A continuous production system for low moisture methylsulfonyl fluoride

Abstract

The utility model relates to methylsulfonyl fluoride preparation technical field discloses a kind of continuous production system of low moisture methylsulfonyl fluoride, including aqueous phase reaction kettle, aqueous phase reaction liquid distillation device, normal temperature phase separation device, low temperature water separation device, continuous rectification device and finished product tank, the feed inlet of aqueous phase reaction kettle's discharge outlet is connected with aqueous phase reaction liquid distillation device, the feed inlet of aqueous phase reaction liquid distillation device's discharge outlet is connected with normal temperature phase separation device, the feed inlet of normal temperature phase separation device's oil phase outlet is connected with low temperature water separation device, the feed inlet of low temperature water separation device's oil phase outlet is connected with continuous rectification device, the heavy component discharge outlet of continuous rectification device is connected with finished product tank.This continuous production system, by the multielement cooperation of staged water removal process, moisture is controlled at low level, with high economy and high environmental protection.

Description

Technical Field

[0001] This utility model relates to the field of methanesulfonyl fluoride preparation technology, and in particular to a continuous production system for low-moisture methanesulfonyl fluoride. Background Technology

[0002] Methylsulfonyl fluoride, a key raw material for the preparation of lithium bis(trifluoromethanesulfonyl)imide (LiTFSI), has a significant impact on the purity and performance of downstream products due to its moisture content. Currently, the preparation methods for low-moisture methylsulfonyl fluoride mainly fall into two categories: First, molecular sieve adsorption is used to remove water from crude methylsulfonyl fluoride. While this method can reduce moisture to some extent, methylsulfonyl fluoride itself is toxic, and its active ingredient will be adsorbed along with the water by the molecular sieve. This leads to the generation of adsorbed waste molecular sieves carrying toxic methylsulfonyl fluoride residues after adsorption saturation, resulting in high environmental disposal costs. Second, direct distillation dehydration of crude methylsulfonyl fluoride is performed. However, due to the difficulty in separating methylsulfonyl fluoride from water, this method requires the extraction of more than 30% of the fore-distillate to achieve the low moisture requirement, resulting in high energy consumption and poor economic efficiency. Utility Model Content

[0003] To address the aforementioned technical problems, this invention provides a continuous production system for low-moisture methanesulfonyl fluoride. Through a multi-unit collaborative staged dehydration process, the moisture content is controlled at a low level, achieving both high economic efficiency and high environmental friendliness.

[0004] The specific technical solution of this utility model is as follows: a continuous production system for low-moisture methanesulfonyl fluoride, comprising an aqueous phase reaction vessel, an aqueous phase reaction liquid distillation device, an ambient temperature phase separation device, a low temperature water separation device, a continuous distillation device, and a finished product tank. The outlet of the aqueous phase reaction vessel is connected to the inlet of the aqueous phase reaction liquid distillation device, the outlet of the aqueous phase reaction liquid distillation device is connected to the inlet of the ambient temperature phase separation device, the oil phase outlet of the ambient temperature phase separation device is connected to the inlet of the low temperature water separation device, the oil phase outlet of the low temperature water separation device is connected to the inlet of the continuous distillation device, and the heavy component outlet of the continuous distillation device is connected to the finished product tank.

[0005] In the aforementioned continuous production system, the crude methanesulfonyl fluoride synthesized in the aqueous phase reactor enters the aqueous phase reaction liquid distillation unit, where methanesulfonyl fluoride and water are distilled off in the form of steam. Subsequently, the steam is condensed and placed in a room temperature phase separation unit to separate into layers. The upper layer is an aqueous phase, and the lower layer is an oil phase mainly composed of methanesulfonyl fluoride. This oil phase is then passed into a low-temperature water separation unit. The low-temperature environment reduces the solubility of water in methanesulfonyl fluoride, causing some dissolved water to precipitate and form an aqueous phase layer, further reducing the water content of the oil phase. Finally, the low-temperature dehydrated oil phase is passed into a continuous distillation unit to remove residual trace amounts of water, yielding low-moisture methanesulfonyl fluoride. This invention's continuous production system utilizes a multi-unit collaborative staged dehydration process to stably control the moisture content of methanesulfonyl fluoride at a low level. Compared to direct distillation, thanks to the pre-treatment of staged dehydration, the moisture content of the material entering the distillation stage is significantly reduced. Only 10-15% of the fore-distillate needs to be collected from the top of the column to meet the low moisture requirement, significantly reducing energy consumption and loss of effective components. Compared to molecular sieve adsorption dehydration, this system does not rely on molecular sieves but achieves deep dehydration through physical separation and material recycling, avoiding the generation of toxic waste molecular sieves at the source. This reduces environmental disposal costs and the risk of secondary pollution, thus balancing the economic efficiency and environmental friendliness of industrial production.

