An electrolytic fluorination device for trifluoromethylsulfonamide

Abstract

The present invention relates to the field of electrolysis technology, and particularly relates to an electrolytic fluorination device for trifluoromethanesulfonamide, comprising: a preparation box, the inner wall of the preparation box is fixedly connected with an electrolytic cell; an adaptive electrolysis adjustment mechanism, the adaptive electrolysis adjustment mechanism includes an anode and a cathode for electrolytic treatment. The temperature of the electrode surface is monitored in real time by an infrared thermometer, and then the concentration of trifluoromethanesulfonamide is fed back, and the electrolysis conditions are automatically adjusted according to the temperature change to prevent the electrolysis reaction from being too violent and reduce the occurrence of side reactions. The infrared thermometer transmits the monitored temperature data to the PLC controller, and the PLC controller automatically adjusts the second electric telescopic rod according to the temperature feedback, so that the second telescopic rod pushes the conductive sheet to slide on the resistance plate, thereby changing the current and voltage between the electrodes, and then controlling the first motor, and further driving the bidirectional screw to rotate in cooperation with the limiting rod to dynamically adjust the distance between the anode and the cathode.

Description

Technical Field

[0001] The present invention relates to the field of electrolysis technology, and particularly to an electrolytic fluorination device for trifluoromethanesulfonamide. Background Art

[0002] Trifluoromethanesulfonamide is an organic compound. It is a strongly acidic sulfonamide. Due to the strong electron-withdrawing effect of its trifluoromethyl group, the electron density on the nitrogen atom of the sulfonamide is significantly reduced, thereby enhancing its acidity. Trifluoromethanesulfonamide is commonly used as a strong acid catalyst in organic synthesis or as an intermediate for other chemical reactions, especially playing an important role in the reaction of forming carbon-nitrogen bonds. In addition, due to its high stability and relatively low toxicity, it also has certain applications in the fields of medicine and materials science. In order to enhance the biological activity of trifluoromethylsulfonamide fluoride, improve pharmacokinetic properties (such as enhancing metabolic stability and biofilm permeability), increase chemical stability, and regulate intermolecular interactions, thereby optimizing molecular properties and making it more suitable for drug development or as a key intermediate for synthesizing complex molecules, electrolytic fluorination of trifluoromethylsulfonamide fluoride is required. And the process of electrolytic fluorination is usually carried out in an electrolytic cell. For example, a new electrolytic cell for hydrogen fluoride electrolysis disclosed in the application number CN202110221655.1 is used for electrolytic treatment in an electrolytic cell.

[0003] When treating trifluoromethanesulfonamide in an electrolytic cell, usually the same voltage and current intensity are applied to two electrodes (anode and cathode). (The applied voltage and current intensity are the same, and there is always the same voltage difference between the two electrodes in actual operation). This unified electrolytic condition can ensure the stability and consistency of the electrolytic process, but this also means that in some cases, the potential difference between the electrodes cannot be flexibly adjusted, thus affecting the electrolytic efficiency or selectivity. Therefore, during the electrolysis process, as the electrolysis of trifluoromethanesulfonamide proceeds, the concentration of trifluoromethanesulfonamide will gradually decrease. Therefore, when treating trifluoromethanesulfonamide with the same voltage and current intensity, due to the consumption of trifluoromethanesulfonamide and the voltage and current still continuing the electrolysis at the original intensity, the electrolytic reaction will be too intense, causing unnecessary side reactions, reducing the selectivity of the target product, and possibly increasing the by-products, affecting the purity of the final product. Therefore, the existing electrolytic cell cannot automatically adjust the voltage intensity and current magnitude according to the concentration of trifluoromethanesulfonamide. Summary of the Invention

[0004] Aiming at the above-mentioned drawbacks of the prior art, the present invention provides an electrolytic fluorination device for trifluoromethanesulfonamide, which can effectively solve the problem that the existing electrolytic cell cannot automatically adjust the voltage intensity and current magnitude according to the concentration of trifluoromethanesulfonamide.

