Production system of o-nitrobenzenesulfonyl chloride

Abstract

The application discloses a production system of o-nitrobenzenesulfonyl chloride, which comprises an etherification reaction kettle, a material transfer structure, a recrystallization pool, a separation mechanism and a chlorination reaction kettle. The material transfer structure comprises a rotary driving mechanism, a rotating disc and a charging disc. A plurality of rotating rods are fixedly connected to the rotating disc. The bottom of the charging disc is provided with a filter screen. A filtering station, a recrystallization station, a first drying station, a chlorination station, a second drying station and a discharging station are sequentially arranged around the rotating disc. The recrystallization pool is located directly below the recrystallization station. Drying boxes are respectively arranged below the first drying station and the second drying station. The chlorination reaction kettle is located directly below the chlorination station. The production system of o-nitrobenzenesulfonyl chloride realizes continuous and automatic production of o-nitrobenzenesulfonyl chloride through the arrangement of the recrystallization station and the multiple chlorination stations, guarantees the purity and yield of the product and improves the production efficiency.

Description

Technical Field

[0001] The invention belongs to the technical field of chemical industry, and particularly relates to a production system of o-nitrobenzenesulfonyl chloride. Background Art

[0002] o-Nitrobenzenesulfonyl chloride is also known as 2-nitrobenzenesulfonyl chloride. It is brown or yellow needle-shaped crystals with a low boiling point and is soluble in ether. Its application areas can be expanded to medicine, high-end dyes and special materials. The applicant disclosed an industrial production method of o-nitrobenzenesulfonyl chloride in the invention patent application number CN201910418925.0. The process involves etherifying o-nitrochlorobenzene and sodium methyl mercaptide to obtain a filter cake, which is recrystallized in a hydrophilic solvent and then chlorinated in a hydrophilic organic acid solvent to obtain the finished o-nitrobenzenesulfonyl chloride. This process can effectively improve the yield of o-nitrobenzenesulfonyl chloride and make the production process easier to control. However, there is currently no suitable production system that can support production. Summary of the Invention

[0003] In order to solve the above technical problems, the technical solution adopted by the present invention is: a production system of o-nitrobenzenesulfonyl chloride, including an etherification reactor, a material transfer structure, a recrystallization tank, a separation mechanism, and a chlorination reactor.

[0004] The material transfer structure includes a rotary drive mechanism, a turntable, and a loading tray. The rotary drive mechanism drives the turntable to rotate. A plurality of rotating rods are fixedly connected to the turntable. The rotating rods are arranged in a row around the circumference of the turntable. The rotating rods are composed of a first horizontal section, a vertical section, and a second horizontal section connected in sequence. One end of the first horizontal section is fixedly connected to the turntable, and the other end is fixedly connected to the upper end of the vertical section. One end of the second horizontal section is fixedly connected to the lower end of the vertical section, and the other end is fixedly connected to the loading tray. A filter is provided at the bottom of the loading tray.

[0005] The rotating disk is surrounded by a filtering station, a recrystallization station, a first drying station, a chlorination station, a second drying station and a material unloading station. The loading tray is driven by a rotary drive mechanism to move to the filtering station, recrystallization station, drying station, chlorination station and material unloading station in sequence.

[0006] A feed pipe is provided at the bottom of the etherification reaction kettle, and the feed pipe is located just above the filtration station;

[0007] The recrystallization pool is located directly below the recrystallization station, and a pool cover is provided on the recrystallization pool. The recrystallization pool is driven up and down by a lifting drive mechanism;

[0008] A drying box is provided below the first drying station and below the second drying station, respectively. The drying boxes are driven up and down by a lifting mechanism, and the drying boxes respectively include a box body and a movable box cover. A heating device is provided in the box body, and the box body is connected to a vacuum pumping device through a vacuum tube.

