for the production of methyl anthranilate to address the problems of the existing technology.
[0004] To solve the problems of the existing technology, the technical solution adopted by this utility model is as follows:
[0005] A washing apparatus for the production of methyl anthranilate includes a neutralization tank, a stirring device inside the neutralization tank, a liquid outlet pipe at the bottom of the neutralization tank connected to a centrifugal extractor, an organic phase outlet of the centrifugal extractor connected to a washing tower, a packing layer inside the washing tower, a water distributor above the packing layer, a drain pipe at the bottom of the washing tower connected to a centrifugal extractor, a conical inner distribution cylinder at the top of the neutralization tank, a circular outer cylinder outside the inner distribution cylinder, multiple liquid guide pipes connected to the neutralization tank evenly arranged at the bottom of the circular outer cylinder and the fixed position of the inner distribution cylinder, and an inlet pipe fixed at the top center of the circular outer cylinder, which is connected to a material inlet pipe and a sodium carbonate solution inlet pipe.
[0006] As a preferred embodiment, the stirring device includes a stirring shaft installed inside the neutralization tank, a stirrer mounted on the stirring shaft, and a stirring motor fixed to the top of the stirring shaft. The stirring motor drives the stirring shaft and the stirrer to rotate, which can fully stir the materials in the neutralization tank, further mix the reaction liquid with the sodium carbonate solution, and ensure that the neutralization reaction proceeds completely.
[0007] As a preferred embodiment, the neutralization tank is equipped with a pH sensor, and an insulating jacket is installed on the outside of the tank. An insulating inlet pipe is located at the bottom of the jacket, and an insulating outlet pipe is located at the top. A temperature sensor is installed inside the tank. This allows for real-time monitoring of the pH value of the solution within the neutralization tank, facilitating timely adjustment of the amount of sodium carbonate solution added to ensure optimal neutralization reaction results. The temperature control medium is introduced into the insulating jacket through the insulating inlet pipe and then discharged through the insulating outlet pipe, maintaining a stable reaction temperature within the neutralization tank and reducing viscosity.
[0008] As a preferred embodiment, the washing tower has at least two layers of packing material. Each layer has a supporting mesh plate at its bottom and a water distributor at its top. Multiple water distributors are connected to inlet pipes. Water is supplied to the water distributors through the inlet pipes, and the water distributors spray the washing water evenly onto the packing layer, ensuring full contact between the washing water and the organic phase on the packing layer, thereby improving the washing effect.
[0009] As a preferred embodiment, a liquid distribution ring pipe is fixed on the outer wall of the water washing tower between each packing layer and the water distributor. Multiple inclined delivery pipes connecting to the water washing tower are uniformly fixed to the bottom of the liquid distribution ring pipe. The liquid distribution ring pipe is connected to a second liquid guide pipe, which in turn connects to a first centrifugal extractor. The organic phase separated by the first centrifugal extractor enters the liquid distribution ring pipe through the second liquid guide pipe, and is then inclinedly fed into the water washing tower through the delivery pipes. This allows the organic phase to be more evenly distributed above the packing layer, ensuring sufficient contact with the washing water.
[0010] As a preferred embodiment, a reinforcing rod is fixed to the top of the inner distribution cylinder, and the top of the reinforcing rod is fixed to the circular outer cylinder. The reinforcing rod has a hollow structure, with both ends penetrating through the circular outer cylinder and the inner distribution cylinder, respectively. The reinforcing rod enhances the connection strength between the inner distribution cylinder and the circular outer cylinder, while the hollow structure allows for cable routing and ventilation.
[0011] As a preferred option, the material inlet pipe and the sodium carbonate solution inlet pipe are symmetrically and inclined on the liquid inlet pipe. This installation method allows the reaction liquid and sodium carbonate solution to be initially mixed after entering the liquid inlet pipe, and then enter the space between the inner distribution cylinder and the outer circular cylinder, further improving the mixing effect.
[0012] The advantages of this utility model compared with the prior art are:
[0013] By setting a conical inner distribution cylinder and a circular outer cylinder at the top of the neutralization tank, as well as multiple liquid guide pipes, the reaction liquid and sodium carbonate solution can be fully mixed and evenly distributed before entering the neutralization tank. Combined with the stirring action of the stirring equipment, the efficiency and completeness of the neutralization reaction are greatly improved. Two-stage centrifugal extractors are used to separate the neutralized mixture and the washed mixture respectively, using a high separation factor to achieve rapid separation and improve separation efficiency. The water washing uses a packed water washing tower with a water distributor, which significantly increases the contact area between the two phases and improves the water washing efficiency. Attached Figure Description
[0014] Figure 1 This is a schematic diagram of the structure of this utility model;
[0015] Figure 2 yes Figure 1 Partial structural diagram Figure 1 ;
[0016] Figure 3 yes Figure 1 Partial structural diagram Figure 2 ;
[0017] The numbers on the map are:
[0018] 1. Material inlet pipe; 2. Sodium carbonate solution inlet pipe; 3. Liquid inlet pipe; 4. Circular outer cylinder; 5. Distribution inner cylinder; 6. Liquid guide pipe one; 7. Stirring motor; 8. Stirring shaft; 9. Insulation jacket; 10. Stirrer; 11. Neutralization tank; 12. Centrifugal extractor one; 13. Liquid guide pipe two; 14. Liquid outlet pipe; 15. Water washing tower; 16. Water inlet pipe; 17. Water distributor; 18. Liquid delivery pipe; 19. Packing layer; 20. Liquid distribution ring pipe; 21. Support mesh plate; 22. Drain pipe; 23. Centrifugal extractor two. Detailed Implementation
[0019] To further understand the features, technical means, and specific objectives and functions achieved by this utility model, the following detailed description of this utility model is provided in conjunction with the accompanying drawings and specific embodiments.
