Process for the separation of o-phenylenediamine from production wastewater

By rotating the filter frame and stirring rod structure, combined with magnetic adsorption and a guide plate design, the problem of filter frame clogging in the o-phenylenediamine separation process is solved, achieving efficient impurity cleaning and o-phenylenediamine extraction.

CN118108362BActive Publication Date: 2025-11-11ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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Patent Information

Application Number
CN202410243296.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-03-04
Publication Date
2025-11-11
Estimated Expiration
2044-03-04

AI Technical Summary

Technical Problem

In existing o-phenylenediamine separation processes, impurities and particles easily clog the filter screen during wastewater filtration, resulting in poor filtration performance.

Method used

The system employs a rotating filter frame and stirring rod structure, combined with magnetic adsorption and a guide plate design, to achieve directional movement and automatic discharge of impurities and particles, avoiding clogging, and extracting o-phenylenediamine using organic solvents.

Benefits of technology

It effectively avoids filter clogging, improves filtration efficiency, and achieves timely removal of impurities through centrifugal force and magnetic adsorption, enhancing the stirring effect and improving the extraction efficiency of o-phenylenediamine.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention discloses a separation process for o-phenylenediamine in production wastewater, relating to the field of o-phenylenediamine recovery technology from wastewater. The separation process includes the following steps: Step 1: Wastewater is poured into a separation device from a first feed pipe, and impurities and solid particles in the wastewater are removed by a rotating filter frame; Step 2: Organic solvent is added to the separation device from a second feed pipe, and then heated to 80-90°C to extract o-phenylenediamine from the wastewater; Step 3: Through crystallization, o-phenylenediamine is precipitated from the organic solvent, and the obtained o-phenylenediamine crystals are dried to remove residual solvent, resulting in dried o-phenylenediamine product. This allows different positions on the filter frame to receive wastewater falling from the first feed pipe and achieve wastewater filtration, thus preventing impurities and particles from accumulating at a certain position on the top of the filter frame, thereby reducing the phenomenon of filter frame clogging.
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Description

Technical Field

[0001] This invention relates to the field of o-phenylenediamine recovery technology from wastewater, specifically a separation process for o-phenylenediamine in production wastewater. Background Technology

[0002] o-Phenylenediamine is an organic compound and an important chemical raw material, commonly used in the production of dyes, rubber, resins, and polyamide fibers. In addition, o-Phenylenediamine is also used as an antioxidant and a pharmaceutical intermediate.

[0003] o-Phenylenediamine is a toxic compound that is harmful to the environment and human health. In order to reduce environmental pollution and protect the ecological environment and human health, o-Phenylenediamine usually needs to be separated from wastewater.

[0004] Existing o-phenylenediamine separation processes require wastewater pretreatment, specifically using filters to remove impurities and particles. However, during filtration, the wastewater continuously falls from a certain position at the top of the filter, easily clogging the filter and resulting in poor filtration efficiency. Therefore, this invention provides a process for separating o-phenylenediamine from production wastewater. Summary of the Invention

[0005] The technical problem solved by this invention is that the existing o-phenylenediamine separation process requires pretreatment of wastewater, specifically by using a filter screen to remove impurities and particles from the wastewater. However, during the filtration process, the wastewater falls from a certain position at the top of the filter screen, and impurities and particles easily clog the filter screen, resulting in poor filtration effect.

[0006] This invention can be achieved through the following technical solution: a separation process for o-phenylenediamine in production wastewater, the separation process comprising the following steps:

[0007] Step 1: Pour the wastewater into the separation device from the first feed pipe, and remove impurities and solid particles from the wastewater by passing through the rotating filter frame;

[0008] Step 2: Add the organic solvent into the separation unit through the second feed pipe, and then heat it to 80-90℃ to extract o-phenylenediamine from the wastewater; the organic solvents commonly used are p-xylene or chlorinated hydrocarbons.

[0009] Step 3: The o-phenylenediamine is precipitated from the organic solvent through crystallization. The obtained o-phenylenediamine crystals are then dried to remove residual solvent, resulting in a dried o-phenylenediamine product.

