Continuous reaction device for producing bis (chlorosulfonyl) imide

Abstract

The utility model discloses a continuous reaction device for producing bis (chlorosulfonyl) imide, which belongs to the technical field of chemical equipment and comprises a horizontal reaction tank and a heat preservation tank, a feed port of the reaction tank is connected with a mixed feed liquid pipe, and a discharge port of the reaction tank is connected with the heat preservation tank through a conveying component; heating layers are arranged outside the reaction tank and the heat preservation tank, a plurality of communicated areas are arranged in the reaction tank and the heat preservation tank, a stirrer is arranged in each area, and a chlorosulfonic acid feeding hole is formed in the top of each area of the reaction tank; a discharge hole of the heat preservation tank is connected with the distillation device; exhaust pipes and condensation reflux assemblies are arranged at the tops of the reaction tank and the heat preservation tank. The chlorosulfonic acid is added into each area of the reaction tank in a multi-drop mode, the reaction tank heats materials through the heat preservation layer to ensure the temperature needed by reaction, and the materials enter the heat preservation tank to be subjected to continuous heat preservation to ensure full reaction of the materials; thionyl chloride in gas exhausted from the reaction tank and the heat preservation tank is cooled and recycled through the condensation backflow assembly, the production efficiency is improved, raw material waste is reduced, and the production cost is reduced.

Description

Technical Field

[0001] This utility model belongs to the field of chemical equipment technology, and specifically relates to a continuous reaction device for the production of dichlorosulfonylimide. 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 process of dichlorosulfonylimide, thionyl chloride, aminosulfonic acid and chlorosulfonic acid need to be mixed and reacted at a suitable temperature to obtain dichlorosulfonylimide.

[0005] Currently, existing reaction equipment uses a reactor. Chlorosulfonic acid, aminosulfonic acid, and thionyl chloride are added sequentially to the reactor, followed by stirring and heating. The materials react within the reactor to produce dichlorosulfonylimide. This production method is batch production; the materials react and heat simultaneously within the reactor before being transferred to subsequent processes. This production model suffers from incomplete reactions and low production efficiency, making continuous production impossible. Utility Model Content

[0006] To address the above problems, this invention provides a continuous reaction apparatus for the production of dichlorosulfonylimide.

[0007] To achieve the above objectives, the technical solution adopted by this utility model is as follows:

[0008] A continuous reaction apparatus for the production of dichlorosulfonamide includes a horizontally placed reaction vessel and an insulated vessel. The inlet of the reaction vessel is connected to a mixed liquid pipe, and the outlet of the reaction vessel is connected to the insulated vessel via a conveying assembly. The reaction vessel and the insulated vessel are sequentially divided into multiple interconnected regions, each region being equipped with a stirrer. Each region of the reaction vessel has a chlorosulfonic acid inlet at its top. The outer walls of both the reaction vessel and the insulated vessel are equipped with heating layers. The outlet of the insulated vessel is connected to a distillation device for the purification process. The tops of both the reaction vessel and the insulated vessel are equipped with exhaust pipes and condensation reflux assemblies.

[0009] Furthermore, the reaction vessel is equipped with multiple baffles and baffles spaced along its length, with the baffles and baffles arranged alternately. The upper end of the baffle is connected to the top wall of the reaction vessel, and the lower end has a gap with the bottom of the reaction vessel. The lower end of the baffle is connected to the bottom of the reaction vessel, and the upper end has a gap with the top wall of the reaction vessel. The reaction vessel is divided into several regions by the baffles and baffles. Each region is equipped with a thermometer and a stirrer, and each region has an exhaust pipe at its top. The internal structure of the insulation tank is the same as that of the reaction vessel. Both the reaction vessel and the insulation tank have discharge pipes at their bottoms.

[0010] Furthermore, the chlorosulfonic acid inlet at the top of the reaction vessel is connected to a feed branch pipe, which is equipped with a control valve and a flow meter. Multiple feed branch pipes are connected in parallel with the main feed pipe. The main feed pipe is connected to the bottom outlet of the chlorosulfonic acid storage tank via a magnetic pump.

