Distillation device for producing bis (chlorosulfonyl) imide

Abstract

The utility model discloses a distillation device for producing bis (chlorosulfonyl) imide, which belongs to the technical field of chemical equipment and comprises a crude product tank I, a primary distillation separation component, a crude product tank II and a secondary distillation separation component, materials in the crude product tank I are conveyed to the primary distillation separation component through a primary conveying component, and materials in the crude product tank II are conveyed to the secondary distillation separation component through a secondary conveying component. Thionyl chloride and chlorosulfonic acid mixed in the materials are sequentially separated out through the first-stage distillation separation assembly and stored in a thionyl chloride turnover tank and a chlorosulfonic acid turnover tank; and the material subjected to primary distillation separation enters a crude product II tank, and is conveyed to a secondary distillation separation assembly through a secondary conveying assembly, so that the finished product bis (chlorosulfonyl) imide can be separated and stored in a finished product tank. According to the utility model, thionyl chloride and chlorosulfonic acid in reaction products can be separated through two times of distillation, so that the waste of raw materials is reduced; and further rectifying the finished product to obtain a bis (chlorosulfonyl) imide finished product with relatively high purity.

Description

Technical Field

[0001] This utility model belongs to the field of chemical equipment technology, and specifically relates to a distillation apparatus for the production of dichlorosulfonamide. Background Technology

[0002] Dichlorosulfonyl imide is a common organic synthetic intermediate widely used in pesticides, pharmaceuticals, dyes, and other fields, possessing high economic value. Dichlorosulfonyl imide is synthesized from thionyl chloride, chlorosulfonic acid, and aminosulfonic acid, and the reaction process is as follows:

[0003] 2SOCl2 + ClSO3H + NH2SO3H Cl2HNO4S2+2SO2 +3HCl .

[0004] In the production of bischlorosulfonylimide, thionyl chloride, aminosulfonic acid, and chlorosulfonic acid are mixed and reacted at a suitable temperature to obtain bischlorosulfonylimide. Because the reactants contain a certain amount of thionyl chloride, the purity of the final product, bischlorosulfonylimide, is poor, and thionyl chloride is wasted. Therefore, it is necessary to develop a production process to recover thionyl chloride, reduce resource waste, and improve the purity of the final bischlorosulfonylimide. Utility Model Content

[0005] To address the above problems, this invention provides a distillation apparatus for the production of dichlorosulfonylimide.

[0006] To achieve the above objectives, the technical solution adopted by this utility model is as follows:

[0007] A distillation apparatus for producing dichlorosulfonamide includes a crude product tank I, a primary distillation separation component, a crude product tank II, and a secondary distillation separation component. The crude product tank I is used to contain materials discharged from the synthesis process. The outlet of the crude product tank I is connected to the inlet of the primary distillation separation component via a primary conveying component. The primary distillation separation component is used to sequentially separate thionyl chloride and chlorosulfonic acid from the material and store them in thionyl chloride and chlorosulfonic acid transfer tanks, respectively. The material from the primary distillation separation component enters the crude product tank II, which is connected to the secondary distillation separation component via a secondary conveying component. The secondary distillation separation component is used to separate the finished dichlorosulfonamide and store it in the finished product tank.

[0008] Furthermore, the primary distillation separation assembly includes a primary distiller, a primary separator, and a primary distillation heat exchanger. The top of the primary distiller is connected to the bottom of the primary separator. The top side of the primary distiller is provided with a material inlet connected to the primary conveying assembly, and the bottom is provided with a discharge port connected to a magnetic pump. The outlet of the magnetic pump is connected to a reflux pipe and a feed pipe, respectively. The feed pipe is connected to the crude product tank II, and the other end of the reflux pipe is connected to the top of the primary separator. The lower part of the primary separator is connected to the bottom of the primary distillation heat exchanger. The top outlet of the primary distillation heat exchanger is connected to a condenser. The bottom outlet of the condenser is connected to a thionyl chloride transfer tank. The bottom outlet pipe of the condenser is connected to a chlorosulfonic acid transfer tank through a bypass pipe. The outlet of the condenser is connected to a tail gas treatment system.