[0010] A further technical improvement of the present invention is that: the separation device includes a separation tank, a first rod is rotatably connected through the top of the separation tank, the first rod is driven by a motor, and a filter frame and a stirring rod are arranged sequentially from top to bottom on the outer wall of the first rod. The filter frame is used to remove impurities and solid particles from the wastewater, and the stirring rod is used to stir the wastewater and organic solvent. A first feed pipe is provided at the top of the separation tank for adding wastewater into the separation tank, and a second feed pipe is provided on the side wall of the separation tank for adding organic solvent into the separation tank, with the bottom end of the second feed pipe located below the filter frame.

[0011] A further technical improvement of the present invention is that: a first discharge trough is provided on one side of the filter frame, a second discharge trough is provided on one side of the separation barrel, and the area of ​​the first discharge trough is smaller than that of the second discharge trough; a baffle is slidably connected through the top of the filter frame, and a first magnet is fixedly connected to the top of the baffle; the bottom of the baffle is located in the first discharge trough; a second magnet is fixedly connected to the inner wall of the separation barrel, and the second magnet is located diagonally above the second discharge trough.

[0012] A further technical improvement of the present invention is that: a guide plate is fixedly and inclinedly connected to the bottom of the second discharge trough, a support plate is fixedly connected to the outer wall of the separation barrel, a collection shell is placed on the top of the support plate, and the bottom of the guide plate is located above the collection shell.

[0013] A further technical improvement of the present invention is that a first spring is fixed between the first magnet and the top of the filter frame, and the first spring is used to reset the baffle.

[0014] A further technical improvement of the present invention is that: a ball bearing is rotatably provided at the bottom of the filter frame, and an annular plate is fixedly connected to the inner wall of the separation barrel, and the ball bearing rolls on the annular plate.

[0015] A further technical improvement of the present invention is that: one end of the stirring rod is rotatably disposed on the side wall of the first rod, a sleeve is sleeved and slidably connected to the outside of the first rod, a through groove is opened on the outer wall of the sleeve, one end of the stirring rod passes through the through groove, a straight rod is fixedly connected to the outer wall of the sleeve, and the straight rod is located below the stirring rod, and the straight rod is used to push the stirring rod upward.

[0016] A further technical improvement of the present invention is that: the top of the sleeve is an inclined surface; a second rod is fixedly connected to the inner wall of the top of the separating barrel; when the first rod rotates, the bottom end of the second rod slides on the top of the sleeve; a circular plate is fixedly connected to the bottom end of the first rod; a bellows is fixedly connected to the bottom of the sleeve, and the bottom end of the bellows is fixedly connected to the top of the circular plate; a second spring is also fixedly connected between the sleeve and the circular plate.

[0017] A further technical improvement of the present invention is that: an elastic waterproof cloth is fixedly connected to the opening of the through groove, and the stirring rod passes through and is fixedly connected to the elastic waterproof cloth.

[0018] A further technical improvement of the present invention is that an electric heating plate is fixedly connected to the bottom inner wall of the separation tank.

[0019] Compared with the prior art, the present invention has the following beneficial effects:

[0020] 1. In this invention, when the motor drives the first rod and the filter frame to rotate, different positions of the filter frame can receive wastewater falling from the first feed pipe and filter the wastewater. This avoids the accumulation of impurities and particles at a certain position on the top of the filter frame, thereby reducing the phenomenon of filter frame blockage.

[0021] 2. In this invention, due to the centrifugal force, impurities and particles will move away from the center of the first rod. When the first magnet moves to the bottom of the second magnet, the first magnet will move upward and attract together with the second magnet. At this time, the first discharge chute is open, which facilitates the discharge of impurities and particles from the first discharge chute and along the guide plate, and finally falls into the collection shell. This facilitates the timely cleaning of impurities inside the filter frame and reduces the overall weight of the first rod and the filter frame.

[0022] 3. In this invention, when the motor drives the first rod to rotate, the first rod will drive the sleeve to rotate together. At this time, the second rod will squeeze the sleeve. With the action of the second spring, the sleeve will slide up and down along the first rod, which will allow the straight rod to squeeze the stirring rod, so that the stirring rod can swing up and down, thereby increasing the stirring range of the stirring rod and facilitating the thorough and uniform mixing of wastewater and organic solvent. Attached Figure Description

[0023] To facilitate understanding by those skilled in the art, the present invention will be further described below with reference to the accompanying drawings.