[0020] Example 1, Reference Figures 1 to 3 A washing apparatus for the production of methyl anthranilate includes a neutralization tank 11, a stirring device inside the neutralization tank 11, a liquid outlet pipe 14 at the bottom of the neutralization tank 11, a centrifugal extractor 12 connected to the liquid outlet pipe 14, an organic phase outlet of the centrifugal extractor 12 connected to a washing tower 15, a packing layer 19 inside the washing tower 15, a water distributor 17 above the packing layer 19, a drain pipe 22 at the bottom of the washing tower 15, a centrifugal extractor 23 connected to the drain pipe 22, a conical inner distribution cylinder 5 at the top of the neutralization tank 11, a circular outer cylinder 4 outside the inner distribution cylinder 5, a plurality of liquid guide pipes 6 evenly arranged at the bottom of the circular outer cylinder 4 and the fixed position of the inner distribution cylinder 5, connecting to the neutralization tank 11, and an inlet pipe 3 fixed in the middle of the top of the circular outer cylinder 4, with a material inlet pipe 1 and a sodium carbonate solution inlet pipe 2 connected to the inlet pipe 3.
[0021] During operation, the methyl anthranilate reaction solution enters the inlet pipe 3 through the material inlet pipe 1, while the sodium carbonate solution also enters the inlet pipe 3 through the sodium carbonate solution inlet pipe 2. The two fluids initially mix by opposing current within the inlet pipe 3, and then flow together into the annular space between the outer cylindrical cylinder 4 and the inner distribution cylinder 5. The mixture flows downwards along the conical outer wall of the inner distribution cylinder 5 within the annular space, further homogenizing during the process, and then disperses into the neutralization tank 11 through the liquid guide pipe 6. At this point, the stirring equipment is activated to continuously agitate the mixture in the neutralization tank 11, ensuring full contact between the reaction solution and the sodium carbonate solution and triggering a neutralization reaction.
[0022] The neutralized mixture enters the centrifugal extractor 12 through the outlet pipe 14, where the organic phase and aqueous phase are initially separated under centrifugal force. The separated organic phase enters the water washing tower 15 through the liquid guide pipe 13, and the washing water enters the water distributor 17. After being atomized by the water distributor 17, it is evenly sprayed onto the surface of the packing layer 19 and comes into contact with the mixture on the packing layer 19. Through mass transfer, the salt and water-soluble impurities in the organic phase are removed.
[0023] The mixture after washing (organic phase and washing water) is collected at the bottom of the washing tower 15 and enters the centrifugal extractor 23 through the drain pipe 22. The organic phase and washing water are deeply separated by high-speed centrifugation, and finally methyl anthranilate organic phase is obtained. The washing wastewater is discharged from the water phase outlet of the centrifugal extractor 23.
[0024] In Example 2, based on Example 1, the stirring device includes a stirring shaft 8 disposed inside the neutralization tank 11, a stirrer 10 mounted on the stirring shaft 8, and a stirring motor 7 fixed to the top of the stirring shaft 8. The stirring motor 7 rotates at a speed of 60-120 r / min.
[0025] A pH sensor is installed inside the neutralization tank 11. An insulation jacket 9 is installed on the outside of the neutralization tank 11. An insulated liquid inlet pipe is located at the bottom of the insulation jacket 9, and an insulated liquid outlet pipe is located at the top of the insulation jacket 9. A temperature sensor is installed inside the neutralization tank 11. The insulation jacket 9 on the outside of the neutralization tank 11 maintains a stable temperature inside the tank by introducing a temperature control medium, such as hot water. The temperature sensor inside the tank monitors the temperature in real time and controls it at 40-50℃; simultaneously, the pH sensor monitors the pH value of the solution and controls it at 7.0-7.5 to ensure complete neutralization. The temperature sensor monitors and transmits the data to a PLC controller in real time. The PLC controller is connected to the pH sensor.
