Post-treatment reaction kettle for 2-hydroxy-benzonitrile

Abstract

The invention discloses a post-treatment reaction kettle for 2-hydroxy-benzonitrile, and relates to the technical field of preparation and processing of 2-hydroxy-benzonitrile, the post-treatment reaction kettle comprises a kettle body, a cover body is fixedly mounted on the kettle body, heating equipment is symmetrically arranged on two sides of the kettle body, and a stirring assembly is arranged in the kettle body; a first filter plate, a second filter plate and a third filter plate are arranged in the kettle body from top to bottom; a limiting block is fixedly mounted in the kettle body, one end of the first filter plate is rotatably connected with the kettle body, the other end of the first filter plate is slidably connected with the limiting block, the second filter plate is movably arranged below the first filter plate, and filter holes of the first filter plate and the second filter plate are staggered. The third filter plate is fixedly mounted below the second filter plate, and an adjusting assembly is arranged on the third filter plate and used for adjusting the height of the second filter plate; the problem that in the prior art, a small amount of impurities such as chloroform exist in 2-hydroxy-benzonitrile obtained by directly evaporating a dichloromethane solution of 2-hydroxy-benzonitrile, and the product quality is affected is solved.

Description

Technical Field

[0001] The invention relates to the technical field of preparation and processing of salicylic nitrile, in particular to a salicylic nitrile post-processing reactor. Background Art

[0002] Salicylonitrile, also known as o-hydroxybenzonitrile, is a white to light yellow crystal with a bitter almond aroma. Salicylonitrile is solid at room temperature and can be dissolved in organic solvents such as ethanol and chloroform, but is insoluble in water. Salicylonitrile is often used as an intermediate for organic synthesis of bunirolol and an intermediate for the fungicide azoxystrobin.

[0003] The existing synthesis method of salicylonitrile usually includes adding raw materials into a reactor, stirring and heating, cooling and distilling, transferring to a dichloromethane solvent, and performing acid washing, water washing, drying and other steps to obtain a dichloromethane solution of salicylonitrile, and finally directly evaporating to obtain solid salicylonitrile.

[0004] Salicylonitrile obtained by directly evaporating a dichloromethane solution of salicylonitrile may contain a small amount of impurities such as chloroform, which may affect the quality of the product. Summary of the invention

[0005] The present invention aims to solve at least one of the technical problems existing in the prior art. To this end, the present invention provides a salicylic nitrile post-treatment reactor, which solves the problem that the salicylic nitrile obtained by directly evaporating a dichloromethane solution of salicylic nitrile in the prior art contains a small amount of impurities such as chloroform, which affects the quality of the product.

[0006] To achieve the above-mentioned object, the present invention provides a salicylic nitrile post-treatment reactor, comprising a reactor body, a cover body fixedly mounted on the reactor body, heating devices symmetrically arranged on both sides of the reactor body, a water inlet, a feed inlet, a first installation box, and a storage tank fixedly mounted on the cover body, a stirring assembly is arranged in the first installation box, a motor is fixedly mounted on one side of the first installation box, and is used to drive the stirring assembly in the first installation box to rotate, and the stirring assembly is arranged in the reactor body;

[0007] The kettle body is provided with a first filter plate, a second filter plate and a third filter plate from top to bottom; a limit block is fixedly installed in the kettle body, one end of the first filter plate is rotatably connected to the kettle body, and the other end is slidably connected to the limit block, the second filter plate is movably arranged below the first filter plate, the filter holes of the first filter plate and the second filter plate are staggered, the third filter plate is fixedly installed below the second filter plate, and an adjustment component is arranged on the third filter plate to adjust the height of the second filter plate.

[0008] As a further solution of the present invention: the first installation box is arranged between the feed inlet and the storage tank, and the water inlet is arranged on a side close to the feed inlet.

[0009] As a further solution of the present invention: a first valve is provided on the feed inlet, and a second valve is provided on the storage tank.

[0010] As a further solution of the present invention: the stirring assembly includes a stirring rod, a stirring blade, and a driven wheel; one end of the stirring rod is rotatably connected to the inner side of the first installation box, and the other end extends into the kettle body, the driven wheel is fixedly installed above the stirring rod, the stirring blades are provided in several groups, and are fixedly and symmetrically installed below the stirring rod, the stirring blades are provided in the kettle body, the driven wheel is provided in the first installation box, a driving wheel is provided in the first installation box, the driving wheel is fixedly connected to the output shaft of the motor, and the driving wheel is meshed with the driven wheel.