[0024] Figure 1 This is a process flow diagram of the present invention;

[0025] Figure 2 This is a partial cross-sectional structural diagram of the separation device in this invention;

[0026] Figure 3 For the present invention Figure 2 A magnified view of a section at point A in the middle;

[0027] Figure 4 For the present invention Figure 2 A magnified view of a section at point B in the middle;

[0028] Figure 5 For the present invention Figure 2A magnified view of a section at point C.

[0029] In the diagram: 1. Separation tank; 2. Rod No. 1; 3. Filter frame; 4. Stirring rod; 5. First feed pipe; 6. Second feed pipe; 7. First discharge chute; 8. Second discharge chute; 9. Baffle; 10. First magnet; 11. Second magnet; 12. Guide plate; 13. Support plate; 14. Collection shell; 15. First spring; 16. Ball bearing; 17. Annular plate; 18. Sleeve; 19. Through groove; 20. Straight rod; 21. Rod No. 2; 22. Circular plate; 23. Corrugated pipe; 24. Second spring; 25. Elastic waterproof cloth. Detailed Implementation

[0030] To further illustrate the technical means and effects of the present invention in achieving its intended purpose, the following detailed description of the specific implementation methods, structures, features, and effects of the present invention, in conjunction with the accompanying drawings and preferred embodiments, is provided.

[0031] Please see Figures 1-5 As shown, a process for separating o-phenylenediamine from production wastewater includes the following steps:

[0032] Step 1: Pour the wastewater into the separation device from the first feed pipe 5, and remove impurities and solid particles from the wastewater by passing through the rotating filter frame 3;

[0033] Step 2: Add the organic solvent into the separation device through the second feed pipe 6, and then heat it to 80-90℃ to extract o-phenylenediamine from the wastewater; the organic solvent is usually p-xylene or chlorinated hydrocarbons.

[0034] Step 3: The o-phenylenediamine is precipitated from the organic solvent through crystallization. The obtained o-phenylenediamine crystals are then dried to remove residual solvent, resulting in a dried o-phenylenediamine product.

[0035] In the above, the separation device includes a separation tank 1, with a rod 2 rotatably connected through and to the top of the separation tank 1. The rod 2 is driven by a motor, which is fixedly installed on the top of the separation tank 1. The output shaft of the motor is fixedly connected to the top of the rod 2. A filter frame 3 and a stirring rod 4 are arranged sequentially from top to bottom on the outer wall of the rod 2. The filter frame 3 is used to remove impurities and solid particles from the wastewater, and the stirring rod 4 is used to stir the wastewater and organic solvent. An electric heating plate is fixedly connected to the inner wall of the bottom of the separation tank 1. The electric heating plate is used to heat the mixture.

[0036] Specifically, a first feed pipe 5 is provided at the top of the separation tank 1, which is used to add wastewater into the separation tank 1. A second feed pipe 6 is provided on the side wall of the separation tank 1, which is used to add organic solvents into the separation tank 1. The bottom end of the second feed pipe 6 is located below the filter frame 3.

[0037] Furthermore, a first discharge trough 7 is provided on one side of the filter frame 3, and a second discharge trough 8 is provided on one side of the separation barrel 1. The area of ​​the first discharge trough 7 is smaller than that of the second discharge trough 8. A baffle 9 is slidably connected through the top of the filter frame 3, and a first magnet 10 is fixedly connected to the top of the baffle 9. The bottom of the baffle 9 is located inside the first discharge trough 7. A second magnet 11 is fixedly connected to the inner wall of the separation barrel 1, and the second magnet 11 is located obliquely above the second discharge trough 8. A guide plate 12 is obliquely fixedly connected to the bottom of the second discharge trough 8. A support plate 13 is fixedly connected to the outer wall of the separation barrel 1. A collection shell 14 is placed on the top of the support plate 13, and the bottom of the guide plate 12 is located above the collection shell 14.

[0038] During operation, when the motor drives the first rod 2 and the filter frame 3 to rotate, different positions of the filter frame 3 can receive wastewater falling from the first feed pipe 5 and filter the wastewater. This prevents impurities and particles from accumulating at a certain position on the top of the filter frame 3, thereby reducing the phenomenon of clogging of the filter frame 3. As the motor rotates, due to the centrifugal force, impurities and particles will move away from the center position of the first rod 2. When the first magnet 10 moves to the bottom of the second magnet 11, the first magnet 10 will move upward and attract together with the second magnet 11. At this time, the first discharge trough 7 is in the open state, which facilitates the discharge of impurities and particles from the first discharge trough 7 and along the guide plate 12, and finally falls into the collection shell 14. As the first rod 2 rotates further, the first magnet 10 will leave the second magnet 11. Under the gravity of the baffle 9, the baffle 9 will cover the first discharge trough 7 again.