[0006] Optionally, the aqueous reaction liquid distillation device includes an aqueous reaction liquid distillation vessel connected to the outlet of the aqueous reaction vessel and an effluent collection tank connected to the outlet of the distillate from the aqueous reaction liquid distillation vessel. The outlet of the effluent collection tank is connected to the inlet of the ambient temperature phase separation device.

[0007] In the above technical solution, since the distillate from the distillation vessel is volatile, if it is directly connected to the ambient temperature phase separation device, the flow shock will disrupt the stratification equilibrium already formed in the phase separation tank, resulting in the repeated appearance of the emulsion layer. However, the distillate collection tank can temporarily store the distillate, providing a stable flow feed to the ambient temperature phase separation device and maintaining the feed amount within a reasonable range each time. This ensures that the phase separation process can efficiently separate the low-moisture crude methanesulfonyl fluoride, laying the foundation for the low-energy operation of subsequent low-temperature water separation and continuous distillation.

[0008] Optionally, the ambient temperature phase separation device includes an ambient temperature phase separation tank and a control unit for controlling the discharge of material from the ambient temperature phase separation tank. The ambient temperature phase separation tank is equipped with a level gauge for monitoring the material height inside the tank and a conductivity meter for monitoring the conductivity of the material at the bottom of the tank. The level gauge and the conductivity meter are electrically connected to the control unit.

[0009] In the above technical solution, the level gauge can track the material height in the tank in real time to avoid overflow due to excessive material or system instability due to insufficient material; the conductivity meter uses the difference in conductivity between the aqueous phase and the oil phase to accurately identify whether the detected material is a qualified oil phase; the control unit receives signals from both and controls the feeding and discharging actions in a coordinated manner.

[0010] Optionally, the oil phase outlet of the ambient temperature phase separator is connected to the inlet of the aqueous phase reaction liquid distillation device and the inlet of the low temperature water separation device via pipelines, forming a switchable flow path. The control unit switches the flow path according to the detection results of the level gauge and conductivity meter, and guides the oil phase separated by the ambient temperature phase separator to the aqueous phase reaction liquid distillation device or the low temperature water separation device.

[0011] In the above technical solution, methylsulfonyl fluoride is the core raw material, and its production cost is relatively high. The methylsulfonyl fluoride with insufficient moisture content after phase separation is reintroduced into the aqueous reaction liquid distillation device and the room temperature phase separation device for secondary treatment. This can not only realize the recovery and utilization of effective components to reduce raw material consumption costs, but also reduce the amount of waste generated, thereby reducing the pressure and cost of subsequent waste treatment, and taking into account both economic efficiency and environmental protection.

[0012] Optionally, the low-temperature water separation device includes a low-temperature water separation tank and a control unit for controlling the discharge of the low-temperature water separation tank. The low-temperature water separation tank is equipped with a level gauge for monitoring the material height inside the tank, and the level gauge is electrically connected to the control unit.

[0013] In the above technical solution, when the liquid level is below the preset lower limit, the control unit triggers the feed valve to open; when the liquid level reaches the preset upper limit, the control unit immediately closes the feed valve, suspending feeding. The control unit controls the opening and closing of the feed valve by collecting real-time material height data in the tank through the level gauge, ensuring the continuous and efficient operation of the entire system.

[0014] Optionally, the low-temperature water separation tank is provided with an overflow return port at the top. The overflow return port is connected to the feed port of the ambient temperature phase separation device through a pipeline to return excess material to the ambient temperature phase separation device.

[0015] In the above technical solution, an overflow return port is provided, which can automatically discharge excess material when the ultra-low temperature water separation tank reaches its capacity, avoiding overflow and causing abnormal pressure, thus providing safety overflow protection. At the same time, it can guide incompletely treated materials containing methanesulfonyl fluoride back to the room temperature phase separation device for reprocessing, improving the recovery rate of effective components and reducing losses. In addition, in a continuous production system, the feed / discharge rates of each device may experience momentary imbalances due to fluctuations in operating conditions. The overflow return port can act as a "buffer channel," adjusting the liquid level of the low temperature water separation tank through material return, maintaining the stability of material flow within the system, and avoiding disruption to the overall production rhythm due to local pressure buildup or material interruption.