[0011] Furthermore, the mixing liquid pipe is connected to the outlet of the mixing tank. The thionyl chloride in the thionyl chloride storage tank is transported to the mixing tank through a magnetic pump and a conveying pipe. The mixing tank is equipped with a stirrer and its top is connected to a compressed air pipe. A lifting device is provided above the mixing tank. The lifting device is used to lift the aminosulfonic acid packaging bag and add aminosulfonic acid to the mixing tank.

[0012] Furthermore, an intermediate tank equipped with a stirrer is provided between the mixing tank and the chemical tank. The inlet end of the discharge pipe of the mixing tank extends downward to near the bottom of the mixing tank, and the outlet end of the discharge pipe is connected to the top of the intermediate tank. The inlet end of the discharge pipe of the intermediate tank extends downward to near the bottom of the intermediate tank, and the outlet end of the discharge pipe extends into the chemical tank and near the bottom of the chemical tank. The discharge pipes between the mixing tank and the intermediate tank, and between the intermediate tank and the chemical tank, are all inclined downward along the direction of liquid flow.

[0013] Furthermore, the internal structure of the chemical tank is the same as that of the reaction vessel, both being divided into several areas by baffles and deflectors. Each area is equipped with a thermometer and a stirrer. The exhaust pipe at the top of each area is connected in parallel with the main pipe. The main pipe is equipped with a control valve and a pressure sensor linked to it. The pressure sensor is used to detect the pressure inside the chemical tank.

[0014] Furthermore, the condensation reflux assembly includes a condenser and a low-temperature heat exchanger. Multiple exhaust pipes at the top of the reaction vessel and the insulation tank are respectively connected to multiple condensers. The bottom discharge pipes of the multiple condensers are respectively connected to the top of the reaction vessel and the insulation tank. The top outlet of the condenser is connected to the exhaust manifold. The exhaust manifold is connected to the lower inlet of the low-temperature heat exchanger. The bottom outlet of the low-temperature heat exchanger is connected to the top of the reaction vessel. The top outlet of the low-temperature heat exchanger is connected to the tail gas pipe. The top outlets of both the condenser and the low-temperature heat exchanger are equipped with thermometers.

[0015] Furthermore, the top outlet pipes of the condenser and the low-temperature heat exchanger are equipped with control valves and pressure sensors linked to them. The pressure sensors are used to detect the outlet pressure of the condenser and the low-temperature heat exchanger.

[0016] The technological advancements achieved by this invention compared to existing technologies are as follows:

[0017] This invention divides a horizontally placed reaction vessel and insulation tank into multiple interconnected areas. Each area of ​​the reaction vessel has a chlorosulfonic acid inlet at its top, allowing for multi-point dripping of chlorosulfonic acid. An external insulation layer heats the materials inside the reaction vessel to ensure the required reaction temperature. The materials then enter the insulation tank for continuous temperature maintenance, ensuring complete reaction. Simultaneously, a condensation reflux assembly cools and recovers thionyl chloride from the exhaust gases of the reaction vessel and insulation tank, further improving the utilization rate of thionyl chloride and thus increasing production output. This invention enables continuous reaction, improves production efficiency, reduces raw material waste, and lowers production costs. Attached Figure Description

[0018] 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.

[0019] In the attached diagram:

[0020] Figure 1 A schematic diagram of a continuous reaction apparatus for the production of dichlorosulfonylimide provided in this embodiment of the present invention;

[0021] Figure 2 for Figure 1 Schematic diagram of the structure of Sinochem's material tank;

[0022] Figure 3 for Figure 1 Schematic diagram of the structure of the intermediate reaction vessel;

[0023] In the picture:

[0024] 1-Magnetic pump; 2-Condenser; 3-Low-temperature heat exchanger; 4-Exhaust main pipe; 5-Baffle; 6-Baffle plate; 7-Discharge pipe; 8-Tail gas pipe; 9-Control valve; 10-Pressure sensor; 11-Thermometer; 12-Agitator; 13-Level gauge; 14-Flow meter;

[0025] 101-Thionyl chloride storage tank; 102-Chlorosulfonic acid storage tank; 103-Battery mixing tank; 104-Chemical tank; 105-Lifting tool; 106-Compressed air pipe; 107-Vacuum phase condenser; 108-Transfer pump; 109-Intermediate tank; 110-Main feed pipe; 111-Branch feed pipe; 201-Reaction tank; 202-Insulated tank. Detailed Implementation

[0026] 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.