[0039] After the first magnet 10 leaves the second magnet 11, a first spring 15 is fixed between the first magnet 10 and the top of the filter frame 3 to facilitate the reset of the baffle 9.

[0040] To facilitate support of the filter frame 3 and reduce the stress on the first rod 2, a ball bearing 16 is rotatably installed at the bottom of the filter frame 3, and an annular plate 17 is fixedly connected to the inner wall of the separation tank 1, with the ball bearing 16 rolling on the annular plate 17.

[0041] In the above description, the specific installation structure of the stirring rod 4 is as follows: one end of the stirring rod 4 is rotatably mounted on the side wall of the first rod 2. A sleeve 18 is sleeved and slidably connected to the outside of the first rod 2. A through groove 19 is opened on the outer wall of the sleeve 18. One end of the stirring rod 4 passes through the through groove 19 and can swing up and down in the through groove 19, which also prevents relative rotation between the sleeve 18 and the first rod 2. A straight rod 20 is fixed to the outer wall of the sleeve 18, and the straight rod 20 is located below the stirring rod 4. The straight rod 20 is used to push the stirring rod 4 upward; the top of the sleeve 18 is an inclined surface, and the second rod 21 is fixed to the inner wall of the top of the separation tank 1. When the first rod 2 rotates, the bottom end of the second rod 21 slides on the top of the sleeve 18; the bottom end of the first rod 2 is fixed to a circular plate 22, and the bottom of the sleeve 18 is fixed to a bellows 23, and the bottom end of the bellows 23 is fixed to the top of the circular plate 22; a second spring 24 is also fixed between the sleeve 18 and the circular plate 22.

[0042] When the motor drives rod 2 to rotate, it will cause rod 2 to drive sleeve 18 to rotate together. At this time, rod 21 will squeeze sleeve 18. With the action of the second spring 24, sleeve 18 will slide up and down along rod 2, which will allow rod 20 to squeeze stirring rod 4, so that stirring rod 4 can swing up and down, thereby increasing the stirring range of stirring rod 4 and making it easier to mix wastewater and organic solvent evenly. The corrugated pipe 23 can prevent wastewater from entering the gap between rod 2 and sleeve 18.

[0043] To prevent wastewater from entering the gap between rod 2 and sleeve 18 through the channel 19, an elastic waterproof cloth 25 is fixedly connected to the opening of the channel 19, and the stirring rod 4 passes through and is fixedly connected to the elastic waterproof cloth 25.

[0044] In use, when the motor drives the first rod 2 and the filter frame 3 to rotate, different positions of the filter frame 3 can receive wastewater falling from the first feed pipe 5 and filter the wastewater. This prevents impurities and particles from accumulating at a certain position on the top of the filter frame 3, thereby reducing the phenomenon of clogging of the filter frame 3. As the motor rotates, due to the centrifugal force, impurities and particles will move away from the center position of the first rod 2. When the first magnet 10 moves to below the second magnet 11, the first magnet 10 will move upward and attract together with the second magnet 11. At this time, the first discharge trough 7 is in the open state, which facilitates the discharge of impurities and particles from the first discharge trough 7 and along the guide plate 12. The wastewater eventually falls into the collection shell 14. As the first rod 2 rotates further, the first magnet 10 will move away from the second magnet 11. Under the gravity of the baffle 9 and the elastic force of the first spring 15, the baffle 9 will move downward and block the first discharge trough 7 again. When the motor drives the first rod 2 to rotate, the first rod 2 will drive the sleeve 18 to rotate together. At this time, the second rod 21 will squeeze the sleeve 18. With the action of the second spring 24, the sleeve 18 will slide up and down along the first rod 2, so that the straight rod 20 can squeeze the stirring rod 4, so that the stirring rod 4 can swing up and down, thereby increasing the stirring range of the stirring rod 4. This is beneficial for thoroughly mixing the wastewater and organic solvent and extracting o-phenylenediamine from the wastewater.