[0016] Optionally, the continuous distillation apparatus includes a falling film evaporator, a distillation column, and a bottom receiving tank. The feed inlet of the falling film evaporator is connected to the oil phase outlet of the low-temperature water separation device, the discharge outlet of the falling film evaporator is connected to the feed inlet of the distillation column, the discharge outlet of the heavy components of the distillation column is connected to the feed inlet of the bottom receiving tank, and the discharge outlet of the bottom receiving tank is connected to the finished product tank.

[0017] Optionally, the continuous distillation apparatus further includes a control unit for controlling the discharge from the bottom receiving tank. The discharge port of the bottom receiving tank is connected to the finished product tank and the ambient temperature phase separation device via pipelines. The bottom receiving tank is equipped with a level gauge for monitoring the material level and a moisture meter for monitoring the material moisture content. The level gauge and moisture meter are electrically connected to the control unit. Based on the detection results of the level gauge and moisture meter, the control unit switches the diversion path to guide the material in the bottom receiving tank to the finished product tank or the ambient temperature phase separation device.

[0018] In the above technical solution, the moisture meter on the receiving tank at the bottom of the tower can detect the moisture content of the material in real time, the level gauge simultaneously monitors the material inventory in the tank, the control unit controls the feeding according to the level gauge, and determines whether the product in the tank is qualified according to the moisture meter, ensuring that qualified products enter the finished product tank, and unqualified products are returned to the previous processing flow for dehydration and purification, avoiding material waste and forming a closed loop of "distillation-detection-recycle", improving the utilization rate of raw materials. In addition, the level gauge can also prevent the material in the tank from accumulating or interrupting the supply. When the liquid level exceeds the upper limit, the feeding is suspended or priority diversion is given. When the liquid level is below the lower limit, it prompts the previous stable supply, ensuring that it matches the rhythm of finished product tank storage and previous distillation process, and further ensuring the continuous and stable operation of the entire system.

[0019] Optionally, the continuous distillation apparatus further includes a top receiving tank, the inlet of which is connected to the light component outlet of the distillation column, and the outlet of which is connected to the inlet of the ambient temperature phase separation device.

[0020] In the above technical solution, when the distillation column is running, a small amount of methanesulfonyl fluoride will be discharged from the light component outlet at the top of the column along with the light component. After entering the receiving tank at the top of the column, the light component condenses into a liquid mixture. This liquid mixture is then returned to the preceding processing flow for dehydration and purification, and finally converted into a qualified finished product. This not only avoids the generation of toxic waste from the source and saves additional environmental disposal costs, but also reduces the raw material loss of methanesulfonyl fluoride, thereby improving the economic efficiency and environmental friendliness of production.

[0021] Optionally, the continuous distillation apparatus further includes a control unit for controlling the discharge from the top receiving tank. The top receiving tank is equipped with a level gauge for monitoring the material level inside the tank. A discharge pump is installed between the discharge port of the top receiving tank and the inlet of the ambient temperature phase separation device. The level gauge and the discharge pump are electrically connected to the control unit. The control unit controls the start and stop of the discharge pump based on the level gauge detection results.

[0022] In the above technical solution, the level gauge on the top receiving tank collects the height data of the condensed liquid mixture in the tank in real time. The control unit automatically adjusts the start and stop of the discharge pump based on the preset level threshold, accurately matching the discharge rhythm of the top receiving tank with the feeding requirements of the ambient temperature phase separation device, so as to realize the automated operation of the system.

[0023] Compared with the prior art, the present invention has at least the following advantages: (1) This utility model achieves efficient and deep dehydration of methanesulfonyl fluoride through a multi-unit collaborative staged dehydration process. It can not only effectively control the moisture content at a low level, but also significantly reduce energy consumption. At the same time, it constructs a full-process material recycling mechanism, which reduces waste generation through the recycling of unqualified materials and does not generate toxic waste, thus reducing environmental disposal pressure. It takes into account both the economic and environmental benefits of industrial production and is easy to industrialize. (2) By adding a control unit that links the entire system, this utility model realizes the automated operation of feeding, discharging, and discharging qualification judgment, which greatly improves production efficiency and stability and meets the needs of industrial continuous production. Attached Figure Description

[0024] Figure 1 This is a system flowchart of this utility model.

[0025] The attached diagram is labeled as follows: 1. Aqueous phase reaction vessel; 2. Aqueous phase reaction liquid distillation vessel; 3. Distillate collection tank; 4. Ambient temperature phase separation tank; 5. Low temperature water separation tank; 6. Falling film evaporator; 7. Bottom receiving tank; 8. Distillation column; 9. Top receiving tank; 10. Finished product tank. Detailed Implementation

[0026] The present invention will be further described below with reference to embodiments. Unless otherwise specified, all devices, connection structures, and methods involved in this invention are known in the art.