[0027] like Figure 1 As shown, a continuous reaction apparatus for the production of dichlorosulfonamide includes a horizontally placed reaction tank 201 and a heat preservation tank 202. The inlet of the reaction tank 201 is connected to a mixed liquid pipe, and the outlet of the reaction tank 201 is connected to the heat preservation tank 202 via a conveying assembly. The reaction tank 201 and the heat preservation tank 202 are sequentially divided into multiple interconnected regions, each region being equipped with a stirrer. Each region of the reaction tank 201 has a chlorosulfonic acid inlet at its top. The outer walls of both the reaction tank 201 and the heat preservation tank 202 are equipped with a heating layer, which is a jacket installed on the outer wall of the tank, and steam is circulated within the jacket. The outlet of the heat preservation tank 202 is connected to a distillation device for the purification process. The tops of both the reaction tank 201 and the heat preservation tank 202 are equipped with an exhaust pipe and a condensation reflux assembly. The mixture in the mixing pipe is a mixture of thionyl chloride and aminosulfonic acid, which reacts in sections with chlorosulfonic acid added dropwise in the reaction tank. As the materials in the reaction tank react, the generated hydrogen chloride and sulfur dioxide are discharged from the exhaust pipe. The thionyl chloride gas can be cooled down by the condensation reflux component and returned to the reaction tank to participate in the reaction again.

[0028] As a preferred structure, such as Figure 1 , 3As shown, the reaction vessel 201 has multiple baffles 5 and multiple baffles 6 spaced along its length. The baffles 5 and baffles 6 are staggered. The upper end of the baffle 6 is connected to the top wall of the reaction vessel 201, and the lower end is separated from the bottom of the reaction vessel 201. The lower end of the baffle 5 is connected to the bottom of the reaction vessel 201, and the upper end is separated from the top wall of the reaction vessel 201. The reaction vessel 201 is divided into several regions by the baffles 5 and baffles 6. Each region is equipped with a thermometer 11 and a stirrer 12, and each region has an exhaust pipe at the top. The internal structure of the heat preservation tank 202 is the same as that of the reaction vessel 201. Both the reaction vessel 201 and the heat preservation tank 202 have discharge pipes 7 at their bottoms. Meanwhile, the chlorosulfonic acid inlet at the top of the reaction vessel 201 is connected to the feed branch pipe 111, which is equipped with a control valve 9 and a flow meter 14. Multiple feed branch pipes 111 are connected in parallel to the main feed pipe 110. The main feed pipe 110 is connected to the bottom outlet of the chlorosulfonic acid storage tank 102 via a magnetic pump 1. The central control console can control the multi-stage control valves to begin dripping chlorosulfonic acid, controlling the dripping rate according to the discharge speed from the reaction vessel; simultaneously, the amount of gas released from the reaction vessel is recorded during the dripping process.

[0029] like Figure 3 As shown, in this embodiment, the reaction vessel is equipped with two baffles and two baffle plates, arranged between the inlet and outlet as follows: baffle, baffle, baffle, baffle, dividing its inner cavity into 5 areas; there are 10 feed branch pipes, and the 10 feed branch pipes correspond one-to-one with the areas in the two reaction vessels.