[0009] The chlorination reaction kettle is located directly below the chlorination station. The chlorination reaction kettle comprises a kettle body and a kettle cover. The chlorination reaction kettle is driven to rise and fall by a lifting mechanism.

[0010] As a preferred embodiment of the above technical solution, the lower end of the inner part of the loading tray is connected to a support ring, the upper end of the inner part of the loading tray is connected to a limit ring, the filter screen is placed on the support ring around it, and the filter screen is installed between the support ring and the limit ring so that it can rotate and move up and down.

[0011] As a preferred embodiment of the above technical solution, a tray is installed in the drying box, and the tray is driven to rotate by a centrifugal drive mechanism.

[0012] As a preferred embodiment of the above technical solution, the number of the chlorination stations is two, the two chlorination stations are arranged in sequence, and the number of the chlorination reaction kettles is two.

[0013] As a preferred embodiment of the above technical solution, a liquid receiving basin is provided below the filtering station, and a liquid receiving hopper is provided between the filtering station and the etherification reactor.

[0014] As a preferred embodiment of the above technical solution, the recrystallization pool and the pool cover are hinged, and the recrystallization pool and the pool cover are respectively provided with notches, and the notch on the recrystallization pool and the notch on the pool cover are spliced ​​to form a first bayonet for the first horizontal section to pass through; the box body and the movable box cover are hinged, and the box body and the movable box cover are respectively provided with notches, and the notch on the box body and the notch on the movable box cover are spliced ​​to form a second bayonet for the first horizontal section to pass through; the kettle body and the kettle cover are hinged, and the kettle body and the kettle cover are respectively provided with notches, and the notch on the kettle body and the notch on the kettle cover are spliced ​​to form a third bayonet for the first horizontal section to pass through.

[0015] As a preferred embodiment of the above technical solution, there is a sealing gasket at each of the notches.

[0016] As a preferred embodiment of the above technical solution, the number of the rotating rods is six, and the number of the loading trays is six.

[0017] As a preferred embodiment of the above technical solution, the lifting mechanism, the jacking mechanism, and the lifting drive mechanism are respectively cylinders or hydraulic cylinders, the rotation drive mechanism is a motor, and the centrifugal drive mechanism is a motor.

[0018] The beneficial effects of the present invention are as follows: the o-nitrobenzenesulfonyl chloride production system of the present invention realizes continuous and automated production of o-nitrobenzenesulfonyl chloride by arranging a recrystallization station and a multiple chlorination station, thereby ensuring the purity and yield of the product and improving production efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a partial structural schematic diagram of the present invention;

[0020] Figure 2 It is a structural diagram of the material transfer structure;

[0021] Figure 3 It is a structural diagram of the drying oven;

[0022] Figure 4 It is a structural diagram of the chlorination reactor. DETAILED DESCRIPTION

[0023] The technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.

[0024] In the description of the present invention, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings and are intended solely to facilitate and simplify the description of the present invention. They are not intended to indicate or imply that the devices or components referred to must have, be constructed, or operate in a specific orientation, and therefore should not be construed as limitations on the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0025] In the description of the present invention, it should be noted that, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "connected" should be understood in a broad sense. For example, they may refer to fixed, detachable, or integral connections; mechanical or electrical connections; direct or indirect connections through an intermediate medium; and internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on the specific circumstances.

[0026] like Figures 1-4 As shown, the production system of o-nitrobenzenesulfonyl chloride includes an etherification reactor 1, a material transfer structure, a recrystallization tank 2, a separation mechanism, and a chlorination reactor 3.

[0027] The material transfer structure includes a rotary drive mechanism 4, a turntable 5, and a charging tray 9. The rotary drive mechanism 4 drives the turntable 5 to rotate. A number of rotating rods are fixedly connected to the turntable 5. The rotating rods are arranged in a row around the circumference of the turntable 5. The rotating rods are composed of a first horizontal section 6, a vertical section 7, and a second horizontal section 8 connected in sequence. One end of the first horizontal section 6 is fixedly connected to the turntable 5, and the other end is fixedly connected to the upper end of the vertical section 7. One end of the second horizontal section 8 is fixedly connected to the lower end of the vertical section 7, and the other end is fixedly connected to the charging tray 9. A filter screen 10 is provided at the bottom of the charging tray 9.