[0027] Example 1 Reference Figure 1 As shown, this utility model provides a continuous production system for low-moisture methanesulfonyl fluoride, including an aqueous phase reactor 1, an aqueous phase reaction liquid distillation device, an ambient temperature phase separation device, a low temperature water separation device, a continuous distillation device, and a finished product tank 10. The outlet of the aqueous phase reactor 1 is connected to the inlet of the aqueous phase reaction liquid distillation device, the outlet of the aqueous phase reaction liquid distillation device is connected to the inlet of the ambient temperature phase separation device, the oil phase outlet of the ambient temperature phase separation device is connected to the inlet of the low temperature water separation device, the oil phase outlet of the low temperature water separation device is connected to the inlet of the continuous distillation device, and the heavy component outlet of the continuous distillation device is connected to the finished product tank 10.

[0028] In the aforementioned continuous production system, the crude methanesulfonyl fluoride synthesized in the aqueous phase reactor enters the aqueous phase reaction liquid distillation unit, where methanesulfonyl fluoride and water are distilled off in the form of steam. Subsequently, the steam is condensed and placed in a room temperature phase separation unit to separate into layers. The upper layer is an aqueous phase, and the lower layer is an oil phase mainly composed of methanesulfonyl fluoride. This oil phase is then passed into a low-temperature water separation unit. The low-temperature environment reduces the solubility of water in methanesulfonyl fluoride, causing some dissolved water to precipitate and form an aqueous phase layer, further reducing the water content of the oil phase. Finally, the low-temperature dehydrated oil phase is passed into a continuous distillation unit to remove residual trace amounts of water, yielding low-moisture methanesulfonyl fluoride. This invention's continuous production system utilizes a multi-unit collaborative staged dehydration process to stably control the moisture content of methanesulfonyl fluoride at a low level. Compared to direct distillation, thanks to the pre-treatment of staged dehydration, the moisture content of the material entering the distillation stage is significantly reduced. Only 10-15% of the fore-distillate needs to be collected from the top of the column to meet the low moisture requirement, significantly reducing energy consumption and loss of effective components. Compared to molecular sieve adsorption dehydration, this system does not rely on molecular sieves but achieves deep dehydration through physical separation and material recycling, avoiding the generation of toxic waste molecular sieves at the source. This reduces environmental disposal costs and the risk of secondary pollution, thus balancing the economic efficiency and environmental friendliness of industrial production.

[0029] In a preferred embodiment of this utility model, such as Figure 1 As shown, the aqueous reaction liquid distillation device includes an aqueous reaction liquid distillation vessel 2 connected to the outlet of the aqueous reaction vessel 1 and an effluent collection tank 3 connected to the outlet of the distillate from the aqueous reaction liquid distillation vessel 2. The outlet of the effluent collection tank 3 is connected to the inlet of the ambient temperature phase separation device.

[0030] The ambient temperature phase separation device includes an ambient temperature phase separation tank 4 and a control unit for controlling the discharge of the ambient temperature phase separation tank 4. The ambient temperature phase separation tank 4 is equipped with a level gauge for monitoring the material height inside the tank and a conductivity meter for monitoring the conductivity of the material at the bottom of the tank. The level gauge and conductivity meter are electrically connected to the control unit.

[0031] Furthermore, the oil phase outlet of the ambient temperature phase separator 4 is connected via pipelines to the inlet of the aqueous phase reaction liquid distillation device and the inlet of the low-temperature water separation device, forming a switchable flow path. The control unit switches the flow path based on the detection results of the level gauge and conductivity meter, directing the oil phase separated from the ambient temperature phase separator 4 to either the aqueous phase reaction liquid distillation device or the low-temperature water separation device. Since the aqueous phase reaction liquid distillation device is installed higher than the ambient temperature phase separator 4, a discharge pump is installed on this return pipeline to drive the oil phase material separated from the ambient temperature phase separator 4 back to the aqueous phase reaction liquid distillation device smoothly.

[0032] The low-temperature water separation device includes a low-temperature water separation tank 5 and a control unit for controlling the discharge of the low-temperature water separation tank 5. The low-temperature water separation tank 5 is equipped with a level gauge for monitoring the material height inside the tank, and the level gauge is electrically connected to the control unit.

[0033] Furthermore, the low-temperature water separation tank 5 is equipped with an overflow return port at its upper part. The overflow return port is connected to the feed port of the ambient temperature phase separation device through a pipeline to return excess material to the ambient temperature phase separation device. Since the ambient temperature phase separation device is installed higher than the low-temperature water separation tank 5, a discharge pump is installed on the return pipeline to drive the excess material in the low-temperature water separation tank 5 back to the ambient temperature phase separation device.