[0011] As a further solution of the present invention: a bearing is arranged in the first installation box, the inner ring of the bearing is fixedly connected to the stirring rod, and the outer ring of the bearing is fixedly connected to the first installation box.

[0012] As a further solution of the present invention: the driving device of the heating device is arranged outside the kettle body, and the heating plate of the heating device is arranged inside the kettle body and symmetrically arranged on both sides of the stirring rod.

[0013] As a further solution of the present invention: the filter pore diameters of the first filter plate and the second filter plate are 5-10 μm.

[0014] As a further solution of the present invention: the adjustment assembly includes a first wedge block, a second wedge block, a stop block, and a bearing block; the stop block and the bearing block are fixedly mounted on the third filter plate, and the distance between the stop block and the bearing block matches the width of the first wedge block; the end of the first wedge block is fixedly connected to the second filter plate, the side of the first wedge block is slidably connected to the stop block, the second wedge block abuts against the first wedge block, the second wedge block and the first wedge block are provided with matching wedge openings, and the second wedge block is slidably connected to the bearing block.

[0015] As a further solution of the present invention: a second installation box is fixedly installed on the side of the kettle body, an electric push rod is fixedly installed in the second installation box, a movable rod is fixedly installed on the output shaft of the electric push rod, the movable rod is slidably connected to the bearing block, and a spring is fixedly installed between the movable rod and the second wedge block.

[0016] As a further solution of the present invention: a material discharge port and a water outlet are fixedly installed on the kettle body, and a third valve is arranged on the material discharge port and the water outlet. The material discharge port is arranged below the heating device, and the water outlet is arranged below the material discharge port.

[0017] Compared with the prior art, the present invention has the following beneficial effects:

[0018] By setting the adjustment component, the electric push rod is started to push the movable rod to slide, driving the second wedge to push the first wedge up and down, thereby driving the second filter plate to abut or move away from the first filter plate. When the first filter plate abuts against the second filter plate, the neutralization reaction solution can be collected. Then the heating device is started to heat the solution after the reaction to precipitate salicylonitrile in the solution. Then water is injected from the water inlet to wash the salicylonitrile particles. After washing, the electric push rod is started to drive the second wedge to move backward, thereby driving the first wedge to move downward, so as to achieve the disengagement of the first filter plate from the second filter plate. The aqueous solution flows down through the first filter plate and the second filter plate, and the salicylonitrile solid particles remain on the first filter plate. Then the heating device is started again to dry the salicylonitrile. After drying, the electric push rod is started again to push the first wedge to move upward. After the second filter plate abuts against the first filter plate, the second filter plate continues to be pushed up, driving the first filter plate to rotate a certain angle, so that the salicylonitrile on the first filter plate flows to the discharge port, which is convenient for the collection of salicylonitrile. That is, the filtration and collection of salicylonitrile can be achieved through the adjustment component. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a front view of a salicylonitrile post-treatment reaction kettle of the present invention;

[0020] Figure 2 This is a schematic structural diagram of a salicylonitrile post-treatment reactor of the present invention;

[0021] Figure 3 A salicylic nitrile post-treatment reactor according to the present invention Figure 2 A magnified image of point A;

[0022] Figure 4 A salicylic nitrile post-treatment reactor according to the present invention Figure 2 Enlarged view of point B.

[0023] In the figure: 1. kettle body; 2. mounting frame; 3. heating equipment; 4. water inlet; 5. material inlet; 6. first valve; 7. motor; 8. first mounting box; 9. material storage tank; 10. second mounting box; 11. material outlet; 12. third valve; 13. second valve; 14. cover body; 15. electric push rod; 16. limit block; 17. stirring rod; 18. stirring blade; 19. bearing; 20. driving wheel; 21. driven wheel; 22. movable rod; 23. spring; 24. second wedge block; 25. first wedge block; 26. first filter plate; 27. second filter plate; 28. stop block; 29. ​​bearing block; 30. third filter plate; 31. water outlet. DETAILED DESCRIPTION

[0024] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0025] like Figure 1-4 As shown, a salicylonitrile post-treatment reactor comprises a reactor body 1, a cover body 14 is fixedly mounted on the reactor body 1, heating devices 3 are symmetrically arranged on both sides of the reactor body 1, a discharge port 11 and a water outlet 31 are fixedly mounted on the reactor body 1, a third valve 12 is arranged on the discharge port 11 and the water outlet 31, the discharge port 11 is arranged below the heating device 3, and the water outlet 31 is arranged below the discharge port 11;