[0009] Furthermore, there are two condensers, namely condenser I and condenser II. The top air inlet of condenser I is connected to the top air outlet of the first-stage distillation heat exchanger through an air inlet pipe, and a thermometer and a pressure sensor are installed on the air inlet pipe. The lower outlet of condenser I is connected to the lower inlet of condenser II. The top exhaust pipe of condenser II is connected to the tail gas treatment system through vacuum pump I, and a thermometer is installed on the exhaust pipe. The bottom outlets of the two condensers are respectively connected to two thionyl chloride transfer tanks. The lower part of condenser I and condenser II are provided with a cooling medium inlet, and the upper part is provided with a cooling medium outlet.

[0010] Furthermore, the bottom discharge pipe of the condenser I is equipped with two bypass pipes, one of which is connected to the chlorosulfonic acid transfer tank and the other of which is connected to the crude product I tank.

[0011] Furthermore, the secondary distillation separation assembly includes a secondary distiller, a secondary separator, and a secondary distillation heat exchanger. The top of the secondary distiller is connected to the bottom of the secondary separator. The top side of the secondary distiller has a material inlet connected to the secondary conveying assembly, and the bottom has a discharge port connected to a magnetic pump. The outlet of the magnetic pump is connected to the top of the secondary separator via a circulation pipe. The lower part of the secondary separator is connected to the bottom of the secondary distillation heat exchanger. The top outlet of the secondary distillation heat exchanger is connected to the top inlet pipe of condenser III, and a thermometer and a pressure sensor are installed on the inlet pipe. The bottom outlet of condenser III is connected to the finished product tank, and the exhaust port of the finished product tank is connected to vacuum pump II. The lower part of condenser III has a cooling medium inlet, and the upper part has a cooling medium outlet.

[0012] Furthermore, a check valve is installed at the outlet of the vacuum pump II. The discharge port of the finished product tank is connected to the magnetic pump, and a check valve is also installed at the discharge port of the magnetic pump. By installing the check valve, air can be prevented from entering the finished product tank and causing contamination after the pump stops.

[0013] Furthermore, the primary conveying component and the secondary conveying component have the same structure, both including a magnetic pump and a conveying pipe. The conveying pipe is equipped with a control valve that can be linked with the magnetic pump to control the feed rate of the primary distillation separation component and the secondary distillation separation component.

[0014] Furthermore, both the crude product tank I and crude product tank II are equipped with heat-insulating coils inside.

[0015] The technological advancements achieved by this invention compared to existing technologies are as follows:

[0016] This invention uses a primary conveying assembly to transport the material from crude product tank I to a primary distillation separation assembly, which sequentially separates and stores the thionyl chloride and chlorosulfonic acid mixtures in the material in thionyl chloride and chlorosulfonic acid transfer tanks, respectively. The material after primary distillation then enters crude product tank II, and is further conveyed to a secondary distillation separation assembly via a secondary conveying assembly, where the finished product, dichlorosulfonylimide, is separated and stored in a finished product tank. This invention achieves separation of thionyl chloride and chlorosulfonic acid from the reaction products through two distillations, and further refines the finished product to obtain a high-purity dichlorosulfonylimide. This invention also recovers thionyl chloride and chlorosulfonic acid from the material, reducing raw material waste and lowering production costs. Attached Figure Description

[0017] The accompanying drawings are provided to further understand the present invention and form part of the specification. They are used together with the embodiments of the present invention to explain the present invention and do not constitute a limitation thereof.

[0018] In the attached diagram:

[0019] Figure 1 A schematic diagram of a distillation apparatus for producing dichlorosulfonylimide is provided for an embodiment of this utility model;

[0020] In the picture:

[0021] 301-Crude Product Tank I; 302-Crude Product Tank II; 303-Thionyl Chloride Transfer Tank; 304-Chlorosulfonic Acid Transfer Tank; 305-Finished Product Tank; 307-First-Stage Separator; 308-First-Stage Distillation Heat Exchanger; 309-Reflux Pipe; 310-Discharge Pipe; 311-Vacuum Pump I; 312-Bypass Pipe; 313-Second-Stage Distiller; 314-Second-Stage Separator; 315-Second-Stage Distillation Heat Exchanger; 316-Circulation Pipe; 317-Vacuum Pump II; 21-Condenser I; 22-Condenser II; 23-Condenser III. Detailed Implementation

[0022] The following specific embodiments can be combined with each other, and the same or similar concepts or processes may not be described again in some embodiments. The embodiments of this utility model will be described below with reference to the accompanying drawings.