[0030] like Figure 1 As shown, the mixing liquid pipe is connected to the outlet of the mixing tank 104. The thionyl chloride in the thionyl chloride storage tank 101 is transported to the mixing tank 103 through the magnetic pump 1 and the conveying pipe. The mixing tank 103 is equipped with a stirrer and its top is connected to the compressed air pipe 106. A lifting device 105 is provided above the mixing tank 103. The lifting device 105 is used to lift the aminosulfonic acid packaging bag and add aminosulfonic acid into the mixing tank 103. Meanwhile, an intermediate tank 109 equipped with a stirrer is provided between the mixing tank 103 and the chemical tank 104. The inlet end of the discharge pipe of the mixing tank 103 extends downwards near the bottom of the mixing tank 103, and the outlet end of the discharge pipe is connected to the top of the intermediate tank 109. The inlet end of the discharge pipe of the intermediate tank 109 extends downwards near the bottom of the intermediate tank 109, and the outlet end of the discharge pipe extends into the chemical tank 104 and near the bottom of the chemical tank 104. The discharge pipes between the mixing tank 103 and the intermediate tank 109, and between the intermediate tank 109 and the chemical tank 104, are all inclined downwards along the direction of liquid flow to avoid material retention in the discharge pipes. After the aminosulfonic acid and thionyl chloride are mixed in the mixing tank, they enter the intermediate tank for further stirring, which can achieve thorough mixing of the two raw materials.

[0031] like Figure 2 As shown, the internal structure of the chemical tank 104 is the same as that of the reaction tank 201. Both are divided into several areas by baffles 5 and baffles 6. Each area is equipped with a thermometer 11 and a stirrer 12. The exhaust pipe at the top of each area is connected in parallel with the main pipe. The main pipe is equipped with a control valve and a pressure sensor 10 linked to it. The pressure sensor 10 is used to detect the pressure inside the chemical tank 104.

[0032] In specific embodiments of this utility model, such as Figure 1 As shown, the condensation reflux assembly includes a condenser 2 and a low-temperature heat exchanger 3. Multiple exhaust pipes at the top of the reaction vessel 201 and the insulation tank 202 are connected to multiple condensers 2. The bottom discharge pipes of the multiple condensers 2 are connected to the top of the reaction vessel 201 and the insulation tank 202, respectively. The top outlet of the condenser 2 is connected to the exhaust manifold. The exhaust manifold is connected to the lower inlet of the low-temperature heat exchanger 3. The bottom outlet of the low-temperature heat exchanger 3 is connected to the top of the reaction vessel 201. The top outlet of the low-temperature heat exchanger 3 is connected to the tail gas pipe 8. The top outlets of both the condenser 2 and the low-temperature heat exchanger 3 are equipped with thermometers 11. The lower and upper parts of the outer wall of the condenser 2 are respectively provided with cooling medium inlets and outlets, which can cool the gas passing through it. In this embodiment, circulating water is used as the cooling medium. The condenser 2 and the cryogenic heat exchanger 3 are equipped with control valves 9 and pressure sensors 10 linked to them on their top outlet pipes. The pressure sensors 10 are used to detect the outlet pressure of the condenser 2 and the cryogenic heat exchanger 3. The condenser and the cryogenic condenser cool the thionyl chloride in the exhaust gas, causing it to condense and flow back into the reaction tank, thus improving material utilization. Finally, the discharged hydrogen chloride and sulfur dioxide flow into the tail gas pipe and enter the tail gas treatment system for purification.

[0033] The following is a specific embodiment of the feeding process of the reaction vessel:

[0034] First, turn on the agitator inside the reaction tank, open the steam valve of the reaction tank, and introduce steam into the jacket of the reaction tank to maintain the temperature between 68-72℃; turn on the circulating water of the condenser and start the exhaust gas treatment system.

[0035] Start feeding: Start the compressed air in the intermediate tank to force the material in the chemical tank into the first reaction tank up to the upper edge of the first baffle inside; open the control valve of the feed main pipe, slowly open the No. 1 chlorosulfonic acid valve on the first feed branch pipe, control the flow rate at 40-60 kg / h, and after two hours open the No. 2 chlorosulfonic acid valve on the second feed branch pipe, control the flow rate at 100-120 kg / h, and stabilize the reaction for 2 hours;

[0036] Continue feeding into the first reaction vessel, controlling the feed flow rate at 2.6-2.7 m³ / h. After 2 hours, open valve #3 for chlorosulfonic acid and control the flow rate at 100-120 kg / h. After another 2 hours, open valve #4 for chlorosulfonic acid and control the flow rate at 100-120 kg / h.