[0026] As an implementation method in the present embodiment, a water inlet 4, a feed inlet 5, a first installation box 8, and a storage tank 9 are fixedly installed on the cover body 14. The first installation box 8 is arranged between the feed inlet 5 and the storage tank 9. The water inlet 4 is arranged on a side close to the feed inlet 5. The storage tank 9 is used to store a neutralization solution, which is a sodium hydroxide solution in the present embodiment. A stirring assembly is arranged in the first installation box 8. A motor 7 is fixedly installed on one side of the first installation box 8 for driving the stirring assembly in the first installation box 8 to rotate. A first valve 6 is arranged on the feed inlet 5, and a second valve 13 is arranged on the storage tank 9. Salicylonitrile obtained by directly evaporating a dichloromethane solution of salicylonitrile is injected through the feed inlet 5. The second valve 13 is opened to add an appropriate amount of sodium hydroxide solution and salicylonitrile for acid-base neutralization reaction to adjust the pH of salicylonitrile; the stirring assembly is arranged in the kettle body 1, and the stirring assembly includes A stirring rod 17, a stirring blade 18, and a driven wheel 21; one end of the stirring rod 17 is rotatably connected to the inner side of the first installation box 8, and the other end extends into the kettle body 1. The driven wheel 21 is fixedly installed above the stirring rod 17. The stirring blade 18 is provided with several groups, which are fixedly and symmetrically installed below the stirring rod 17. The stirring blade 18 is arranged in the kettle body 1, and the driven wheel 21 is arranged in the first installation box 8. A driving wheel 20 is arranged in the first installation box 8, and the driving wheel 20 is fixedly connected to the output shaft of the motor 7. The driving wheel 20 is meshed with the driven wheel 21. By driving the driving wheel 20 to rotate, the stirring assembly can be driven to operate; a bearing 19 is arranged in the first installation box 8, and the inner ring of the bearing 19 is fixedly connected to the stirring rod 17, and the outer ring of the bearing 19 is fixedly connected to the first installation box 8, in order to provide a certain support for the stirring rod 17 without affecting the movement of the stirring rod 17;

[0027] As an implementation method in this embodiment, the driving device of the heating device 3 is arranged on the outside of the kettle body 1, the heating plate of the heating device 3 is arranged in the kettle body 1, and is symmetrically arranged on both sides of the stirring rod 17, and the first filter plate 26, the second filter plate 27, and the third filter plate 30 are arranged below the stirring blade 18 from near to far; the limit block 16 is fixedly installed in the kettle body 1, one end of the first filter plate 26 is rotatably connected to the kettle body 1, and the other end is slidably connected to the limit block 16, and the second filter plate 27 is movably arranged at Below the first filter plate 26, the first filter plate 26 and the second filter plate 27 are both filter plates with a filter hole diameter of 5-10 μm, and the filter holes are arranged in a staggered manner. When the second filter plate 27 abuts against the first filter plate 26, the neutralized solution in the kettle body 1 cannot be filtered from the first filter plate 26 to the second filter plate 27; the third filter plate 30 is fixedly installed below the second filter plate 27, and the third filter plate 30 is provided with an adjustment component for adjusting the height of the second filter plate 27, thereby adjusting the distance between the second filter plate 27 and the first filter plate 26;