[0034] The continuous distillation unit includes a falling film evaporator 6, a distillation column 8, a bottom receiving tank 7, a top receiving tank 9, and a control unit for controlling the discharge of the top receiving tank 9 and the discharge of the bottom receiving tank 7. The inlet of the falling film evaporator 6 is connected to the oil phase outlet of the low-temperature water separation unit, the outlet of the falling film evaporator 6 is connected to the inlet of the distillation column 8, the outlet of the heavy components of the distillation column 8 is connected to the inlet of the bottom receiving tank 7, the outlet of the bottom receiving tank 7 is connected to the finished product tank 10, the inlet of the top receiving tank 9 is connected to the outlet of the light components of the distillation column 8, and the outlet of the top receiving tank 9 is connected to the inlet of the ambient temperature phase separation unit.

[0035] Furthermore, the continuous distillation unit also includes a control unit for controlling the discharge of the bottom receiving tank 7. The discharge port of the bottom receiving tank 7 is connected to the finished product tank 10 and the ambient temperature phase separation device through pipelines. The bottom receiving tank 7 is equipped with a level gauge for monitoring the material height in the tank and a moisture meter for monitoring the moisture content of the material. The level gauge and the moisture meter are electrically connected to the control unit. Based on the detection results of the level gauge and the moisture meter, the control unit switches the diversion path to guide the material in the bottom receiving tank 7 to the finished product tank 10 or the ambient temperature phase separation device.

[0036] Furthermore, the continuous distillation unit also includes a control unit for controlling the discharge of the top receiving tank 9. The top receiving tank 9 is equipped with a level gauge for monitoring the material level inside the tank. A discharge pump is installed between the discharge port of the top receiving tank 9 and the inlet of the ambient temperature phase separation device. The level gauge and the discharge pump are electrically connected to the control unit. The control unit controls the start and stop of the discharge pump based on the level gauge detection results.

[0037] Figure 1 In the diagram, instrument "L" is a level gauge, which provides real-time feedback on the material level in the tank to prevent the discharge pump from running dry or overflowing due to insufficient material. Instrument "A" is a pneumatic control instrument, which controls the valve opening and closing according to the control unit's instructions. The conductivity meter and moisture meter are not shown in the diagram but are described in words. The conductivity meter accurately identifies the purity of the oil phase by detecting the conductivity of the material at the bottom of the ambient temperature phase separation tank 4 (the oil phase mainly composed of methanesulfonyl fluoride) to prevent water phase entrainment. The moisture meter detects the moisture content of the material in the receiving tank 7 at the bottom of the tower to determine whether the product in the tank is qualified.

[0038] In this embodiment, the control units for the ambient temperature phase separation device, the low temperature water separation device, and the continuous distillation device are the same control unit. This same control unit can synchronously receive and process monitoring data from the three devices, realizing centralized data acquisition, unified analysis, and coordinated control throughout the entire process, achieving automated control of the entire system. The specific control logic is as follows: After receiving the level gauge signals from each device, the control unit automatically determines whether the feeding conditions are met based on preset thresholds, and then precisely controls the feed valve action of the corresponding device; after receiving the conductivity meter or moisture meter signal, it automatically verifies whether the discharge conditions are met, and then drives the switching of the branch valves through pneumatic control instruments to achieve directional material conveying. By coordinating the feeding and discharging rhythms of each stage through unified scheduling by the control unit, production efficiency and stability are greatly improved, adapting to the needs of continuous industrial production.

[0039] The ambient temperature phase separation tank 4 has three independent feed ports at the top: the first feed port is connected to the outlet of the distillate collection tank 3 and is used to receive the material after the previous distillation treatment; the second feed port is connected to the overflow return port of the low temperature water separation tank 5, which can return the material overflowing from the low temperature water separation tank 5 due to excessive liquid level to the ambient temperature phase separation tank 4, avoid material waste and ensure the stable operation of the low temperature water separation tank 5; the third feed port is connected to the circulating material pipeline of the continuous distillation unit. It should be noted that the medium in this circulating material pipeline is a mixture, specifically including the light components collected and condensed by the top receiving tank 9 and the material detected as unqualified by the bottom receiving tank 7. Through this feed port, the two types of circulating materials are introduced into the ambient temperature phase separation tank 4 together to participate in the phase separation treatment again, forming a closed loop of material recovery throughout the entire process.