[0026] The washing tower 15 has at least two layers of packing material 19. Each layer has a supporting mesh plate 21 at its bottom and a water distributor 17 above it. Multiple water distributors 17 are connected to inlet pipes 16. A 10% sodium carbonate solution enters through the sodium carbonate solution inlet pipe 2. The water distributor 17 is a lotus-shaped washing water distributor. The specific surface area of the packing material in the packing layer 19 is 250-350 m² / g. 2 / m 3 .
[0027] Each layer of packing 19 and the water distributor 17 has a liquid distribution ring pipe 20 fixed on the outer wall of the water washing tower 15. Multiple inclined delivery pipes 18, connecting to the water washing tower 15, are evenly fixed to the bottom of the liquid distribution ring pipe 20. The liquid distribution ring pipe 20 is connected to a second liquid guide pipe 13, which is connected to a centrifugal extractor 12. The organic phase entering through the second liquid guide pipe 13 enters the liquid distribution ring pipe 20, and then evenly enters the water washing tower 15 through the delivery pipes 18, distributing more evenly on the packing layer 19. Liquid pumps can be installed on the outlet pipe 14 and the second liquid guide pipe 13 as needed.
[0028] A reinforcing rod is fixed to the top of the inner distribution cylinder 5. The top of the reinforcing rod is fixed to the circular outer cylinder 4. The reinforcing rod has a hollow structure, and its two ends pass through the circular outer cylinder 4 and the inner distribution cylinder 5, respectively. The connection between the reinforcing rod and the circular outer cylinder 4 and the inner distribution cylinder 5 is sealed by welding.
[0029] Material inlet pipe 1 and sodium carbonate solution inlet pipe 2 are symmetrically and obliquely installed on liquid inlet pipe 3.
[0030] The above embodiments only illustrate one or more implementations of this utility model, and their descriptions are relatively specific and detailed, but they should not be construed as limiting the scope of this utility model patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this utility model, and these all fall within the protection scope of this utility model. Therefore, the protection scope of this utility model patent should be determined by the appended claims.
Claims
1. A washing apparatus for the production of methyl anthranilate, comprising a neutralization tank (11), wherein a stirring device is provided inside the neutralization tank (11), and a liquid outlet pipe (14) is provided at the bottom of the neutralization tank (11), characterized in that: The outlet pipe (14) is connected to a centrifugal extractor (12). The organic phase outlet of the centrifugal extractor (12) is connected to a water washing tower (15). The water washing tower (15) is equipped with a packing layer (19). A water distributor (17) is provided above the packing layer (19). The bottom of the water washing tower (15) is equipped with a drain pipe (22). The drain pipe (22) is connected to a centrifugal extractor (23). The top of the neutralization tank (11) is equipped with a conical inner cylinder (5). The outer side of the inner cylinder (5) is equipped with a circular outer cylinder (4). The bottom of the circular outer cylinder (4) and the fixed part of the inner cylinder (5) are evenly equipped with multiple liquid guide pipes (6) that connect to the neutralization tank (11). The top middle of the circular outer cylinder (4) is fixed with an inlet pipe (3). The inlet pipe (3) is connected to a material inlet pipe (1) and a sodium carbonate solution inlet pipe (2).
2. A methylanaline production washing device according to claim 1, characterized in that, The mixing equipment includes a mixing shaft (8) installed in a neutralization tank (11), a stirrer (10) is provided on the mixing shaft (8), and a stirring motor (7) is fixed on the top of the mixing shaft (8).
3. A methylanaline production washing device according to claim 1, characterized in that, A pH sensor is installed inside the neutralization tank (11), and an insulation jacket (9) is installed on the outside of the neutralization tank (11). An insulation inlet pipe is installed at the bottom of the insulation jacket (9), and an insulation outlet pipe is installed at the top of the insulation jacket (9). A temperature sensor is installed inside the neutralization tank (11).
4. A methylanaline production washing device according to claim 1, characterized in that, The water washing tower (15) has at least two layers of packing layer (19), each packing layer (19) has a support mesh plate (21) at the bottom, and each packing layer (19) has a water distributor (17) above it. Multiple water distributors (17) are connected to water inlet pipes (16).
5. A methylanaline production washing device according to claim 4, characterized in that, Each packing layer (19) and the water distributor (17) is connected to a liquid distribution ring pipe (20) on the outer wall of the water washing tower (15). Multiple inclined liquid delivery pipes (18) connecting the water washing tower (15) are uniformly fixed at the bottom of the liquid distribution ring pipe (20). The liquid distribution ring pipe (20) is connected to a liquid guide pipe (23), which is connected to a centrifugal extractor (12).
6. A methylanaline production washing device according to claim 1, characterized in that, A reinforcing rod is fixed to the top of the inner cylinder (5). The top of the reinforcing rod is fixed to the outer cylinder (4). The reinforcing rod has a hollow structure, and the two ends of the reinforcing rod pass through the outer cylinder (4) and the inner cylinder (5) respectively.
7. A methylanaline production washing device according to claim 1, characterized in that, The material inlet pipe (1) and the sodium carbonate solution inlet pipe (2) are symmetrically and obliquely installed on the liquid inlet pipe (3).