[0028] As an implementation method in this embodiment, the adjustment component includes a first wedge block 25, a second wedge block 24, a stopper 28, and a bearing block 29; the stopper 28 is fixedly installed on the bearing block 29 on the third filter plate 30, and the distance between the stopper 28 and the bearing block 29 matches the width of the first wedge block 25; the end of the first wedge block 25 is fixedly connected to the second filter plate 27, the side of the first wedge block 25 is slidably connected to the stopper 28, the second wedge block 24 and the first wedge block 25 are abutted, the second wedge block 24 and the first wedge block 25 are provided with matching wedge openings, the second wedge block 24 and the bearing block 29 are slidably connected, an electric push rod 15 is fixedly installed in the second installation box 10, the output shaft of the electric push rod 15 is fixedly installed with a movable rod 22, the movable rod 22 is slidably connected to the bearing block 29, and a spring 23 is fixedly installed between the movable rod 22 and the second wedge block 24, the purpose of the above setting is to start the electric push rod 15 to push the movable rod 22 to slide, drive the second wedge block 24 to push the first wedge block 25 to move up and down, thereby The second filter plate 27 is moved to contact or move away from the first filter plate 26. When the first filter plate 26 and the second filter plate 27 contact each other, the neutralization reaction solution can be collected. Then, the heating device 3 is started to heat the solution after the reaction to precipitate the salicylonitrile in the solution. Then, water is injected from the water inlet 4 to wash the salicylonitrile particles. After washing, the electric push rod 15 is started to drive the second wedge block 24 to move backward, thereby driving the first wedge block 25 to move downward, so as to achieve the separation of the first filter plate 26 from the second filter plate 27. The aqueous solution flows down through the first filter plate 26 and the second filter plate 27, and the solid particles of salicylic nitrile remain on the first filter plate 26. The heating device 3 is then started again to dry the salicylic nitrile. After drying, the electric push rod 15 is started again to push the first wedge block 25 to move upward, and the second filter plate 27 is pushed against the first filter plate 26 and continues to move the second filter plate 27 upward, driving the first filter plate 26 to rotate a certain angle, so that the salicylic nitrile on the first filter plate 26 flows to the discharge port 11, which is convenient for the collection of salicylic nitrile.

[0029] As an implementation method in this embodiment, a plurality of pairs of mounting frames 2 are fixedly installed under the kettle body 1 to facilitate the fixation of the entire device.

[0030] Working principle:

[0031] When in use, salicylonitrile obtained by directly evaporating a dichloromethane solution of salicylonitrile is injected through the feed port 5, and the second valve 13 is opened to add an appropriate amount of sodium hydroxide solution to carry out acid-base neutralization reaction with the salicylonitrile to adjust the pH of the salicylonitrile; the motor 7 is started to drive the stirring assembly in the first installation box 8 to rotate to accelerate the neutralization reaction process, and then the heating device 3 is started to heat the solution after the reaction to precipitate the salicylonitrile in the solution, and then water is injected from the water inlet 4 to wash the salicylonitrile particles. After the washing is completed, the electric push rod 15 is started to drive the second wedge block 24 to move backward, thereby driving the first The wedge block 25 moves downward to achieve the disengagement of the first filter plate 26 from the second filter plate 27, and the aqueous solution flows down through the first filter plate 26 and the second filter plate 27, and the salicylon solid particles remain on the first filter plate 26. Then, the heating device 3 is started again to dry the salicylon. After drying, the electric push rod 15 is started again to push the first wedge block 25 to move upward, and the second filter plate 27 continues to push the second filter plate 27 upward after abutting against the first filter plate 26, driving the first filter plate 26 to rotate a certain angle, so that the salicylon on the first filter plate 26 flows to the discharge port 11, which is convenient for the collection of salicylon.

[0032] In the description of the present invention, it should be understood that the terms "upper", "lower", "left", "right", etc. indicating directions or positional relationships are based on the directions or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific direction, and a specific direction structure and operation, and therefore, cannot be understood as a limitation on the present invention. In addition, "first" and "second" are only for descriptive purposes, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, unless otherwise specified, "multiple" means two or more.

[0033] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", etc. should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or an indirect connection through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0034] The above is a detailed description of an embodiment of the present invention, but the content is only a preferred embodiment of the present invention and cannot be considered to limit the scope of implementation of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the patent coverage of the present invention.

Claims

1. A salicylic nitrile post-treatment reactor, characterized in that: The invention comprises a kettle body (1), a cover body (14) is fixedly mounted on the kettle body (1), heating devices (3) are symmetrically arranged on both sides of the kettle body (1), a water inlet (4), a material inlet (5), a first installation box (8), and a material storage tank (9) are fixedly mounted on the cover body (14), a stirring assembly is arranged in the first installation box (8), a motor (7) is fixedly mounted on one side of the first installation box (8) for driving the stirring assembly in the first installation box (8) to rotate, and the stirring assembly is arranged in the kettle body (1); a first filter plate (26), a first filter plate (27), a first filter plate (28), a first filter plate (29), a first filter plate (30), a first filter plate (31), a first filter plate (32), a first filter plate (33), a first filter plate (34), a first filter plate (35), a first filter plate (36), a first filter plate (37), a first filter plate (38), a first filter plate (39), a first filter plate (40), a first filter plate (41), a first filter plate (42), a first filter plate (43), a first filter plate (44), a first filter plate (45), a first filter plate (46), a first filter plate (47), a first filter plate (48), a first filter plate (49), a first filter plate (50), a first filter plate (51), a first filter plate (52), a first filter plate (53), a first filter plate (54), a first filter plate (55), a first filter plate (56), a first filter plate (57), a first filter plate (58), a first filter plate (59), a first filter plate (60), a first filter plate (61), a first filter plate (62), a first filter plate (63), a first filter plate (64), a first filter plate (65), a first filter plate (66), a first filter plate (67), a first filter plate (68), a first filter plate (69), a first filter plate (71), a a second filter plate (27) and a third filter plate (30); a limit block (16) is fixedly installed in the kettle body (1); one end of the first filter plate (26) is rotatably connected to the kettle body (1), and the other end is slidably connected to the limit block (16); the second filter plate (27) is movably arranged below the first filter plate (26); the filter holes of the first filter plate (26) and the second filter plate (27) are staggered; the third filter plate (30) is fixedly installed below the second filter plate (27); and an adjustment component is arranged on the third filter plate (30) for adjusting the height of the second filter plate (27).