[0037] When the material reaches the upper edge of the second baffle, open the No. 5 chlorosulfonic acid valve after 2 hours and control the flow rate at 100-120 kg / h.

[0038] The material then enters the second reactor. After 2 hours, valve #6 (chlorosulfonic acid) is opened, and the flow rate is controlled at 100-120 kg / h. After another 2 hours, valve #7 (chlorosulfonic acid) is opened, and the flow rate is controlled at 100-120 kg / h.

[0039] After the material reaches the upper edge of the first baffle of the second reactor, open valve #8 (chlorosulfonic acid) after 2 hours, controlling the flow rate at 100-120 kg / h; open valve #9 (chlorosulfonic acid) after 2 hours, controlling the flow rate at 100-120 kg / h.

[0040] After the material reaches the upper edge of the second baffle of the second reactor, samples are taken from the last section of the reactor 2 hours later to test the chlorosulfonic acid content. Based on the test results, the No. 10 chlorosulfonic acid valve is opened appropriately to control the flow rate at 40-60 kg / h.

[0041] Then, feed the material into the first insulation tank and open the steam valve on the jacket of the insulation tank to control the temperature at 80-85℃; when the material reaches the second insulation tank, open the steam valve on the jacket of the insulation tank to control the temperature at 85-90℃.

[0042] During the reaction process in the reaction tank and the heat preservation tank, the pressure is controlled at 0.1 MPa. This serves two purposes: first, it increases the reaction temperature and promotes a more complete reaction; second, maintaining positive pressure raises the boiling point of thionyl chloride, reduces the amount of thionyl chloride in the tail gas, and makes it easier to recover.

[0043] In a specific production batch of this utility model, 21 tons of thionyl chloride, 5.06 tons of aminosulfonic acid, and 6.3 tons of chlorosulfonic acid are used for the reaction. The thionyl chloride and aminosulfonic acid are heated to 70-75 degrees Celsius in a chemical tank and kept at that temperature for 6 hours. The mixture is then fed into the reaction tank, and the chlorosulfonic acid is added dropwise at multiple points in sections while stirring to improve the reaction efficiency.

[0044] In summary, this invention boasts advantages such as a reasonable and compact structural design. After thionyl chloride and aminosulfonic acid are mixed in the mixing tank, the mixture is heated in the chemical tank under the action of compressed air. Then, compressed air forces the material in the chemical tank into the reaction tank. Multiple feed branches add chlorosulfonic acid dropwise into the reaction tank in sections, ensuring thorough reaction of the materials in each section. During the reaction, a condenser and a low-temperature heat exchanger are used to cool the volatilized thionyl chloride, allowing it to flow back to the reaction tank to continue participating in the reaction. The material then enters an insulation tank for continuous heat preservation, ensuring complete reaction. This invention enables continuous reaction, improves reaction efficiency through multi-point dropwise addition of chlorosulfonic acid, and simultaneously increases production efficiency, reduces production costs, and meets the requirements of continuous production.

[0045] 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 continuous reaction apparatus for the production of dichlorosulfonylimide, characterized in that: The device includes a horizontally placed reaction vessel and an insulated tank. The inlet of the reaction vessel is connected to a mixed liquid pipe, and the outlet of the reaction vessel is connected to the insulated tank via a conveying assembly. The reaction vessel and the insulated tank are sequentially divided into multiple interconnected areas, each of which is equipped with a stirrer. Each area of ​​the reaction vessel has a chlorosulfonic acid inlet at its top. The outer walls of both the reaction vessel and the insulated tank are equipped with heating layers. The outlet of the insulated tank is connected to a distillation device in the purification process. The top of both the reaction vessel and the insulated tank is equipped with an exhaust pipe and a condensation reflux assembly.

