An efficient 2-aminosulfonyl-n,n-dimethylnicotinamide production device

Abstract

The utility model relates to an efficient 2-amino sulfonyl-N, N-dimethyl nicotinamide production device relates to organic synthesis technical field. The reaction kettle, reagent tank and metering pump are installed on the bottom crowbar, the upper portion of reaction kettle is equipped with track, the track is made into plane archimedes spiral structure by I -beam, the upper portion of guide rail is fixedly connected with stand, four stands are fixedly connected with two cross beams on the upper portion, and the cross beam is fixed on the inner wall of reaction kettle. The beneficial effect of the utility model is that the amount of oxidizing agent sprayed by the metering pump each time can be understood as carrying out oxidation reaction with a three-dimensional solution unit, the trolley moves to the next three-dimensional solution unit, the metering pump sprays oxidizing agent again, the telescopic rod of the electric push rod drops by a distance, the trolley moves reversely from the center of the guide rail to the outermost side, and the oxidizing agent sprayed by the metering pump uniformly mixes and reacts with the aqueous solution of N-dimethyl nicotinamide in the layer, so that the solution in the reaction kettle can be mixed and reacted with the oxidizing agent as a whole.

Description

Technical Field

[0001] This invention relates to the fields of pharmaceutical equipment manufacturing and formulation manufacturing technology, and in particular to a high-efficiency 2-aminosulfonyl-N,N-dimethylnicotinamide production device. Background Technology

[0002] Aminosulfonyl-N,N-dimethylnicotinamide is an important intermediate in the herbicide nicosulfuron technical grade. Nicosulfuron is a chemical pharmaceutical raw material. Currently, the industrial production route uses 2-chloro-N,N-dimethylnicotinamide as a raw material. First, it reacts with sulfur, sodium sulfide, and water to prepare 2-mercapto-N,N-dimethylnicotinamide. Its aqueous solution is then chlorinated with chlorine in the presence of an organic solvent to synthesize 3-(dimethylcarbamoyl)pyridine-2-sulfonyl chloride. Then, ammonia is introduced into the organic solution of 3-(dimethylcarbamoyl)pyridine-2-sulfonyl chloride to prepare 2-aminosulfonyl-N,N-dimethylnicotinamide. The overall yield of the entire reaction process is between 70% and 80%, with the yields of the thiolation and amination steps both exceeding 98%. The key step affecting the yield is the reaction of 2-mercapto-N,N-dimethylnicotinamide with chlorine to synthesize the 3-(dimethylcarbamoyl)pyridine-2-sulfonyl chloride step.

[0003] The reaction of 2-mercapto-N,N-dimethylnicotinamide with chlorine is essentially an oxidation-chlorination process. In current batch reactors, the oxidation and chlorination stages occur almost simultaneously. The oxidation stage releases a large amount of heat, making temperature control difficult. Furthermore, the chlorination product, 3-(dimethylcarbamoyl)pyridine-2-sulfonyl chloride, is readily hydrolyzed in a high-temperature system with water present. This explains why current batch reactor yields are only 70%–80%. Therefore, reducing the hydrolysis of 3-(dimethylcarbamoyl)pyridine-2-sulfonyl chloride during the reaction is key to improving the yield of this step.

[0004] Some literature has made improvements to this approach, such as CN 116813539 B, which describes the addition of a measured amount of oxidant after the preparation of the sodium salt of 2-mercapto-N,N-dimethylnicotinamide. This separates the strongly exothermic oxidation stage, effectively reducing the heat accumulation during the chlorination stage and avoiding the hydrolysis of 3-(dimethylcarbamoyl)pyridine-2-sulfonyl chloride. However, while the dropwise addition method slows down the heat accumulation, it cannot guarantee uniform contact and reaction between the aqueous solution of 2-mercapto-N,N-dimethylnicotinamide and the oxidant in the reactor. Stirring also fails to ensure this, thus reducing the reaction efficiency. Summary of the Invention

[0005] To address the aforementioned problems, this invention provides a highly efficient 2-aminosulfonyl-N,N-dimethylnicotinamide production apparatus.