[0040] The continuous production system for low-moisture methanesulfonyl fluoride of this utility model is implemented according to the following steps: Step (1): Add the crude methanesulfonyl fluoride produced by aqueous phase reaction vessel 1 to aqueous phase reaction liquid distillation vessel 2, control the vessel temperature at 110℃ for atmospheric pressure distillation, and collect the distillate in distillate collection tank 3. Step (2): Control the addition of the distillate from step (1) to the ambient temperature phase separation tank 4, allowing the solution to separate at ambient temperature. After phase separation, crude methanesulfonyl fluoride is obtained and enters the next process. Step (3): Add the methanesulfonyl fluoride from step (2) into the low-temperature water separation tank 5, control the temperature of the low-temperature water separation tank 5 to 0-10℃, and let the solution separate into water at low temperature. The upper aqueous phase layer is recirculated into the room temperature phase separation tank 4 through the overflow return port, and the lower methanesulfonyl fluoride layer enters the next process. Step (4): The methyl sulfonyl fluoride from step (3) is fed into the falling film evaporator 6 and then purified by the distillation column 8. The top fraction is stored in the top receiving tank 9 and circulated into the ambient temperature phase separation tank 4 by a pump. The bottom fraction is stored in the bottom receiving tank 7. After passing the moisture test by the moisture analyzer, it enters the finished product tank 10. If it fails the test, it is circulated into the ambient temperature phase separation tank 4 by a pump.

[0041] The preferred low-temperature water separation tank 5 has a temperature of 0-5℃.

[0042] Example 2 The continuous production system for low-moisture methanesulfonyl fluoride of Example 1 was validated. The validation process was as follows: Step (1): First, the crude methanesulfonyl fluoride that has completed the reaction in the aqueous phase reactor 1 is transported to the aqueous phase reaction liquid distillation vessel 2 through the system pipeline. The temperature of the distillation vessel is controlled to be stable at 110℃. The distillate produced by distillation is collected in the distillate collection tank 3 after condensation. Step (2): After the material in the distillate collection tank 3 reaches the set liquid level, it is introduced into the ambient temperature phase separation tank 4, the feed valve is closed and the phase separation is allowed to stand for 30 minutes. After the conductivity of the lower oil phase reaches the standard, the oil phase is transported to the low temperature water separation tank 5. Step (3): The temperature inside the low-temperature water separation tank 5 is stably controlled at 10℃; under low-temperature conditions, the residual water and methanesulfonyl fluoride are separated into two layers. The water phase exceeding the height of the overflow return port is returned to the ambient temperature phase separation tank 4 for recycling and treatment, while the lower low-moisture oil phase is sent to the falling film evaporator 6 for treatment. Step (4): After the falling film evaporator 6 completes the atmospheric pressure evaporation of low moisture methanesulfonyl fluoride, the material is transported to the continuous distillation column 8; the distillation column 8 is controlled to operate at atmospheric pressure, the number of trays is set to 10, and the continuous distillation mode is adopted. At the same time, the proportion of light components collected from the top of the column is adjusted to about 10%; the qualified methanesulfonyl fluoride collected from the bottom of the distillation column 8 is stored in the finished product tank 10. The product in the finished product tank 10 is tested for moisture, and the result is 955 ppm.

[0043] Example 3 The continuous production system for low-moisture methanesulfonyl fluoride of Example 1 was validated. The validation process was as follows: Step (1): First, the crude methanesulfonyl fluoride that has completed the reaction in the aqueous phase reactor 1 is transported to the aqueous phase reaction liquid distillation vessel 2 through the system pipeline. The temperature of the distillation vessel is controlled to be stable at 110℃. The distillate produced by distillation is collected in the distillate collection tank 3 after condensation. Step (2): After the material in the distillate collection tank 3 reaches the set liquid level, it is introduced into the ambient temperature phase separation tank 4, the feed valve is closed and the phase separation is allowed to stand for 30 minutes. After the conductivity of the lower oil phase reaches the standard, the oil phase is transported to the low temperature water separation tank 5. Step (3): The temperature inside the low-temperature water separation tank 5 is stably controlled at 5℃; under low-temperature conditions, the residual water and methylsulfonyl fluoride are separated into two layers. The water phase exceeding the height of the overflow return port is returned to the ambient temperature phase separation tank 4 for recycling and treatment, while the lower low-moisture oil phase is sent to the falling film evaporator 6 for treatment. Step (4): After the falling film evaporator 6 completes the atmospheric pressure evaporation of low moisture methanesulfonyl fluoride, the material is transported to the continuous distillation column 8; the distillation column 8 is controlled to operate at atmospheric pressure, the number of trays is set to 10, and the continuous distillation mode is adopted. At the same time, the proportion of light components collected from the top of the column is adjusted to about 10%; the qualified methanesulfonyl fluoride collected from the bottom of the distillation column 8 is stored in the finished product tank 10, and the product in the finished product tank 10 is tested for moisture, and the result is 685ppm.