[0028] The turntable 5 is surrounded by a filtering station 11, a recrystallization station 12, a first drying station 13, a chlorination station 14, a second drying station 15 and a feeding station 16. The loading tray 9 is driven by the rotary drive mechanism 4 to move to the filtering station 11, the recrystallization station 12, the drying station, the chlorination station 14 and the feeding station 16 in sequence.

[0029] A discharge pipe 17 is provided at the bottom of the etherification reactor 1, and is located directly above the filtering station 11. A certain amount of o-nitrochlorobenzene and liquid sodium methyl mercaptide undergo an etherification reaction in the etherification reactor 1. After the reaction is completed, the product is discharged from the discharge pipe 17 and filtered through the filter screen 10 on the loading tray 9 to obtain a filter cake.

[0030] The recrystallization tank 2 is located directly below the recrystallization station 12. A tank cover 18 is provided on the recrystallization tank 2, which is driven up and down by a lifting drive mechanism 19. A hydrophilic alcohol solvent (methanol, ethanol, propanol, or ethylene glycol) is contained in the recrystallization tank 2. The tank cover 18 is opened, and the lifting drive mechanism 19 drives the recrystallization tank 2 to rise, allowing the charging tray 9 to enter the recrystallization tank 2 and be immersed below the liquid level of the hydrophilic alcohol solvent. The tank cover 18 is closed, and the filter cake is recrystallized in the hydrophilic alcohol solvent. After completion, the tank cover 18 is opened, and the recrystallization tank 2 descends, and the filter cake is dried automatically after waiting for a period of time.

[0031] Drying boxes are provided below the first drying station 13 and below the second drying station 15, respectively. The drying boxes are driven up and down by a lifting mechanism 20, and the drying boxes include a box body 21 and a movable box cover 22. A heating device is provided in the box body 21, and the box body 21 is connected to the vacuum equipment through a vacuum tube 23. The lifting mechanism 20 drives the drying box to rise, so that the loading tray 9 at this station enters the box body 21. Then the movable box cover 22 is closed tightly. The heating device starts heating, and at the same time the vacuum equipment is turned on to vacuum the drying box, so that the moisture and other gases in the drying box are quickly separated from the filter cake. After the drying is completed, the movable box cover 22 is opened, the box body 21 descends, and the loading tray 9 rotates and moves to the next station.

[0032] The chlorination reactor 3 is located directly below the chlorination station 14, and the chlorination reactor 3 includes a kettle body and a kettle cover 24, and is driven to rise by a lifting mechanism. The kettle cover 24 is provided with a cover net 35. After the charging tray 9 is rotated to the chlorination station 14, the chlorination reactor 3 rises, so that part of the first horizontal section 6 and the entire vertical section 7 and the entire second horizontal section 8 extend into the chlorination reactor 3. Then the kettle cover 24 is tightly covered, and the cover net 35 covers the upper end of the charging tray 9, so that the filter cake is clamped between the cover net 35 and the filter screen 10, and a closed reaction space is formed in the chlorination reactor 3. The chlorination reactor 3 is filled with a hydrophilic organic acid solvent. During the chlorination reaction, chlorine gas is filled at the bottom of the chlorination reactor 3. The kettle cover 24 is connected to a chlorine gas collection tank through a chlorine gas recovery pipe, and a gas pump is installed on the chlorine gas recovery pipe. The excess chlorine gas is recovered and reused. After the chlorination reaction is completed, the kettle cover 24 is opened, the chlorination reactor 3 is lowered, and after a period of time, the charging tray 9 is rotated and moved to the next station.