[0006] The technical solution provided by this invention is: a high-efficiency 2-aminosulfonyl-N,N-dimethylnicotinamide production device, including a bottom skid, on which a reaction vessel, a reagent tank, a metering pump and a control box are installed. The reaction vessel has a cylindrical structure, and a track is provided on the upper part of the reaction vessel. The track is made of I-beams bent into a planar Archimedean spiral structure. Four columns are fixedly connected to the upper part of the track, and two crossbeams are fixedly connected to the upper part of the four columns. The two crossbeams intersect each other and are fixed to the inner wall of the reaction vessel.

[0007] A trolley is suspended on the guide rail. An electric push rod is fixedly connected to the bottom of the trolley. A nozzle is fixedly connected to the bottom of the telescopic rod of the electric push rod. The nozzle is connected to a heat transfer hose. A dosing hose is installed inside the heat transfer hose. A round hole is provided in the center of the reaction vessel on the crossbeam. The heat transfer hose and the dosing hose extend upwards out of the round hole of the crossbeam and are connected to a winding machine. The winding machine has a dosing pipe A connected to a metering pump. The inlet of the metering pump is connected to the dosing tank through a valve.

[0008] The winding machine includes a base on which a refrigeration unit, a heat exchange box, a roller, and a spring box are mounted. Supports are located on both sides of the roller, and the roller is rotatably connected to the supports. One side of the roller is connected to the spring box, and the other side has a hollow shaft, which is rotatably connected to the supports. A heat transfer pipe and a chemical dosing hose are wound on the roller. The ends of the heat transfer pipe and the chemical dosing hose extend into the hollow shaft, and the heat transfer hose is fixedly connected to the hollow shaft. The heat transfer hose extends out of the hollow shaft and into the heat exchange box. A heat exchange head with a hollow structure is located inside the heat exchange box. A connecting pipe A is located on the heat exchange head and is rotatably connected to the heat transfer hose via a mechanical seal. A chemical dosing pipe A is located inside the heat exchange box and is fixedly connected to the heat exchange head via a support plate. The chemical dosing pipe A is rotatably connected to the chemical dosing hose via a mechanical seal. The chemical dosing pipe A extends out of the heat exchange box and connects to a metering pump. The heat exchange box is filled with refrigerant, and a refrigerant circulation pipe connects the heat exchange box to the refrigeration unit.

[0009] The nozzle has a hollow structure and includes a shell. A connecting pipe B is provided on one side of the shell. The connecting pipe B is connected to the heat transfer hose through a sealing ring and threads. The dosing hose is connected to the dosing pipe B through threads and a sealing ring. The dosing pipe B extends to the bottom of the shell and extends out of the shell. The outer side of the shell is provided with circumferentially distributed heat exchange fins. The heat exchange fins have a hollow structure and are in communication with the inside of the shell. A layer of capillary material is adhered to the inner surface of the heat exchange fins, the shell, the connecting pipe B, the heat transfer hose, the connecting pipe A, and the heat exchange head. The above space is evacuated to a negative pressure state and is filled with working fluid.

[0010] The outer ring of the turntable bearing is connected to the round hole of the crossbeam by bolts. The inner ring of the turntable bearing is connected to the fixed pulley A. The crossbeam has a fixed pulley B outside the round hole. The fixed pulley B is located at the top of the crossbeam. The heat transfer hose passes around the fixed pulley A and fixed pulley B from the bottom and then winds onto the drum.

[0011] The trolley includes a chassis, an electric push rod is fixedly connected to the chassis, two drive wheels are provided on the chassis, the drive wheels are connected to a reduction gearbox, the reduction gearbox is connected to a motor, and two follower wheels are provided on the opposite side of the drive wheels on the chassis. The drive wheels and follower wheels are located on both sides of the vertical rib of the guide rail I-beam.

[0012] The electric push rod is equipped with a limit ring, which is located on the inside of the guide rail. The heat transfer hose passes through the limit ring, and the column is located on the outermost ring of the guide rail helix.

[0013] The control box has wires connecting the refrigeration unit, motor, and electric actuator.