[0005] To achieve the above object, the present invention is realized through the following technical solutions:

[0006] The present invention provides an electrolytic fluorination device for trifluoromethanesulfonamide, comprising:

[0007] A preparation box, the inner wall of which is fixedly connected with an electrolytic cell;

[0008] An adaptive electrolysis adjustment mechanism, which includes an anode and a cathode for electrolytic treatment. The outer walls of the anode and the cathode are in airtight sliding contact with a protective shell. The outer wall of the protective shell is fixedly connected with a connecting shell. A connecting port is opened between the connecting shell and the protective shell. An infrared thermometer is fixedly connected to the inner wall of the connecting shell. The anode and the cathode are commonly electrically connected to a sliding rheostat. The adaptive electrolysis adjustment mechanism further includes an electrode adjustment component for adjusting the distance between the anode and the cathode;

[0009] A gas supply and mixing mechanism, which includes an exhaust pump for injecting fluorine gas into the electrolytic cell. A rotating groove is opened on the inner bottom wall of the electrolytic cell. The inner wall of the rotating groove is airtight and rotatably provided with a first rotating plate. A plurality of air inlet pipes are embedded in the first rotating plate, and one-way valves are arranged in the air inlet pipes.

[0010] Preferably, the electrode adjustment component includes a first motor fixedly connected to the outer wall of the preparation box. The output end of the first motor is fixedly connected with a bidirectional screw rod. A limiting rod is fixedly connected to the inner wall of the preparation box. Both ends of the bidirectional screw rod are threadedly connected with threaded blocks, and the limiting rod slidably penetrates through the two threaded blocks. The bottom ends of the two threaded blocks are respectively fixedly connected with the top ends of the cathode and the anode. A bidirectional telescopic rod is fixedly connected between the two threaded blocks. The top end of the bidirectional telescopic rod is fixedly connected with an adjustment shell, and the sliding rheostat is located in the adjustment shell.

[0011] Preferably, sliding grooves are opened on both inner walls of the electrolytic cell. The inner walls of the sliding grooves are slidably connected with connecting telescopic rods. The fixed ends of the connecting telescopic rods are embedded with first permanent magnets. The telescopic ends of the connecting telescopic rods are fixedly connected with the outer wall of the protective shell. Extension plates are fixedly connected to both outer walls of the preparation box. The bottom ends of the extension plates are fixedly connected with first electric telescopic rods. The telescopic ends of the first electric telescopic rods are fixedly connected with second permanent magnets that are magnetically attracted to the first permanent magnets. The infrared thermometer is electrically connected to a PLC controller to form a detection circuit.

[0012] Preferably, the slide rheostat includes a resistance plate fixedly connected to the top wall inside the adjustment housing. A second electric telescopic rod is fixedly connected to the inner wall of the adjustment housing. The telescopic end of the second electric telescopic rod is fixedly connected to a conductive sheet that makes sliding contact with the resistance plate. The resistance plate and the conductive sheet form an adjustment circuit. During the sliding process of the conductive sheet on the resistance plate away from the second electric telescopic rod, the resistance of the slide rheostat in the adjustment circuit gradually increases. The PLC controller is electrically connected to the second electric telescopic rod and the first motor to form a control circuit.

[0013] Preferably, the gas supply and mixing mechanism further includes a gas storage tank fixedly connected to the outer wall of the preparation tank, and fluorine gas is stored in the gas storage tank. A second motor is fixedly connected to the bottom end of the preparation tank. The output end of the second motor is fixedly connected to a second rotating plate. The top end of the second rotating plate is fixedly connected to an exhaust pump. The output end of the exhaust pump is fixedly connected to a connecting pipe. The output end of the connecting pipe is fixedly connected to an exhaust hood. The exhaust hood is fixedly connected to the bottom end of the first rotating plate. The air suction end of the exhaust pump is fixedly connected to an air inlet ring. The outer wall of the air inlet ring is rotatably connected to a connecting ring. The inner wall of the connecting ring is fixedly communicated with an air suction pipe. The other end of the air suction pipe passes through the outer wall of the preparation tank and is communicated with the inside of the gas storage tank.

[0014] Preferably, it further includes a temperature control mechanism. The temperature control mechanism further includes a cooling groove opened inside the first rotating plate. A refrigeration pipe is arranged on the inner wall of the cooling groove. The top end of the second rotating plate is fixedly connected to a water pump. The water discharge end of the water pump passes through the exhaust hood and the first rotating plate and is connected to one end of the refrigeration pipe. The other end of the refrigeration pipe is fixedly communicated with a drain pipe, and the drain pipe passes through the first rotating plate and the exhaust hood and extends to the inner bottom of the preparation tank.

[0015] Preferably, a semiconductor refrigeration plate is embedded in the inner bottom wall of the preparation tank, and the refrigeration end of the semiconductor refrigeration plate faces the inside of the preparation tank, and the heating end of the semiconductor refrigeration plate faces the lower part of the preparation tank. Refrigerating water is poured between the preparation tank and the electrolytic cell. The PLC controller is electrically connected to the exhaust pump and the semiconductor refrigeration plate to form a control circuit.