[0033] Further, the inside lower end of the charging tray 9 is connected with a supporting ring 25, and the inside upper end of the charging tray 9 is connected with a limiting ring 26, the filter screen 10 is arranged around the supporting ring 25, and the filter screen 10 is rotatably and movably arranged between the supporting ring 25 and the limiting ring 26.

[0034] Further, the drying box is provided with a tray 27, and the tray 27 is driven to rotate by a centrifugal driving mechanism 28. After the drying box rises, the tray 27 supports the filter screen 10, so that the filter screen 10 is separated from the supporting ring 25. Then the centrifugal driving mechanism 28 drives the tray 27 to rotate the filter screen 10, and further drives the filter cake on the filter screen 10 to rotate, so that the internal liquid is quickly spun dry under the action of centrifugal force. At the same time, the filter cake is separated from the charging tray 9 before drying, so as to reduce the adhesion phenomenon, ensure the full progress of the subsequent chlorination reaction, facilitate the discharging and continuous production.

[0035] Further, the number of chlorination stations 14 is two, and the two chlorination stations 14 are arranged in sequence, and the number of chlorination reactors 3 is two. The first chlorination reaction and the second chlorination reaction are sequentially performed in the two chlorination reactors 3, so as to ensure the product purity.

[0036] Further, the filtering station 11 is provided below with a liquid receiving basin 29, and the filtering station 11 and the etherification reactor 1 are provided with a liquid receiving hopper 30. After the etherification reactor 1 is completed, the reaction product is received by the liquid receiving hopper 30, filtered by the filter screen 10 on the charging tray 9, so as to realize solid-liquid separation. The liquid part is received by the liquid receiving basin 29 and reused.

[0037] Furthermore, the recrystallization tank 2 is hingedly connected to the tank cover 18, and each of the recrystallization tank 2 and the tank cover 18 is provided with a notch. The notch on the recrystallization tank 2 and the notch on the tank cover 18 are spliced ​​to form a first slot for the first horizontal section 6 to pass through. The box body 21 and the movable box cover 22 are hingedly connected, and each of the box body 21 and the movable box cover 22 is provided with a notch. The notch on the box body 21 and the notch on the movable box cover 22 are spliced ​​to form a second slot for the first horizontal section 6 to pass through. The kettle body and the kettle cover 24 are hingedly connected, and each of the kettle body and the kettle cover 24 is provided with a notch. The notch on the kettle body and the notch on the kettle cover 24 are spliced ​​to form a third slot for the first horizontal section 6 to pass through. The recrystallization process, drying process, and chlorination process are all carried out in a relatively closed environment to reduce gas overflow and ensure a stable reaction environment.

[0038] Furthermore, the notches are all provided with sealing gaskets, which can fully ensure the airtightness during the reaction and drying processes.

[0039] Furthermore, the number of the rotating rods is six, and the number of the loading trays 9 is six. The six workstations simultaneously carry out corresponding processing processes, so that the entire production system forms continuous production.

[0040] Furthermore, the lifting mechanism, the jacking mechanism 20, and the lifting drive mechanism 19 are respectively cylinders or hydraulic cylinders, the rotation drive mechanism 4 is a motor, and the centrifugal drive mechanism 28 is a motor. Other existing drive mechanisms that can play the same role can also be used instead.

[0041] It is worth mentioning that the technical features such as motors, cylinders, reactors involved in the patent application of this invention should be regarded as prior art. The specific structure, working principle and possible control method and spatial layout method of these technical features can be selected by conventional means in the field and should not be regarded as the inventive point of this patent. This patent will not be further elaborated.

[0042] The above describes in detail the preferred specific embodiments of the present invention. It should be understood that ordinary technicians in this field can make many modifications and changes based on the concept of the present invention without creative work. Therefore, any technical solutions that can be obtained by technicians in this technical field through logical analysis, reasoning or limited experiments based on the concept of the present invention on the basis of existing technologies should be within the scope of protection determined by the claims.