2. A salicylic nitrile post-treatment reactor according to claim 1, characterized in that: The first installation box (8) is arranged between the feed inlet (5) and the storage tank (9), and the water inlet (4) is arranged on a side close to the feed inlet (5).

3. A salicylic nitrile post-treatment reactor according to claim 2, characterized in that: The feed inlet (5) is provided with a first valve (6), and the storage tank (9) is provided with a second valve (13).

4. A salicylic nitrile post-treatment reactor according to claim 1, characterized in that: The stirring assembly comprises a stirring rod (17), a stirring blade (18), and a driven wheel (21); one end of the stirring rod (17) is rotatably connected to the inner side of the first installation box (8), and the other end extends into the kettle body (1); the driven wheel (21) is fixedly installed above the stirring rod (17); the stirring blade (18) is provided in a plurality of groups and is fixedly and symmetrically installed below the stirring rod (17); the stirring blade (18) is arranged in the kettle body (1); the driven wheel (21) is arranged in the first installation box (8); a driving wheel (20) is arranged in the first installation box (8); the driving wheel (20) is fixedly connected to the output shaft of the motor (7), and the driving wheel (20) is meshed with the driven wheel (21).

5. A salicylic nitrile post-treatment reactor according to claim 4, characterized in that: A bearing (19) is arranged in the first installation box (8), the inner ring of the bearing (19) is fixedly connected to the stirring rod (17), and the outer ring of the bearing (19) is fixedly connected to the first installation box (8).

6. A salicylic nitrile post-treatment reactor according to claim 4, characterized in that: The driving device of the heating device (3) is arranged outside the kettle body (1), and the heating plate of the heating device (3) is arranged inside the kettle body (1) and symmetrically arranged on both sides of the stirring rod (17).

7. A salicylic nitrile post-treatment reactor according to claim 1, characterized in that: The filter pore diameters of the first filter plate (26) and the second filter plate (27) are 5-10 μm.

8. A salicylic nitrile post-treatment reactor according to claim 1, characterized in that: The adjustment assembly comprises a first wedge block (25), a second wedge block (24), a stop block (28), and a bearing block (29); the stop block (28) and the bearing block (29) are fixedly mounted on the third filter plate (30), and the distance between the stop block (28) and the bearing block (29) matches the width of the first wedge block (25); the end of the first wedge block (25) is fixedly connected to the second filter plate (27), the side of the first wedge block (25) is slidably connected to the stop block (28), the second wedge block (24) is abutted against the first wedge block (25), matching wedge openings are provided on the second wedge block (24) and the first wedge block (25), and the second wedge block (24) is slidably connected to the bearing block (29).

9. A salicylic nitrile post-treatment reactor according to claim 8, characterized in that: A second installation box (10) is fixedly installed on the side of the kettle body (1), an electric push rod (15) is fixedly installed in the second installation box (10), a movable rod (22) is fixedly installed on the output shaft of the electric push rod (15), the movable rod (22) is slidably connected to the bearing block (29), and a spring (23) is fixedly installed between the movable rod (22) and the second wedge block (24).

10. A salicylic nitrile post-treatment reactor according to claim 1, characterized in that: A material discharge port (11) and a water outlet (31) are fixedly mounted on the kettle body (1), and a third valve (12) is arranged on both the material discharge port (11) and the water outlet (31). The material discharge port (11) is arranged below the heating device (3), and the water outlet (31) is arranged below the material discharge port (11).

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