[0016] Preferably, a preparator is fixedly connected to the top end of the support plate. A feeding port is jointly opened at the top ends of the preparator and the preparation tank, and a first sealing plug is arranged in the feeding port. A first pumping pump is fixedly connected to the bottom end of the support plate. The pumping end of the first pumping pump is fixedly connected to a pumping pipe communicated with the outlet of the preparator. The discharging end of the first pumping pump is fixedly connected to a discharging pipe, and the other end of the discharging pipe is located above the electrolytic cell. A cleaning port is opened on the outer wall of the preparation tank, and a second sealing plug is arranged in the cleaning port. A gas collector is fixedly connected to the outer wall of the preparation tank. An air outlet pipe is fixedly communicated between the gas collector and the inside of the preparation tank. A collection tank is fixedly connected to the outer wall of the preparation tank. A second pumping pump is fixedly connected to the outer wall of the preparation tank. The pumping end of the second pumping pump is communicated with the inside of the electrolytic cell, and the discharging end of the second pumping pump is communicated with the collection tank. A support frame is fixedly connected to the bottom end of the preparation tank.

[0017] The technical solution provided by the present invention has the following beneficial effects compared with the known prior art:

[0018] 1. The temperature on the surface of the electrode is monitored in real time by an infrared thermometer, and then the concentration of trifluoromethanesulfonamide is fed back. According to the temperature change, the electrolysis conditions are automatically adjusted to prevent the electrolysis reaction from being too violent and reduce the occurrence of side reactions. The infrared thermometer transmits the monitored temperature data to the PLC controller. The PLC controller automatically adjusts the second electric telescopic rod according to the temperature feedback, so that the second telescopic rod pushes the conductive sheet to slide on the resistance plate, thereby changing the current and voltage between the electrodes. Then, the first motor is controlled, and then the bidirectional screw rod is driven to rotate in cooperation with the limiting rod to dynamically adjust the distance between the anode and the cathode to maintain an appropriate electric field strength, so as to achieve real-time adjustment of the voltage and current intensity of the electrode according to the concentration of trifluoromethanesulfonamide, thereby optimizing the electrolysis conditions and improving the reaction efficiency and product selectivity.

[0019] 2. According to the concentration of trifluoromethanesulfonamide fed back by the temperature monitored in real time, the PLC controller automatically adjusts the power of the exhaust pump to dynamically control the amount of fluorine gas injected into the electrolytic cell. The reason for this dynamic adjustment is that the concentration of fluorine gas and other reactants needs to be kept balanced during the electrolysis process. As the concentration of trifluoromethanesulfonamide decreases, the electrolysis reaction rate may decrease. Therefore, by slowly reducing the injection rate of fluorine gas, the chemical balance can be maintained, ensuring that the electrolysis reaction proceeds under the best conditions, thereby improving the reaction efficiency. Description of the Drawings

[0020] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0021] Figure 1 Schematic three-dimensional structure of the present invention Figure 1 ;

[0022] Figure 2 Schematic three-dimensional structure of the present invention Figure 2 ;

[0023] Figure 3 Schematic cross-sectional three-dimensional structure diagram of the present invention;

[0024] Figure 4 Schematic cross-sectional three-dimensional structure diagram of the internal part of the present invention;

[0025] Figure 5 Schematic cross-sectional three-dimensional structure diagram of the connection shell part of the present invention;

[0026] Figure 6 Schematic three-dimensional structure diagram of the partial internal part of the present invention;

[0027] Figure 7 Schematic three-dimensional structure diagram of the electrolytic cell of the present invention;

[0028] Figure 8 Schematic cross-sectional three-dimensional structure diagram of the first rotating plate of the present invention.

[0029] Reference numerals: 1, preparation tank; 2, electrolytic cell; 3, adaptive electrolysis adjustment mechanism; 31, anode; 32, cathode; 33, protective shell; 34, connecting shell; 35, infrared thermometer; 36, electrode adjustment assembly; 361, first motor; 362, bidirectional screw; 363, limiting rod; 364, threaded block; 365, bidirectional telescopic rod; 366, adjustment shell; 37, sliding groove; 38, connecting telescopic rod; 39, extension plate; 310, first electric telescopic rod; 311, second permanent magnet block; 312, support plate; 313, conductive sheet; 314, resistance plate; 315, second electric telescopic rod; 4, gas supply and mixing mechanism; 41, exhaust pump; 42, first rotating plate; 43, intake pipe; 44, gas storage tank; 45, second motor; 46, second rotating plate; 47, connecting pipe; 48, exhaust hood; 49, temperature control mechanism; 491, cooling tank; 492, refrigeration pipe; 493, water pump; 494, drain pipe; 495, semiconductor refrigeration plate; 410, intake ring; 411, connecting ring; 412, suction pipe; 5, preparator; 6, feeding port; 7, first feeding pump; 8, feeding pipe; 9, discharging pipe; 10, cleaning port; 11, gas collector; 12, outlet pipe; 13, collection tank; 14, second feeding pump; 15, support frame. Detailed implementation manners

[0030] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are some, but not all, of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0031] The present invention will be further described below with reference to the embodiments.