[0014] The beneficial effects of this invention are as follows: the trolley moves from the outermost edge of the guide rail towards the center. During the movement of the trolley, the oxidant sprayed by the metering pump uniformly mixes and reacts with the aqueous solution of N-dimethylnicotinamide in this layer. The amount of oxidant sprayed by the metering pump each time can be understood as reacting with one three-dimensional solution unit. When the trolley moves to the next three-dimensional solution unit, the metering pump sprays oxidant again. When the trolley moves to the innermost edge of the guide rail, the telescopic rod of the electric push rod descends a distance, and the trolley moves in the opposite direction, from the center of the guide rail to the outermost edge. The oxidant sprayed by the metering pump uniformly mixes and reacts with the aqueous solution of N-dimethylnicotinamide in this layer, thereby allowing the solution in the reaction vessel to be mixed and reacted with the oxidant as a whole.

[0015] The nozzle, heat transfer hose, and heat exchange head form a heat pipe system with high thermal conductivity. The nozzle and heat exchange fins are the evaporation ends. The working liquid has a low evaporation point in the negative pressure environment. The evaporating working liquid carries away the heat from the oxidant reaction. The evaporating working liquid condenses in the heat exchange head. The condensed working liquid returns to the evaporation end under the capillary effect of the capillary, thereby reducing the hydrolysis rate of 3-(dimethylcarbamoyl)pyridine-2-sulfonyl chloride and increasing the product yield. Attached Figure Description

[0016] Appendix Figure 1 This is a schematic diagram of the structure of the present invention;

[0017] Appendix Figure 2 It is attached Figure 1 Top view;

[0018] Appendix Figure 3 This is a partial structural diagram of the present invention;

[0019] Appendix Figure 4 It is attached Figure 3 Sectional view at point B;

[0020] Appendix Figure 5 This is a schematic diagram of the nozzle structure;

[0021] Appendix Figure 6 It is attached Figure 5 Enlarged view of point C;

[0022] Appendix Figure 7 This is a structural diagram of a winding machine;

[0023] Appendix Figure 8 It is attached Figure 7 Enlarged view of point A;

[0024] Appendix Figure 9 It is attached Figure 7 Enlarged view of point E;

[0025] Appendix Figure 10 It is attached Figure 1 Enlarged view of point D;

[0026] Appendix Figure 11 This is a structural diagram of the car.

[0027] In the diagram: 1-Bottom skid, 2-Reaction vessel, 3-Reagent tank, 4-Dosing hose, 5-Winder, 6-Guide rail, 601-Column, 602-Beam, 603-Round hole, 7-Electric push rod, 701-Telescopic rod, 702-Limit ring, 8-Heat transfer hose, 9-Trolley, 901-Chassis, 902-Motor, 903-Reduction gearbox, 904-Drive wheel, 905-Follower wheel, 10-Control box, 11-Drum, 1101-Empty 12-Spindle, 13-Curling box, 14-Heat exchange box, 15-Refrigeration unit, 16-Dosing pipe A, 17-Metering pump, 18-Heat exchange head, 1801-Connecting pipe A, 19-Mechanical seal, 20-Nozzle, 201-Outer shell, 202-Heat exchange fins, 203-Connecting pipe B, 21-Dosing pipe B, 22-Capillary material, 23-Rotating bearing, 24-Fixed pulley A, 25-Fixed pulley B, 26-Base, 27-Support plate. Detailed Implementation

[0028] like Figures 1-11 As shown, a high-efficiency 2-aminosulfonyl-N,N-dimethylnicotinamide production device includes a bottom skid 1, on which a reaction vessel 2, a reagent tank 3, a metering pump 17, and a control box 10 are installed. The reaction vessel 2 has a cylindrical structure, and a track 6 is provided on the upper part of the reaction vessel 2. The track 6 is made of I-beams bent into a planar Archimedean spiral structure. Four columns 601 are fixedly connected to the upper part of the track 6, and two crossbeams 602 are fixedly connected to the upper part of the four columns 601. The two crossbeams 602 intersect each other and are fixed to the inner wall of the reaction vessel 2.