[0044] Example 4 The continuous production system for low-moisture methanesulfonyl fluoride of Example 1 was validated. The validation process was as follows: Step (1): First, the crude methanesulfonyl fluoride that has completed the reaction in the aqueous phase reactor 1 is transported to the aqueous phase reaction liquid distillation vessel 2 through the system pipeline. The temperature of the distillation vessel is controlled to be stable at 110℃. The distillate produced by distillation is collected in the distillate collection tank 3 after condensation. Step (2): After the material in the distillate collection tank 3 reaches the set liquid level, it is introduced into the ambient temperature phase separation tank 4, the feed valve is closed and the phase separation is allowed to stand for 30 minutes. After the conductivity of the lower oil phase reaches the standard, the oil phase is transported to the low temperature water separation tank 5. Step (3): The temperature inside the low-temperature water separation tank 5 is stably controlled at 0℃; under low-temperature conditions, the residual water and methylsulfonyl fluoride are separated into two layers. The water phase exceeding the height of the overflow return port is returned to the ambient temperature phase separation tank 4 for recycling and treatment, while the lower low-moisture oil phase is sent to the falling film evaporator 6 for treatment. Step (4): After the falling film evaporator 6 completes the atmospheric pressure evaporation of low moisture methanesulfonyl fluoride, the material is transported to the continuous distillation column 8; the distillation column 8 is controlled to operate at atmospheric pressure, the number of trays is set to 10, and the continuous distillation mode is adopted. At the same time, the proportion of light components collected from the top of the column is adjusted to about 10%; the qualified methanesulfonyl fluoride collected from the bottom of the distillation column 8 is stored in the finished product tank 10. The product in the finished product tank 10 is tested for moisture, and the result is 502 ppm.

[0045] Example 5 The continuous production system for low-moisture methanesulfonyl fluoride of Example 1 was validated. The validation process was as follows: Step (1): First, the crude methanesulfonyl fluoride that has completed the reaction in the aqueous phase reactor 1 is transported to the aqueous phase reaction liquid distillation vessel 2 through the system pipeline. The temperature of the distillation vessel is controlled to be stable at 140℃. The distillate produced by distillation is collected in the distillate collection tank 3 after condensation. Step (2): After the material in the distillate collection tank 3 reaches the set liquid level, it is introduced into the ambient temperature phase separation tank 4, the feed valve is closed and the phase separation is allowed to stand for 30 minutes. After the conductivity of the lower oil phase reaches the standard, the oil phase is transported to the low temperature water separation tank 5. Step (3): The temperature inside the low-temperature water separation tank 5 is stably controlled at 5℃; under low-temperature conditions, the residual water and methylsulfonyl fluoride are separated into two layers. The water phase exceeding the height of the overflow return port is returned to the ambient temperature phase separation tank 4 for recycling and treatment, while the lower low-moisture oil phase is sent to the falling film evaporator 6 for treatment. Step (4): After the falling film evaporator 6 completes the atmospheric pressure evaporation of low moisture methanesulfonyl fluoride, the material is transported to the continuous distillation column 8; the distillation column 8 is controlled to operate at atmospheric pressure, the number of trays is set to 10, and the continuous distillation mode is adopted. At the same time, the proportion of light components collected from the top of the column is adjusted to about 10%; the qualified methanesulfonyl fluoride collected from the bottom of the distillation column 8 is stored in the finished product tank 10. The product in the finished product tank 10 is tested for moisture, and the result is 421 ppm.

[0046] The verification results of Examples 2 to 5 prove that the continuous production system for low-moisture methanesulfonyl fluoride of this invention can stably produce low-moisture methanesulfonyl fluoride products, and the resulting methanesulfonyl fluoride can be controlled with a moisture content of ≤0.1%, which has reached the industry standard level.

[0047] The above are merely preferred embodiments of the present utility model and are not intended to limit the present utility model in any way. Any simple modifications, alterations, or equivalent structural transformations made to the above embodiments based on the technical essence of the present utility model shall still fall within the protection scope of the present utility model.

Claims

1. A continuous production system for low-moisture methanesulfonyl fluoride, characterized in that, It includes an aqueous phase reactor (1), an aqueous phase reaction liquid distillation device, an ambient temperature phase separation device, a low temperature water separation device, a continuous distillation device, and a finished product tank (10). The outlet of the aqueous phase reactor (1) is connected to the inlet of the aqueous phase reaction liquid distillation device, the outlet of the aqueous phase reaction liquid distillation device is connected to the inlet of the ambient temperature phase separation device, the oil phase outlet of the ambient temperature phase separation device is connected to the inlet of the low temperature water separation device, the oil phase outlet of the low temperature water separation device is connected to the inlet of the continuous distillation device, and the heavy component outlet of the continuous distillation device is connected to the finished product tank (10).