[0032] Embodiment: Refer to Figures 1 to 8 , an electrolytic fluorination device for trifluoromethylsulfonamide, comprising: a preparation tank 1, and an electrolytic cell 2 fixedly connected to the inner wall of the preparation tank 1;

[0033] Through the adaptive electrolysis adjustment mechanism 3, the voltage and current of the electrodes can be adaptively adjusted according to the concentration of the electrolysis raw materials. Refer to Figures 1 to 5, the adaptive electrolysis adjustment mechanism 3 includes an anode 31 and a cathode 32 for electrolysis treatment. The outer walls of the anode 31 and the cathode 32 are in airtight sliding contact with a protective shell 33. A connecting shell 34 is fixedly connected to the outer wall of the protective shell 33. A connection port is provided between the connecting shell 34 and the protective shell 33. An infrared thermometer 35 is fixedly connected to the inner wall of the connecting shell 34. The anode 31 and the cathode 32 are commonly electrically connected to a rheostat. The adaptive electrolysis adjustment mechanism 3 further includes an electrode adjustment component 36 for adjusting the distance between the anode 31 and the cathode 32. There is no electrolyte between the protective shell 33 and the connecting shell 34;

[0034] Among them, the electrode adjustment component 36 includes a first motor 361 fixedly connected to the outer wall of the preparation tank 1. The output end of the first motor 361 is fixedly connected to a bidirectional screw 362. A limiting rod 363 is fixedly connected to the inner wall of the preparation tank 1. Both ends of the bidirectional screw 362 are threadedly connected with threaded blocks 364, and the limiting rod 363 slidably penetrates through the two threaded blocks 364. The bottom ends of the two threaded blocks 364 are respectively fixedly connected to the top ends of the cathode 32 and the anode 31. A bidirectional telescopic rod 365 is fixedly connected between the two threaded blocks 364. The top end of the bidirectional telescopic rod 365 is fixedly connected to an adjustment shell 366, and the rheostat is located inside the adjustment shell 366. The threads on both sides of the bidirectional screw 362 are opposite, which can make the two threaded blocks 364 move in opposite directions.

[0035] The following structure can reflect the change in the concentration of the electrolysis raw material. Refer to Figure 4 , sliding grooves 37 are provided on both inner walls of the electrolytic cell 2. A connecting telescopic rod 38 is slidably connected to the inner wall of the sliding groove 37. A first permanent magnet is embedded at the fixed end of the connecting telescopic rod 38. The telescopic end of the connecting telescopic rod 38 is fixedly connected to the outer wall of the protective shell 33. Extension plates 39 are fixedly connected to both outer walls of the preparation tank 1. A first electric telescopic rod 310 is fixedly connected to the bottom end of the extension plate 39. A second permanent magnet 311 magnetically attracted to the first permanent magnet is fixedly connected to the telescopic end of the first electric telescopic rod 310. The infrared thermometer 35 is electrically connected to a PLC controller to form a detection circuit. The connecting telescopic rod 38 can make the protective shell 33 and the connecting shell 34 move synchronously during the movement of the two electrodes. And the first electric telescopic rod 310 is preset to move slowly downward, and can automatically and slowly reset after it cannot move downward, and this cycle continues.

[0036] Among them, the sliding rheostat includes a resistance plate 314 fixedly connected to the inner top wall of the adjustment shell 366. A second electric telescopic rod 315 is fixedly connected to the inner wall of the adjustment shell 366. The telescopic end of the second electric telescopic rod 315 is fixedly connected to a conductive sheet 313 that slidably contacts the resistance plate 314. The resistance plate 314 and the conductive sheet 313 form an adjustment circuit. During the sliding process of the conductive sheet 313 on the resistance plate 314 away from the second electric telescopic rod 315, the resistance of the sliding rheostat in the adjustment circuit gradually increases. The PLC controller is electrically connected to the second electric telescopic rod 315 and the first motor 361 to form a control circuit.