[0029] A trolley 9 is hung on the guide rail 6. An electric push rod 7 is fixedly connected to the bottom of the trolley 9. A nozzle 20 is fixedly connected to the bottom of the telescopic rod 701 of the electric push rod 7. The nozzle 20 is connected to the heat transfer hose 8. A dosing hose 4 is provided inside the heat transfer hose 8. A round hole 603 is provided in the center of the reaction vessel 2 on the crossbeam 602. The heat transfer hose 8 and the dosing hose 4 extend upwards out of the round hole 603 of the crossbeam 602 and are connected to the winding machine 5. The winding machine 5 has a dosing pipe A16 connected to the metering pump 17. The inlet of the metering pump 17 is connected to the dosing tank 3 through a valve.

[0030] The winding machine 5 includes a base 26, on which a refrigeration unit 15, a heat exchange box 14, a drum 11, and a spring box 13 are respectively mounted. Supports 12 are provided on both sides of the drum 11, and the drum 11 is rotatably connected to the supports 12. One side of the drum 11 is connected to the spring box 13, which has the same structure as the automatic winding device for overhead cranes. A hollow shaft 1101 is provided on the other side of the drum 11, and the hollow shaft 1101 is rotatably connected to the supports 12. A heat transfer pipe 8 and a chemical dosing hose 4 are wound on the drum 11, and the ends of the heat transfer pipe 8 and the chemical dosing hose 4 extend into the hollow shaft 1101. The heat transfer hose 8 is fixedly connected to the hollow shaft 1101. After extending out of the hollow shaft 1101, the heat transfer hose 8 extends into the heat exchange box 14. The heat exchange box 14 is equipped with a heat exchange head 18, which has a hollow structure. The heat exchange head 18 is equipped with a connecting pipe A1801. The connecting pipe A1801 is rotatably sealed to the heat transfer hose 8 through a mechanical seal 19. The heat exchange box 14 is equipped with a dosing pipe A16. The dosing pipe A16 and the heat exchange head 18 are fixedly connected to the heat exchange box 14 through a support plate 27. The dosing pipe A16 is rotatably sealed to the dosing hose 4 through a mechanical seal 19.

[0031] The structure allows the heat transfer hose 8 at the center of the drum 411 to rotate and seal with the connecting pipe A1801 when the drum 11 rotates to receive and release the heat transfer pipe 8, and the dosing hose 4 and the dosing pipe A16 to rotate and seal with each other.

[0032] The dosing pipe A16 extends out of the heat exchange box 14 and connects to the metering pump 17. The heat exchange box 14 is filled with refrigerant and has a refrigerant circulation pipe connected to the refrigeration unit 15.

[0033] The nozzle 20 has a hollow structure and includes a housing 201. A connecting pipe B203 is provided on one side of the housing 201. The connecting pipe B203 is connected to the heat transfer hose 8 via a sealing ring and threads. The dosing hose 4 is connected to the dosing pipe B21 via threads and a sealing ring. The dosing pipe B21 extends to the bottom of the housing 201 and protrudes from the housing 201. The outer side of the housing 201 has circumferentially distributed heat exchange fins 202. The heat exchange fins 202 have a hollow structure and communicate with the interior of the housing 201. The components include the heat exchange fins 202, the housing 201, the connecting pipe B203, and the heat transfer hose 8. A layer of capillary material 22 is adhered to the inner surface of the connector A1801 and the heat exchange head 18. The space is evacuated to a negative pressure state and filled with working fluid. The nozzle 20, the heat transfer hose 8 and the heat exchange head 18 form a heat pipe system with high heat conduction capacity. The nozzle 20 and the heat exchange fins 202 are the evaporation ends. The working fluid has a low evaporation point in the negative pressure environment. The evaporating working fluid carries away the heat from the reaction of the oxidant. The evaporating working fluid condenses in the heat exchange head 18. The condensed working fluid returns to the evaporation end under the capillary effect of the capillary material 22.

[0034] When adding the oxidant, the metering pump 17 pumps the oxidant from the reagent tank 3 into the dosing pipe A16, which is then converted into a dosing hose 4 by the winding machine 5. The dosing hose 4 is converted into a dosing pipe B21 in the nozzle 20, and sprayed out from the nozzle 20 to react with the aqueous solution of N-dimethylnicotinamide. The heat generated by oxidation is carried away by the heat pipe system. Since the dosage of the oxidant sprayed by the metering pump 17 is constant for each stroke, the heat pipe system is designed to carry the heat released when the oxidant sprayed in this stroke participates in the reaction. In other words, the temperature of the solution in the overall reaction vessel 2 will not rise when the oxidant is injected.