[0023] like Figure 1 As shown, a distillation apparatus for the production of dichlorosulfonamide is disclosed. The distillation apparatus includes a crude product tank I 301, a primary distillation separation component, a crude product tank II 302, and a secondary distillation separation component. The crude product tank I 301 is connected to the outlet of an insulated tank 202 and is used to contain the material discharged from the synthesis process. The outlet of the crude product tank I 301 is connected to the inlet of the primary distillation separation component via a primary conveying component. The primary distillation separation component is used to sequentially separate thionyl chloride and chlorosulfonic acid from the material and store them in a thionyl chloride transfer tank 303 and a chlorosulfonic acid transfer tank 304. The material from the primary distillation separation component enters the crude product tank II 302, which is connected to the secondary distillation separation component via a secondary conveying component. The secondary distillation separation component is used to separate the finished dichlorosulfonamide and store it in a finished product tank 305. The crude product tank contains crude dichlorosulfonamide doped with chlorosulfonic acid and thionyl chloride. The chlorosulfonic acid and thionyl chloride can be distilled out separately by the primary distillation separation unit, and then the dichlorosulfonamide is distilled out by the secondary distillation separation unit.

[0024] In a specific embodiment of this utility model, the primary distillation separation assembly includes a primary distiller 306, a primary separator 307, and a primary distillation heat exchanger 308. The top of the primary distiller 306 is connected to the bottom of the primary separator 307. The top side of the primary distiller 306 is provided with a material inlet connected to the primary conveying assembly, and the bottom is provided with a discharge port connected to the magnetic pump 1. The outlet of the magnetic pump 1 is connected to the reflux pipe 309 and the feed pipe 310, respectively. The feed pipe 310 is connected to the coarse feed pipe 308. The product is connected to tank 302, and the other end of the reflux pipe 309 is connected to the top of the primary separator 307; the lower part of the primary separator 307 is connected to the bottom of the primary distillation heat exchanger 308, the top outlet of the primary distillation heat exchanger 308 is connected to condenser 2, the bottom outlet of condenser 2 is connected to thionyl chloride transfer tank 303, the bottom outlet pipe of condenser 2 is connected to chlorosulfonic acid transfer tank 304 through a bypass pipe, and the outlet of condenser 2 is connected to the tail gas treatment system. Through the aforementioned primary distillation separation assembly, thionyl chloride is first distilled at 125±2℃ (vacuum degree ≤20 kPa), and then condensed by a condenser into a thionyl chloride transfer tank 303. From there, it is pumped from the transfer tank to a thionyl chloride storage tank for recycling and reuse. After distillation until no liquid is produced, the temperature is raised to 130±2℃ (vacuum degree ≤5 kPa), and chlorosulfonic acid begins to distill out. This chlorosulfonic acid is then condensed by a condenser into a chlorosulfonic acid transfer tank 304, and from there, it is pumped from the transfer tank to a chlorosulfonic acid storage tank for recycling and reuse.

[0025] The condenser 2 consists of two units: condenser I 21 and condenser II 22. The top inlet of condenser I 21 is connected to the top outlet of the first-stage distillation heat exchanger 308 via an inlet pipe, which is equipped with a thermometer and a pressure sensor. The bottom outlet of condenser I 21 is connected to the bottom inlet of condenser II 22. The top exhaust pipe of condenser II 22 is connected to the tail gas treatment system via a vacuum pump I 311, and this exhaust pipe is equipped with a thermometer. The bottom outlets of condensers I 21 and II 22 are respectively connected to two thionyl chloride transfer tanks 303. Both condensers I 21 and II 22 have cooling medium inlets at the bottom and cooling medium outlets at the top. Based on the different boiling points of thionyl chloride and chlorosulfonic acid, thionyl chloride and chlorosulfonic acid are cooled and condensed, then fed into thionyl chloride transfer tank 303 and chlorosulfonic acid transfer tank 304, respectively.