[0037] The gas supply and mixing mechanism 4 can supply the required gas in real time and adjust it in real time. Refer to Figure 6 、 Figure 7 The gas supply and mixing mechanism 4 includes an exhaust pump 41 for injecting fluorine gas into the electrolytic cell 2. A rotating groove is provided on the inner bottom wall of the electrolytic cell 2. The inner wall of the rotating groove is hermetically and rotatably provided with a first rotating plate 42. A plurality of air inlet pipes 43 are embedded in the first rotating plate 42, and check valves are provided in the air inlet pipes 43. The check valves can prevent the electrolyte from entering the air inlet pipes 43.

[0038] Among them, the gas supply and mixing mechanism 4 further includes a gas storage tank 44 fixedly connected to the outer wall of the preparation box 1, and fluorine gas is stored in the gas storage tank 44. A second motor 45 is fixedly connected to the bottom end of the preparation box 1, and the second motor 45 has waterproof performance. The output end of the second motor 45 is fixedly connected to a second rotating plate 46. The top end of the second rotating plate 46 is fixedly connected to the exhaust pump 41. The output end of the exhaust pump 41 is fixedly connected to a connecting pipe 47. The output end of the connecting pipe 47 is fixedly connected to an exhaust hood 48. The exhaust hood 48 is fixedly connected to the bottom end of the first rotating plate 42. The air suction end of the exhaust pump 41 is fixedly connected to an air inlet ring 410. The outer wall of the air inlet ring 410 is rotatably connected to a connecting ring 411. The inner wall of the connecting ring 411 is fixedly communicated with an air suction pipe 412. The other end of the air suction pipe 412 passes through the outer wall of the preparation box 1 and is connected to the inside of the gas storage tank 44.

[0039] The electrolysis temperature can be controlled by the temperature control mechanism 49. Refer to Figure 8 The temperature control mechanism 49 further includes a cooling groove 491 opened inside the first rotating plate 42. A refrigeration pipe 492 is provided on the inner wall of the cooling groove 491. The top end of the second rotating plate 46 is fixedly connected to a water pump 493. The drainage end of the water pump 493 passes through the exhaust hood 48 and the first rotating plate 42 and is connected to one end of the refrigeration pipe 492. The other end of the refrigeration pipe 492 is fixedly communicated with a drainage pipe 494, and the drainage pipe 494 passes through the first rotating plate 42 and the exhaust hood 48 and extends to the inner bottom of the preparation box 1.

[0040] Among them, a semiconductor refrigeration plate 495 is embedded in the inner bottom wall of the preparation tank 1, and the refrigeration end of the semiconductor refrigeration plate 495 faces the inside of the preparation tank 1, and the heating end of the semiconductor refrigeration plate 495 faces the lower part of the preparation tank 1. Refrigerating water is poured between the preparation tank 1 and the electrolytic cell 2. The PLC controller is electrically connected to the exhaust pump 41 and the semiconductor refrigeration plate 495 to form a control loop.

[0041] A preparator 5 is fixedly connected to the top end of the support plate 312. The preparator 5 and the top end of the preparation tank 1 are jointly provided with a feeding port 6, and a first sealing plug is arranged in the feeding port 6. The bottom end of the support plate 312 is fixedly connected to a first feeding pump 7. The feeding end of the first feeding pump 7 is fixedly connected to a feeding pipe 8 communicated with the outlet of the preparator 5. The discharging end of the first feeding pump 7 is fixedly connected to a discharging pipe 9, and the other end of the discharging pipe 9 is located above the electrolytic cell 2. A cleaning port 10 is arranged on the outer wall of the preparation tank 1, and a second sealing plug is arranged in the cleaning port 10. A gas collector 11 is fixedly connected to the outer wall of the preparation tank 1. An air outlet pipe 12 is fixedly communicated between the gas collector 11 and the inside of the preparation tank 1. A collection tank 13 is fixedly connected to the outer wall of the preparation tank 1. A second feeding pump 14 is fixedly connected to the outer wall of the preparation tank 1. The feeding end of the second feeding pump 14 is communicated with the inside of the electrolytic cell 2, and the discharging end of the second feeding pump 14 is communicated with the collection tank 13. A support frame 15 is fixedly connected to the bottom end of the preparation tank 1.

[0042] The working principle of the present invention is as follows:

[0043] First, the raw materials for preparing trifluoromethanesulfonamide, trifluoromethanesulfonic acid and ammonia, are put into the preparator 5 through the feeding port 6. The trifluoromethanesulfonamide is prepared by the preparator 5 and turned into a liquid. The liquid trifluoromethanesulfonamide in the preparator 5 is pumped out by the first feeding pump 7, and the liquid trifluoromethanesulfonamide is discharged into the electrolytic cell 2 through the discharging pipe 9. The electrolyte is discharged into the electrolytic cell 2 through the cleaning port 10, and then the second sealing plug is reinserted into the cleaning port 10.