[0035] The operating procedure of the trolley 9 is as follows: The trolley 9 moves from the outermost side of the guide rail 6 towards the center. During the movement of the trolley 9, the oxidant sprayed by the metering pump 17 will uniformly mix and react with the aqueous solution of N-dimethylnicotinamide in this layer. The amount of oxidant sprayed by the metering pump 17 each time can be understood as reacting with one unit of three-dimensional solution. The trolley 9 moves to the next unit of three-dimensional solution, and the metering pump 17 sprays oxidant again. When the trolley 9 moves to the innermost side of the guide rail 6, the telescopic rod 701 of the electric push rod 7 drops a distance, and the trolley 9 moves in the opposite direction, from the center of the guide rail 6 to the outermost side. The oxidant sprayed by the metering pump 17 will uniformly mix and react with the aqueous solution of N-dimethylnicotinamide in this layer. In this way, the solution in the reaction vessel 2 can be mixed and reacted with the oxidant as a whole.

[0036] The outer ring of the turntable bearing 23 is bolted into the round hole 603 of the crossbeam 602. The inner ring of the turntable bearing 23 is connected to the fixed pulley A24. The crossbeam 602 has a fixed pulley B25 outside the round hole 603. The fixed pulley B25 is located on the upper part of the crossbeam 602. The heat transfer hose 8 passes around the fixed pulley A24 and fixed pulley B25 from the bottom and is wound onto the drum 11. When the trolley 9 moves, it drives the heat transfer hose 8 to move. The turntable bearing 23 drives the top pulley A24 to rotate, so as to prevent the heat transfer hose 8 from getting stuck due to tangled winding.

[0037] The trolley 9 includes a chassis 901, which is fixedly connected to an electric push rod 7. Two drive wheels 904 are provided on the chassis 901. The drive wheels 904 are connected to a reduction gearbox 903, which is connected to a motor 902. Two follower wheels 905 are provided on the chassis 901 opposite to the drive wheels 904. The drive wheels 904 and follower wheels 905 are located on both sides of the vertical ribs of the I-beam of the guide rail 6.

[0038] The electric push rod 7 is equipped with a limiting ring 702, which is located on the inside of the guide rail 6. The heat transfer hose 8 passes through the limiting ring 702, and the column 601 is located on the outermost ring of the guide rail 6 spiral. This arrangement ensures that the heat transfer hose 8 will not get tangled with the column 601 when the trolley 9 moves along the guide rail 6.

[0039] The control box 10 has wires connecting the refrigeration unit 15, the motor 902, and the electric push rod 7.

Claims

1. A high-efficiency 2-aminosulfonyl-N,N-dimethylnicotinamide production apparatus, comprising a bottom skid (1), characterized in that: The bottom skid (1) is equipped with a reaction vessel (2), a reagent tank (3), a metering pump (17) and a control box (10). The reaction vessel (2) is a cylindrical structure. The upper part of the reaction vessel (2) is equipped with a track (6). The track (6) is made of I-beams and formed into a planar Archimedean spiral structure. The upper part of the guide rail (6) is fixedly connected to four columns (601). The upper part of the four columns (601) is fixedly connected to two crossbeams (602). The two crossbeams (602) intersect each other. The crossbeams (602) are fixed on the inner wall of the reaction vessel (2). A trolley (9) is hung on the guide rail (6). An electric push rod (7) is fixedly connected to the bottom of the trolley (9). A nozzle (20) is fixedly connected to the bottom of the telescopic rod (701) of the electric push rod (7). The nozzle (20) is connected to the heat transfer hose (8). A dosing hose (4) is provided inside the heat transfer hose (8). A round hole (603) is provided in the center of the reaction vessel (2) on the crossbeam (602). The heat transfer hose (8) and the dosing hose (4) extend upwards through the round hole (603) of the crossbeam (602) and are connected to the winding machine (5). The winding machine (5) has a dosing pipe A (16) connected to the metering pump (17). The inlet of the metering pump (17) is connected to the dosing tank (3) through a valve.