[0026] In the specific design, the bottom discharge pipe of the condenser I 21 is equipped with two bypass pipes 312. One bypass pipe 312 is connected to the chlorosulfonic acid turnover tank 304, and the other bypass pipe 312 is connected to the crude product tank I 301. This allows the material discharged from the condenser I to return to the crude product tank I and continue to participate in distillation, thereby increasing the yield of dichlorosulfonamide.

[0027] In a specific embodiment of this utility model, the secondary distillation separation assembly includes a secondary distiller 313, a secondary separator 314, and a secondary distillation heat exchanger 315. The top of the secondary distiller 313 is connected to the bottom of the secondary separator 314. The top side of the secondary distiller 314 has a material inlet connected to the secondary conveying assembly, and the bottom has a discharge port connected to the magnetic pump 1. The outlet of the magnetic pump 1 is connected to the top of the secondary separator 314 through a circulation pipe 316. The lower part of the secondary separator 314 is connected to the bottom of the secondary distillation heat exchanger 315. The top outlet of the secondary distillation heat exchanger 315 is connected to the top inlet pipe of the condenser III 23, and the inlet pipe is equipped with a thermometer and a pressure sensor. The bottom outlet of the condenser III 23 is connected to the finished product tank 305, and the exhaust port of the finished product tank 305 is connected to the vacuum pump II 317. The lower part of the condenser III has a cooling medium inlet, and the upper part has a cooling medium outlet. The above-mentioned two-stage distillation separation unit can distill off the dichlorosulfonamide in the residue to obtain a high-purity dichlorosulfonamide product.

[0028] In the specific design, the outlet of the vacuum pump II 317 is equipped with a check valve. The discharge port of the finished product tank 305 is connected to the magnetic pump 1, and a check valve is also installed at the discharge port of the magnetic pump 1. By installing the check valve, air can be prevented from entering the finished product tank and causing contamination after the pump stops.

[0029] The primary and secondary conveying components have identical structures, both including a magnetic pump 1 and a conveying pipe. The conveying pipe is equipped with a control valve that can be linked to the magnetic pump 1 to control the feed rate to both the primary and secondary distillation separation components. Simultaneously, both crude product tank I 301 and crude product tank II 302 are equipped with insulation coils to preheat the material temperature to the process requirements, thereby reducing the heating time required during distillation and improving production efficiency.

[0030] In the actual production process, the mass percentages of the components in the crude product in crude product tank I are as follows: 55-60% dichlorosulfonyl imide, 30-35% thionyl chloride, and 2-5% chlorosulfonic acid. After distillation by the primary distillation separation unit, the crude product entering crude product tank II contains dichlorosulfonyl imide with impurities. After distillation by the secondary distillation separation unit, the residue remaining in the secondary distillation apparatus is still residue.

[0031] In summary, this invention has the advantages of reasonable structural design and good structural continuity. The thionyl chloride and chlorosulfonic acid mixed in the dichlorosulfonylimide are separated sequentially by primary distillation and stored in thionyl chloride and chlorosulfonic acid transfer tanks for easy recycling. The remaining material is then transported to a secondary distillation separation unit, where the finished dichlorosulfonylimide is separated and stored in a finished product tank, yielding a high-purity dichlorosulfonylimide product. This invention enables the separation of thionyl chloride and chlorosulfonic acid from the reaction products through two distillations, and further purification of the finished product by distillation. This invention can recover thionyl chloride and chlorosulfonic acid from the material, reducing raw material waste, lowering production costs, and increasing the product yield.

[0032] Finally, it should be noted that the above description is merely a preferred embodiment of this utility model and is not intended to limit the utility model. Although the utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this utility model should be included within the scope of protection of the claims of this utility model.