2. The continuous reaction apparatus for producing dichlorosulfonylimide according to claim 1, characterized in that: The reaction vessel is equipped with multiple baffles and baffles spaced along its length. The baffles and baffles are staggered. The upper end of the baffle is connected to the top wall of the reaction vessel, and the lower end has a gap with the bottom of the reaction vessel. The lower end of the baffle is connected to the bottom of the reaction vessel, and the upper end has a gap with the top wall of the reaction vessel. The reaction vessel is divided into several regions by the baffles and baffles. Each region is equipped with a thermometer and a stirrer, and each region has an exhaust pipe at the top. The internal structure of the insulation tank is the same as that of the reaction vessel. Both the reaction vessel and the insulation tank have discharge pipes at their bottoms.

3. The continuous reaction apparatus for producing dichlorosulfonylimide according to claim 2, characterized in that: The chlorosulfonic acid inlet at the top of the reaction vessel is connected to a feed branch pipe, which is equipped with a control valve and a flow meter. Multiple feed branch pipes are connected in parallel with the main feed pipe. The main feed pipe is connected to the bottom outlet of the chlorosulfonic acid storage tank via a magnetic pump.

4. A continuous reaction apparatus for the production of dichlorosulfonylimide according to claim 2, characterized in that: The mixing liquid pipe is connected to the outlet of the mixing tank. The thionyl chloride in the thionyl chloride storage tank is transported to the mixing tank through a magnetic pump and a conveying pipe. The mixing tank is equipped with a stirrer and its top is connected to a compressed air pipe. A lifting device is provided above the mixing tank. The lifting device is used to lift the aminosulfonic acid packaging bag and add aminosulfonic acid to the mixing tank.

5. A continuous reaction apparatus for the production of dichlorosulfonylimide according to claim 4, characterized in that: An intermediate tank equipped with a stirrer is provided between the mixing tank and the chemical tank. The inlet end of the discharge pipe of the mixing tank extends downward to near the bottom of the mixing tank, and the outlet end of the discharge pipe is connected to the top of the intermediate tank. The inlet end of the discharge pipe of the intermediate tank extends downward to near the bottom of the intermediate tank, and the outlet end of the discharge pipe extends into the chemical tank and near the bottom of the chemical tank. The discharge pipes between the mixing tank and the intermediate tank, and between the intermediate tank and the chemical tank, are all inclined downward along the direction of liquid flow.

6. A continuous reaction apparatus for the production of dichlorosulfonylimide according to claim 5, characterized in that: The internal structure of the chemical tank is the same as that of the reaction vessel, both of which are divided into several areas by baffles and deflectors. Each area is equipped with a thermometer and a stirrer. The exhaust pipe at the top of each area is connected in parallel with the main pipe. The main pipe is equipped with a control valve and a pressure sensor linked to it. The pressure sensor is used to detect the pressure inside the chemical tank.

7. A continuous reaction apparatus for the production of dichlorosulfonylimide according to any one of claims 1-6, characterized in that: The condensation reflux assembly includes a condenser and a low-temperature heat exchanger. Multiple exhaust pipes at the top of the reaction vessel and the insulation tank are connected to multiple condensers. The bottom discharge pipes of the multiple condensers are connected to the top of the reaction vessel and the insulation tank. The top outlet of the condenser is connected to the exhaust manifold. The exhaust manifold is connected to the lower inlet of the low-temperature heat exchanger. The bottom outlet of the low-temperature heat exchanger is connected to the top of the reaction vessel. The top outlet of the low-temperature heat exchanger is connected to the tail gas pipe. The top outlets of both the condenser and the low-temperature heat exchanger are equipped with thermometers.

8. A continuous reaction apparatus for the production of dichlorosulfonylimide according to claim 7, characterized in that: The top outlet pipes of the condenser and the low-temperature heat exchanger are equipped with control valves and pressure sensors linked to them. The pressure sensors are used to detect the outlet pressure of the condenser and the low-temperature heat exchanger.

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