Claims

1. A production system for o-nitrobenzenesulfonyl chloride, characterized in that: It includes etherification reactor, material transfer structure, recrystallization tank, separation mechanism, chlorination reactor, The material transfer structure includes a rotary drive mechanism, a turntable, and a loading tray. The rotary drive mechanism drives the turntable to rotate. A plurality of rotating rods are fixedly connected to the turntable. The rotating rods are arranged in a row around the circumference of the turntable. The rotating rods are composed of a first horizontal section, a vertical section, and a second horizontal section connected in sequence. One end of the first horizontal section is fixedly connected to the turntable, and the other end is fixedly connected to the upper end of the vertical section. One end of the second horizontal section is fixedly connected to the lower end of the vertical section, and the other end is fixedly connected to the loading tray. A filter is provided at the bottom of the loading tray. The rotating disk is surrounded by a filtering station, a recrystallization station, a first drying station, a chlorination station, a second drying station and a material unloading station. The loading tray is driven by a rotary drive mechanism to move to the filtering station, the recrystallization station, the first drying station, the chlorination station, the second drying station and the material unloading station in sequence. A feed pipe is provided at the bottom of the etherification reaction kettle, and the feed pipe is located just above the filtration station; The recrystallization pool is located directly below the recrystallization station, and a pool cover is provided on the recrystallization pool. The recrystallization pool is driven up and down by a lifting drive mechanism; A drying box is provided below the first drying station and below the second drying station, respectively. The drying boxes are driven up and down by a lifting mechanism, and the drying boxes respectively include a box body and a movable box cover. A heating device is provided in the box body, and the box body is connected to a vacuum pumping device through a vacuum tube. The chlorination reaction kettle is located directly below the chlorination station. The chlorination reaction kettle includes a kettle body and a kettle cover. The chlorination reaction kettle is driven to rise and fall by a lifting mechanism. The lower end of the inner part of the charging tray is connected to a support ring, and the upper end of the inner part of the charging tray is connected to a limit ring. The filter screen is placed on the support ring all around. The filter screen can be rotatably and moved up and down between the support ring and the limit ring. A tray is installed in the drying box, and the tray is driven to rotate by a centrifugal drive mechanism. There are two chlorination stations, and the two chlorination stations are arranged in sequence. There are two chlorination reaction kettles. A liquid receiving basin is provided below the filtration station, and a liquid receiving hopper is provided between the filtration station and the etherification reaction kettle.

2. The production system of o-nitrobenzenesulfonyl chloride as claimed in claim 1, wherein The recrystallization pool and the pool cover are hinged, and the recrystallization pool and the pool cover are respectively provided with notches, and the notch on the recrystallization pool and the notch on the pool cover are spliced ​​to form a first bayonet for the first horizontal section to pass through; the box body and the movable box cover are hinged, and the box body and the movable box cover are respectively provided with notches, and the notch on the box body and the notch on the movable box cover are spliced ​​to form a second bayonet for the first horizontal section to pass through; the kettle body and the kettle cover are hinged, and the kettle body and the kettle cover are respectively provided with notches, and the notch on the kettle body and the notch on the kettle cover are spliced ​​to form a third bayonet for the first horizontal section to pass through.

3. The production system of o-nitrobenzenesulfonyl chloride as claimed in claim 2, wherein The notches are all provided with sealing pads.

4. The production system of o-nitrobenzenesulfonyl chloride as claimed in claim 3, wherein The number of the rotating rods is six, and the number of the loading trays is six.

5. The production system of o-nitrobenzenesulfonyl chloride as claimed in claim 4, wherein The lifting mechanism, jacking mechanism, and lifting drive mechanism are respectively cylinders or hydraulic cylinders, the rotation drive mechanism is a motor, and the centrifugal drive mechanism is a motor.

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