[0045] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A process for separating o-phenylenediamine from production wastewater, characterized in that: The separation process includes the following steps: Step 1: Pour the wastewater into the separation device from the first feed pipe (5), and remove impurities and solid particles from the wastewater through the rotating filter frame (3); Step 2: Add the organic solvent into the separation device through the second feed pipe (6), and then heat it to 80-90℃ to extract o-phenylenediamine from the wastewater; Step 3: The o-phenylenediamine is precipitated from the organic solvent through crystallization. The obtained o-phenylenediamine crystals are then dried to remove residual solvent, resulting in a dried o-phenylenediamine product. The separation device includes a separation tank (1), with a first rod (2) rotatably connected through the top of the separation tank (1). The first rod (2) is driven by a motor. A filter frame (3) and a stirring rod (4) are arranged sequentially from top to bottom on the outer wall of the first rod (2). The filter frame (3) is used to remove impurities and solid particles from the wastewater, and the stirring rod (4) is used to stir the wastewater and organic solvent. A first feed pipe (5) is provided at the top of the separation tank (1) to add wastewater into the separation tank (1). A second feed pipe (6) is provided on the side wall of the separation tank (1) to add organic solvent into the separation tank (1), and the bottom end of the second feed pipe (6) is located below the filter frame (3). The filter frame (3) has a first discharge trough (7) on one side, and the separation barrel (1) has a second discharge trough (8) on one side. The area of ​​the first discharge trough (7) is smaller than that of the second discharge trough (8). The top of the filter frame (3) is slidably connected to a baffle (9), and the top of the baffle (9) is fixedly connected to a first magnet (10). The bottom of the baffle (9) is located inside the first discharge trough (7). The inner wall of the separation barrel (1) is fixedly connected to a second magnet (11), and the second magnet (11) is located diagonally above the second discharge trough (8).

2. The separation process for o-phenylenediamine from production wastewater according to claim 1, characterized in that, The bottom of the second discharge trough (8) is fixedly connected to a guide plate (12) at an incline. The outer wall of the separation barrel (1) is fixedly connected to a support plate (13). A collection shell (14) is placed on the top of the support plate (13), and the bottom of the guide plate (12) is located above the collection shell (14).

3. The separation process for o-phenylenediamine from production wastewater according to claim 2, characterized in that, A first spring (15) is fixed between the first magnet (10) and the top of the filter frame (3), and the first spring (15) is used to reset the baffle (9).

4. The separation process for o-phenylenediamine from production wastewater according to claim 1, characterized in that, The bottom of the filter frame (3) is rotatably equipped with ball bearings (16), and the inner wall of the separation barrel (1) is also fixedly connected with an annular plate (17), on which the ball bearings (16) roll.

5. The process for separating o-phenylenediamine from production wastewater according to claim 1, characterized in that, One end of the stirring rod (4) is rotatably mounted on the side wall of the first rod (2). A sleeve (18) is sleeved and slidably connected to the outside of the first rod (2). A through groove (19) is opened on the outer wall of the sleeve (18). One end of the stirring rod (4) passes through the through groove (19). A straight rod (20) is fixed to the outer wall of the sleeve (18) and the straight rod (20) is located below the stirring rod (4). The straight rod (20) is used to push the stirring rod (4) upward.

6. The separation process for o-phenylenediamine from production wastewater according to claim 5, characterized in that, The top of the sleeve (18) is an inclined surface. A second rod (21) is fixed to the inner wall of the top of the separation barrel (1). When the first rod (2) rotates, the bottom end of the second rod (21) slides on the top of the sleeve (18). A circular plate (22) is fixed to the bottom end of the first rod (2). A bellows (23) is fixed to the bottom of the sleeve (18), and the bottom end of the bellows (23) is fixed to the top of the circular plate (22). A second spring (24) is also fixed between the sleeve (18) and the circular plate (22).

7. The process for separating o-phenylenediamine from production wastewater according to claim 5, characterized in that, An elastic waterproof cloth (25) is fixedly connected to the opening of the through groove (19), and the stirring rod (4) passes through and is fixedly connected to the elastic waterproof cloth (25).

8. The process for separating o-phenylenediamine from production wastewater according to claim 1, characterized in that, An electric heating plate is fixed to the bottom inner wall of the separation tank (1).

Citation Information

Patent Citations

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    US20170050119A1