[0044] The fluorine gas in the gas storage tank 44 is pumped out by the exhaust pump 41, and the fluorine gas is discharged into the exhaust hood 48 through the connecting pipe 47. The fluorine gas is discharged into the electrolyte and liquid trifluoromethylsulfonamide in the electrolytic cell 2 through the inlet pipe 43. And the second motor 45 is started to drive the second rotating plate 46 to rotate. The exhaust pump 41 is driven to rotate synchronously by the second rotating plate 46, and then the exhaust hood 48 is driven to rotate synchronously. Finally, the first rotating plate 42 is driven to rotate, so that the fluorine gas is discharged into the electrolytic cell 2 in all directions. The electrolyte and trifluoromethylsulfonamide are mixed by the slow rotation of the first rotating plate 42, and the fluorination is made more uniform during the subsequent electrofluorination process. At the same time, the semiconductor refrigeration plate 495 needs to be started to cool the chilled water in the preparation tank 1. Then the water pump 493 is started, and the chilled water is discharged into the refrigeration pipe 492 through the water pump 493, so that the refrigeration pipe 492 cools the electrolyte, and the electrolyte is at about -10°C. This temperature can ensure that the fluorination reaction proceeds under efficient and controllable conditions, and at the same time reduce the occurrence of side reactions;

[0045] By energizing the sliding rheostat, the anode 31 and the cathode 32 are energized, and trifluoromethylsulfonamide is electrofluorinated. At the same time, the concentration of trifluoromethylsulfonamide will gradually decrease due to the electrofluorination of trifluoromethylsulfonamide. Therefore, the supply of reactants is insufficient. Coupled with the relatively high voltage and current intensity, the electrolysis conditions may be too intense, promoting unnecessary side reactions. The increase in side reactions will lead to a decrease in the selectivity of the target product and an increase in by-products, affecting the purity of the final product. Therefore, the electrolysis of trifluoromethylsulfonamide requires real-time regulation of voltage and current intensity. As the electrolysis concentration of trifluoromethylsulfonamide decreases and electrolysis is carried out at high voltage and current intensity, excessive energy input will occur. Especially when the concentration of trifluoromethylsulfonamide is low, the electrolysis reaction rate decreases, and the effect of energy conversion into reactants decreases. The excess energy will cause the temperature of the electrolyte to rise, which is most obvious on the surface of the electrode. The reason is that the electrofluorination reaction is most intense near the electrode;

[0046] Therefore, by starting the first electric telescopic rod 310, the first electric telescopic rod 310 pushes the second permanent magnet block 311 to slide downward slowly, and then drives the second permanent magnet block 311 and the connecting telescopic rod 38 to move synchronously, and then drives the protective shell 33 and the connecting shell 34 to move synchronously. The surface of the electrode can be cleaned by the movement of the protective shell 33. The reason is that impurities or other reaction intermediates in the electrolyte may be adsorbed on the surface of the electrode, hindering the progress of the electrochemical reaction. Therefore, the electrode needs to be cleaned, and the temperature of the electrode surface is monitored in real time by the infrared thermometer 35 during the cleaning process. When the monitored temperature rises, it means that the concentration of trifluoromethylsulfonamide has decreased. Therefore, the voltage and current need to be adjusted;

[0047] The measured temperature data is transmitted to the PLC controller through the infrared thermometer 35, and then the PLC controller controls the start of the second electric telescopic rod 315. The second electric telescopic rod 315 pushes the conductive sheet 313 forward (the moving distance of the conductive sheet 313 is proportional to the temperature measured by the infrared ray). The conductive sheet 313 moves on the resistance plate 314, thereby changing the current passing through the electrode, and further changing the current intensity and voltage intensity, so as to adjust the current and voltage passing through the electrode in real time according to the concentration of trifluoromethanesulfonamide, so as to ensure that the electrofluorination reaction is carried out under optimal conditions, thereby improving the reaction efficiency, reducing unnecessary side reactions, and improving the selectivity and yield of the target product. And the PLC controller controls the power of the exhaust pump 41 to be gradually reduced to slowly reduce the fluorine gas injected into the electrolytic cell 2. The reason is that during the electrolysis process, the concentration of fluorine gas and other reactants needs to maintain a certain balance. The decrease in the concentration of trifluoromethanesulfonamide may lead to a decrease in the electrolysis reaction rate. Therefore, it is necessary to slowly reduce the injection rate of fluorine gas to maintain the chemical balance.