2. The continuous production system for low-moisture methanesulfonyl fluoride according to claim 1, characterized in that, The aqueous reaction liquid distillation device includes an aqueous reaction liquid distillation vessel (2) connected to the outlet of the aqueous reaction vessel (1) and a distillate collection tank (3) connected to the outlet of the distillate from the aqueous reaction liquid distillation vessel (2). The outlet of the distillate collection tank (3) is connected to the inlet of the ambient temperature phase separation device.

3. The continuous production system for low-moisture methanesulfonyl fluoride according to claim 1, characterized in that, The ambient temperature phase separation device includes an ambient temperature phase separation tank (4) and a control unit for controlling the discharge of the ambient temperature phase separation tank (4). The ambient temperature phase separation tank (4) is equipped with a level gauge for monitoring the height of the material in the tank and a conductivity meter for monitoring the conductivity of the material in the tank. The level gauge and the conductivity meter are electrically connected to the control unit.

4. The continuous production system for low-moisture methanesulfonyl fluoride according to claim 3, characterized in that, The oil phase outlet of the ambient temperature phase separation tank (4) is connected to the inlet of the aqueous phase reaction liquid distillation device and the inlet of the low temperature water separation device through pipelines, forming a switchable flow path. The control unit switches the flow path according to the detection results of the level gauge and conductivity meter, and guides the oil phase separated by the ambient temperature phase separation tank (4) to the aqueous phase reaction liquid distillation device or the low temperature water separation device.

5. The continuous production system for low-moisture methanesulfonyl fluoride according to claim 1, characterized in that, The low-temperature water separation device includes a low-temperature water separation tank (5) and a control unit for controlling the discharge of the low-temperature water separation tank (5). The low-temperature water separation tank (5) is equipped with a level gauge for monitoring the height of the material inside the tank, and the level gauge is electrically connected to the control unit.

6. The continuous production system for low-moisture methanesulfonyl fluoride according to claim 5, characterized in that, The low-temperature water separation tank (5) is provided with an overflow return port at the top. The overflow return port is connected to the feed port of the ambient temperature phase separation device through a pipeline so as to return the excess material to the ambient temperature phase separation device.

7. A continuous production system for low-moisture methanesulfonyl fluoride according to any one of claims 1 to 6, characterized in that, The continuous distillation apparatus includes a falling film evaporator (6), a distillation column (8), and a bottom receiving tank (7). The feed inlet of the falling film evaporator (6) is connected to the oil phase outlet of the low-temperature water separation device, the discharge outlet of the falling film evaporator (6) is connected to the feed inlet of the distillation column (8), the discharge outlet of the heavy component of the distillation column (8) is connected to the feed inlet of the bottom receiving tank (7), and the discharge outlet of the bottom receiving tank (7) is connected to the finished product tank (10).

8. The continuous production system for low-moisture methanesulfonyl fluoride according to claim 7, characterized in that, The continuous distillation apparatus also includes a control unit for controlling the discharge of the bottom receiving tank (7). The discharge port of the bottom receiving tank (7) is connected to the finished product tank (10) and the ambient temperature phase separation device through pipelines. The bottom receiving tank (7) is equipped with a level gauge for monitoring the material height in the tank and a moisture meter for monitoring the moisture content of the material. The level gauge and the moisture meter are electrically connected to the control unit. The control unit switches the diversion path according to the detection results of the level gauge and the moisture meter, and guides the material in the bottom receiving tank (7) to the finished product tank (10) or the ambient temperature phase separation device.

9. A continuous production system for low-moisture methanesulfonyl fluoride according to claim 7, characterized in that, The continuous distillation apparatus also includes a top receiving tank (9), the inlet of which is connected to the light component outlet of the distillation column (8), and the outlet of which is connected to the inlet of the ambient temperature phase separation device.

10. A continuous production system for low-moisture methanesulfonyl fluoride according to claim 9, characterized in that, The continuous distillation apparatus also includes a control unit for controlling the discharge of the top receiving tank (9). The top receiving tank (9) is equipped with a level gauge for monitoring the material height inside the tank. A discharge pump is provided between the discharge port of the top receiving tank (9) and the inlet of the ambient temperature phase separation device. The level gauge and the discharge pump are electrically connected to the control unit. The control unit controls the start and stop of the discharge pump according to the detection result of the level gauge.

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