Claims

1. A distillation apparatus for the production of dichlorosulfonylimide, characterized in that: The system includes a crude product tank I, a primary distillation separation unit, a crude product tank II, and a secondary distillation separation unit. The crude product tank I is used to contain the material discharged from the synthesis process. The outlet of the crude product tank I is connected to the inlet of the primary distillation separation unit via a primary conveying unit. The primary distillation separation unit is used to sequentially separate thionyl chloride and chlorosulfonic acid from the material and store them in thionyl chloride and chlorosulfonic acid transfer tanks, respectively. The material from the primary distillation separation unit enters the crude product tank II, which is connected to the secondary distillation separation unit via a secondary conveying unit. The secondary distillation separation unit is used to separate the finished product, dichlorosulfonamide, and store it in the finished product tank.

2. The distillation apparatus for producing dichlorosulfonylimide according to claim 1, characterized in that: The primary distillation separation assembly includes a primary distiller, a primary separator, and a primary distillation heat exchanger. The top of the primary distiller is connected to the bottom of the primary separator. The top side of the primary distiller has a material inlet connected to the primary conveying assembly, and the bottom has a discharge port connected to a magnetic pump. The outlet of the magnetic pump is connected to a reflux pipe and a feed pipe, respectively. The feed pipe is connected to the crude product tank II, and the other end of the reflux pipe is connected to the top of the primary separator. The lower part of the primary separator is connected to the bottom of the primary distillation heat exchanger. The top outlet of the primary distillation heat exchanger is connected to a condenser. The bottom outlet of the condenser is connected to a thionyl chloride transfer tank. The bottom outlet pipe of the condenser is connected to a chlorosulfonic acid transfer tank through a bypass pipe. The outlet of the condenser is connected to a tail gas treatment system.

3. The distillation apparatus for producing dichlorosulfonylimide according to claim 2, characterized in that: There are two condensers, namely condenser I and condenser II. The top air inlet of condenser I is connected to the top air outlet of the first-stage distillation heat exchanger through an air inlet pipe, and a thermometer and a pressure sensor are installed on the air inlet pipe. The bottom outlet of condenser I is connected to the bottom inlet of condenser II. The top exhaust pipe of condenser II is connected to the tail gas treatment system through vacuum pump I, and a thermometer is installed on the exhaust pipe. The bottom outlets of the two condensers are respectively connected to two thionyl chloride transfer tanks.

4. The distillation apparatus for producing dichlorosulfonylimide according to claim 3, characterized in that: The bottom discharge pipe of the condenser I is equipped with two bypass pipes, one of which is connected to the chlorosulfonic acid transfer tank and the other of which is connected to the crude product I tank.

5. A distillation apparatus for producing dichlorosulfonylimide according to claim 1, characterized in that: The secondary distillation separation assembly includes a secondary distiller, a secondary separator, and a secondary distillation heat exchanger. The top of the secondary distiller is connected to the bottom of the secondary separator. The top side of the secondary distiller has a material inlet connected to the secondary conveying assembly, and the bottom has a discharge port connected to a magnetic pump. The outlet of the magnetic pump is connected to the top of the secondary separator through a circulation pipe. The lower part of the secondary separator is connected to the bottom of the secondary distillation heat exchanger. The top outlet of the secondary distillation heat exchanger is connected to the top inlet pipe of condenser III, and a thermometer and a pressure sensor are installed on the inlet pipe. The bottom outlet of condenser III is connected to the finished product tank, and the exhaust port of the finished product tank is connected to vacuum pump II.

6. A distillation apparatus for producing dichlorosulfonylimide according to claim 5, characterized in that: The outlet of the vacuum pump II is equipped with a check valve.

7. A distillation apparatus for producing dichlorosulfonylimide according to claim 1, characterized in that: The primary and secondary conveying components have the same structure, both including a magnetic pump and a conveying pipe. The conveying pipe is equipped with a control valve that can be linked with the magnetic pump to control the feed rate of the primary and secondary distillation separation components.

8. A distillation apparatus for producing dichlorosulfonylimide according to any one of claims 1-7, characterized in that: Both crude product tank I and crude product tank II are equipped with heat-insulating coils inside.

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