2. The high-efficiency 2-aminosulfonyl-N,N-dimethylnicotinamide production apparatus according to claim 1, characterized in that: The winding machine (5) includes a base (26), on which a refrigeration unit (15), a heat exchange box (14), a drum (11), and a spring box (13) are respectively installed. Supports (12) are provided on both sides of the drum (11), and the drum (11) is rotatably connected to the supports (12). One side of the drum (11) is connected to the spring box (13), and the other side of the drum (11) is provided with a hollow shaft (1101), which is rotatably connected to the supports (12). A heat transfer pipe (8) and a chemical dosing hose (4) are wound on the drum (11). The ends of the heat transfer pipe (8) and the chemical dosing hose (4) extend into the hollow shaft (1101). The heat transfer hose (8) is fixedly connected to the hollow shaft (1101). After the heat transfer hose (8) extends out of the hollow shaft (1101), The heat exchanger extends into the heat exchange box (14), which is equipped with a heat exchange head (18). The heat exchange head (18) has a hollow structure and a connecting pipe A (1801) is provided on the heat exchange head (18). The connecting pipe A (1801) is connected to the heat transfer hose (8) through a mechanical seal (19). The heat exchange box (14) is equipped with a dosing pipe A (16). The dosing pipe A (16) and the heat exchange head (18) are fixedly connected in the heat exchange box (14) through a support plate (27). The dosing pipe A (16) is connected to the dosing hose (4) through a mechanical seal (19). The dosing pipe A (16) extends out of the heat exchange box (14) and is connected to a metering pump (17). The heat exchange box (14) is filled with refrigerant and has a refrigerant circulation pipe connected to the refrigeration unit (15).

3. A high-efficiency 2-aminosulfonyl-N,N-dimethylnicotinamide production apparatus according to claim 1 or 2, characterized in that: The nozzle (20) is a hollow structure. The nozzle (20) includes a shell (201). A connecting pipe B (203) is provided on one side of the shell (201). The connecting pipe B (203) is connected to the heat transfer hose (8) through a sealing ring and thread. The dosing hose (4) is connected to the dosing pipe B (21) through a thread and sealing ring. The dosing pipe B (21) extends to the bottom of the shell (201) and extends out of the shell (201). The outer side of the shell (201) is provided with circumferentially distributed heat exchange fins (202). The heat exchange fins (202) are hollow and communicate with the inside of the shell (201). A layer of capillary material (22) is adhered to the inner surface of the heat exchange fins (202), the shell (201), the connecting pipe B (203), the heat transfer hose (8), the connecting pipe A (1801), and the heat exchange head (18). The above space is drawn into a negative pressure state and the above space is filled with working fluid.

4. The high-efficiency 2-aminosulfonyl-N,N-dimethylnicotinamide production apparatus according to claim 1, characterized in that: The outer ring of the turntable bearing (23) is connected to the round hole (603) of the crossbeam (602) by bolts. The inner ring of the turntable bearing (23) is connected to the fixed pulley A (24). The crossbeam (602) is provided with a fixed pulley B (25) outside the round hole (603). The fixed pulley B (25) is located on the upper part of the crossbeam (602).

5. The high-efficiency 2-aminosulfonyl-N,N-dimethylnicotinamide production apparatus according to claim 1, characterized in that: The trolley (9) includes a chassis (901), which is fixedly connected to an electric push rod (7). Two drive wheels (904) are provided on the chassis (901). The drive wheels (904) are connected to a gearbox (903). The gearbox (903) is connected to a motor (902). Two follower wheels (905) are provided on the chassis (901) opposite to the drive wheels (904). The drive wheels (904) and follower wheels (905) are located on both sides of the vertical ribs of the I-beam of the guide rail (6).

6. A high-efficiency 2-aminosulfonyl-N,N-dimethylnicotinamide production apparatus according to claim 1 or 5, characterized in that: The electric push rod (7) is equipped with a limiting ring (702), which is located on the inside of the guide rail (6). The heat transfer hose (8) passes through the limiting ring (702), and the column (601) is located on the outermost ring of the guide rail (6) spiral.

7. The high-efficiency 2-aminosulfonyl-N,N-dimethylnicotinamide production apparatus according to claim 1, characterized in that: The control box (10) has wires connecting the refrigeration unit (15), the motor (902), and the electric push rod (7).

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