[0048] As the concentration of trifluoromethanesulfonamide decreases, the ion concentration in the electrolyte will also decrease, which will lead to an increase in resistance (the reason is that the decrease in the ion concentration and mobility in the electrolyte leads to a decrease in conductivity, thereby causing an increase in resistance). In order to maintain an appropriate electric field strength, it is necessary to adjust the electrode distance to ensure that the reaction continues to proceed efficiently. Therefore, the PLC controller adjusts the distance between the two electrodes in real time according to the feedback temperature. As the concentration of trifluoromethanesulfonamide gradually decreases, the distance between the two electrodes is gradually reduced. The reason is that approaching the electrodes can increase the electric field strength, thereby maintaining an appropriate current density and ensuring that the reaction continues to proceed efficiently. Therefore, the PLC controller controls the start of the first motor 361, the first motor 361 drives the bidirectional screw 362 to rotate, and then through the limit of the two threaded blocks 364 by the limit rod 363, the two threaded blocks 364 drive the two electrodes to slowly approach, move to a suitable position (adjusted according to the feedback temperature), and then stop the second motor 45.

[0049] During the electrolysis process, the generated gas is collected through the gas collector 11. When the electrolysis is completed (according to past electrolysis experience), the electrolyte in the electrolytic cell 2 is pumped out through the second pumping pump 14 and discharged into the collection box 13 for subsequent treatment.

[0050] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements on some of the technical features; and these modifications or replacements will not cause the essence of the corresponding technical solutions to deviate from the protection scope of the technical solutions of the various embodiments of the present invention.

Claims

1. An electrolytic fluorination device for trifluoromethylsulfonamide, characterized in that, Including: A preparation box (1), the inner wall of the preparation box (1) is fixedly connected with an electrolytic cell (2); An adaptive electrolysis adjustment mechanism (3), the adaptive electrolysis adjustment mechanism (3) includes an anode (31) and a cathode (32) for electrolysis treatment, the outer walls of the anode (31) and the cathode (32) are in airtight sliding contact with a protective shell (33), the outer wall of the protective shell (33) is fixedly connected with a connecting shell (34), a connecting port is provided between the connecting shell (34) and the protective shell (33), the inner wall of the connecting shell (34) is fixedly connected with an infrared thermometer (35), the anode (31) and the cathode (32) are commonly electrically connected to a sliding rheostat, and the adaptive electrolysis adjustment mechanism (3) further includes an electrode adjustment component (36) for adjusting the distance between the anode (31) and the cathode (32); A gas supply and mixing mechanism (4), the gas supply and mixing mechanism (4) includes an exhaust pump (41) for injecting fluorine gas into the electrolytic cell (2), a rotating groove is provided on the inner bottom wall of the electrolytic cell (2), a first rotating plate (42) is rotatably arranged in the inner wall of the rotating groove in an airtight manner, a plurality of air inlet pipes (43) are embedded in the first rotating plate (42), and a one-way valve is arranged in the air inlet pipe (43); The electrode adjustment component (36) includes a first motor (361) fixedly connected to the outer wall of the preparation box (1), the output end of the first motor (361) is fixedly connected with a bidirectional screw rod (362), a limiting rod (363) is fixedly connected to the inner wall of the preparation box (1), both ends of the bidirectional screw rod (362) are threadedly connected with threaded blocks (364), and the limiting rod (363) slidably penetrates through the two threaded blocks (364), the bottom ends of the two threaded blocks (364) are respectively fixedly connected with the top ends of the cathode (32) and the anode (31), a bidirectional telescopic rod (365) is fixedly connected between the two threaded blocks (364), the top end of the bidirectional telescopic rod (365) is fixedly connected with an adjustment shell (366), and the sliding rheostat is located in the adjustment shell (366); Sliding grooves (37) are provided on both inner walls of the electrolytic cell (2), a connecting telescopic rod (38) is slidably connected to the inner wall of the sliding groove (37), a first permanent magnet is embedded in the fixed end of the connecting telescopic rod (38), the telescopic end of the connecting telescopic rod (38) is fixedly connected with the outer wall of the protective shell (33), extension plates (39) are fixedly connected to both outer walls of the preparation box (1), a first electric telescopic rod (310) is fixedly connected to the bottom end of the extension plate (39), a second permanent magnet (311) magnetically attracted to the first permanent magnet is fixedly connected to the telescopic end of the first electric telescopic rod (310), and the infrared thermometer (35) is electrically connected to a PLC controller to form a detection circuit; The sliding rheostat includes a resistance plate (314) fixedly connected to the inner top wall of an adjustment housing (366). A second electric telescopic rod (315) is fixedly connected to the inner wall of the adjustment housing (366). The telescopic end of the second electric telescopic rod (315) is fixedly connected to a conductive sheet (313) that is in sliding contact with the resistance plate (314). The resistance plate (314) and the conductive sheet (313) form an adjustment circuit. During the sliding process of the conductive sheet (313) on the resistance plate (314) away from the second electric telescopic rod (315), the resistance of the sliding rheostat in the adjustment circuit gradually increases. The PLC controller is electrically connected to the second electric telescopic rod (315) and the first motor (361) to form a control circuit.

2. The electrolytic fluorination equipment for trifluoromethylsulfonamide according to claim 1, characterized in that, The gas supply and mixing mechanism (4) further includes a gas storage tank (44) fixedly connected to the outer wall of the preparation tank (1), and fluorine gas is stored in the gas storage tank (44). A second motor (45) is fixedly connected to the bottom end of the preparation tank (1). The output end of the second motor (45) is fixedly connected to a second rotating plate (46). The top end of the second rotating plate (46) is fixedly connected to an exhaust pump (41). The output end of the exhaust pump (41) is fixedly connected to a connecting pipe (47). The output end of the connecting pipe (47) is fixedly connected to an exhaust hood (48). The exhaust hood (48) is fixedly connected to the bottom end of the first rotating plate (42). The air suction end of the exhaust pump (41) is fixedly connected to an intake ring (410). The outer wall of the intake ring (410) is rotatably connected to a connecting ring (411). The inner wall of the connecting ring (411) is fixedly communicated with an air suction pipe (412). The other end of the air suction pipe (412) passes through the outer wall of the preparation tank (1) and is communicated with the inside of the gas storage tank (44).

3. An electrolytic fluorination device for trifluoromethylsulfonamide according to claim 2, characterized in that, It further includes a temperature control mechanism (49). The temperature control mechanism (49) further includes a cooling groove (491) formed inside the first rotating plate (42). A refrigeration pipe (492) is arranged on the inner wall of the cooling groove (491). A water pump (493) is fixedly connected to the top end of the second rotating plate (46). The drainage end of the water pump (493) passes through the exhaust hood (48) and the first rotating plate (42) and is connected to one end of the refrigeration pipe (492). The other end of the refrigeration pipe (492) is fixedly communicated with a drainage pipe (494), and the drainage pipe (494) passes through the first rotating plate (42) and the exhaust hood (48) and extends to the inner bottom of the preparation tank (1).

4. An electrolytic fluorination apparatus for trifluoromethylsulfonamide according to claim 3, characterized in that, A semiconductor refrigeration plate (495) is embedded in the inner bottom wall of the preparation tank (1). The refrigeration end of the semiconductor refrigeration plate (495) faces the inside of the preparation tank (1), and the heating end faces downward of the preparation tank (1). Refrigerated water is poured between the preparation tank (1) and the electrolytic cell (2). The PLC controller is electrically connected to the exhaust pump (41) and the semiconductor refrigeration plate (495) to form a control circuit.

5. An electrolytic fluorination apparatus for trifluoromethylsulfonamide according to claim 1, characterized in that, The inner wall of the preparation box (1) is fixedly connected with a support plate (312). The top end of the support plate (312) is fixedly connected with a preparator (5). The preparator (5) and the top end of the preparation box (1) are jointly provided with a feeding port (6), and a first sealing plug is arranged in the feeding port (6). The bottom end of the support plate (312) is fixedly connected with a first pumping pump (7). The pumping end of the first pumping pump (7) is fixedly connected with a pumping pipe (8) communicated with the outlet of the preparator (5). The discharging end of the first pumping pump (7) is fixedly connected with a discharging pipe (9), and the other end of the discharging pipe (9) is located above the electrolytic cell (2). The outer wall of the preparation box (1) is provided with a cleaning port (10), and a second sealing plug is arranged in the cleaning port (10). The outer wall of the preparation box (1) is fixedly connected with a gas collector (11). The gas collector (11) and the inside of the preparation box (1) are jointly and fixedly communicated with an air outlet pipe (12). The outer wall of the preparation box (1) is fixedly connected with a collection box (13). The outer wall of the preparation box (1) is fixedly connected with a second pumping pump (14). The pumping end of the second pumping pump (14) is communicated with the inside of the electrolytic cell (2). The discharging end of the second pumping pump (14) is communicated with the collection box (13). The bottom end of the preparation box (1) is fixedly connected with a support frame (15).

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