Electrolytic fluorination equipment for trifluoromethyl sulfonamide

Abstract

The invention relates to the technical field of electrolysis, in particular to trifluoromethyl sulfonamide electrolytic fluorination equipment which comprises a preparation box, and the inner wall of the preparation box is fixedly connected with an electrolytic bath; and the self-adaptive electrolysis adjusting mechanism comprises an anode and a cathode which are used for electrolytic treatment. The temperature of the surface of the electrode is monitored in real time through the infrared thermometer, then the concentration of trifluoromethyl sulfonamide is fed back, electrolysis conditions are automatically adjusted according to temperature changes, the electrolytic reaction is prevented from being too violent, side reactions are reduced, the infrared thermometer transmits monitored temperature data to the PLC, and the PLC controls the temperature of the electrode. The PLC automatically adjusts a second electric telescopic rod according to temperature feedback, so that the second telescopic rod pushes a conducting strip to slide on a resistance plate, current and voltage between electrodes are changed, then a first motor is controlled, a bidirectional screw is driven to rotate to be matched with a limiting rod, and the distance between the anode and the cathode is dynamically adjusted.

Description

Technical Field

[0001] The invention relates to the technical field of electrolysis, and in particular to an electrolytic fluorination device for trifluoromethylsulfonamide. Background Art

[0002] Trifluoromethylsulfonamide is an organic compound, which is a strongly acidic sulfonamide. Due to the strong electron-withdrawing effect of its trifluoromethyl group, the electron density on the nitrogen atom of sulfonamide is significantly reduced, thereby enhancing its acidity. Trifluoromethylsulfonamide is often used as a strong acid catalyst or as an intermediate in other chemical reactions in organic synthesis, especially in the reaction of forming carbon-nitrogen bonds. It plays an important role. 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 make trifluoromethylsulfonamide fluoride enhance the biological activity of the compound, improve the pharmacokinetic properties (such as improving metabolic stability and biomembrane permeability), increase chemical stability, and regulate intermolecular interactions, thereby optimizing the molecular properties and making it more suitable for drug development or as a key intermediate for the synthesis of complex molecules, it is necessary to electrofluorinate trifluoromethylsulfonamide, and the process of electrofluorination is usually carried out in an electrolytic cell. For example, a new electrolytic cell for hydrogen fluoride electrolysis disclosed in application number CN202110221655.1 uses an electrolytic cell for electrolysis.

[0003] When treating trifluoromethylsulfonamide in an electrolytic cell, the same voltage and current intensity are usually applied to the 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 uniform electrolysis condition ensures the stability and consistency of the electrolysis process, but it also means that in some cases, the potential difference between the electrodes cannot be flexibly adjusted, thereby affecting the electrolysis efficiency or selectivity. Therefore, during the electrolysis process, the concentration of trifluoromethylsulfonamide will gradually decrease as trifluoromethylsulfonamide is electrolyzed. Therefore, trifluoromethylsulfonamide is treated with the same voltage and current intensity. Due to the consumption of trifluoromethylsulfonamide and the voltage and current continue to be electrolyzed at the original intensity, the electrolysis reaction will be too intense, causing unnecessary side reactions, reducing the selectivity of the target product, and the by-products may increase, affecting the purity of the final product. Therefore, the existing electrolytic cell cannot automatically adjust the voltage intensity and current size according to the concentration of trifluoromethylsulfonamide. Summary of the invention

[0004] In view of the above-mentioned shortcomings of the prior art, the present invention provides an electrolytic fluorination device for trifluoromethylsulfonamide, which can effectively solve the problem that the electrolytic cell of the prior art cannot automatically adjust the voltage intensity and current size according to the concentration of trifluoromethylsulfonamide.

[0005] To achieve the above objectives, the present invention is implemented through the following technical solutions: The present invention provides an electrolytic fluorination device for trifluoromethylsulfonamide, comprising: A preparation box, the inner wall of which is fixedly connected with an electrolytic cell; An adaptive electrolysis regulating mechanism, the adaptive electrolysis regulating mechanism comprising an anode and a cathode for electrolysis treatment, the outer walls of the anode and the cathode being in airtight sliding contact with a protective shell, the outer wall of the protective shell being fixedly connected with a connecting shell, a connecting port being provided between the connecting shell and the protective shell, an infrared thermometer being fixedly connected with the inner wall of the connecting shell, the anode and the cathode being electrically connected to a sliding rheostat, and the adaptive electrolysis regulating mechanism further comprising an electrode regulating assembly for adjusting the distance between the anode and the cathode; A gas supply mixing mechanism, the gas supply mixing mechanism includes an exhaust pump for injecting fluorine gas into the electrolytic cell, the inner bottom wall of the electrolytic cell is provided with a rotating groove, the inner wall of the rotating groove is provided with a first rotating plate for airtight rotation, a plurality of air inlet pipes are embedded in the interior of the first rotating plate, and a one-way valve is provided in the air inlet pipe.

[0006] Preferably, the electrode adjustment assembly includes a first motor fixedly connected to the outer wall of the preparation box, a bidirectional screw is fixedly connected to the output end of the first motor, a limiting rod is fixedly connected to the inner wall of the preparation box, both ends of the bidirectional screw are threadedly connected to threaded blocks, and the limiting rod slides through the two threaded blocks, the bottom ends of the two threaded blocks are respectively fixedly connected to the top of the cathode and the anode, a bidirectional telescopic rod is fixedly connected between the two threaded blocks, the top of the bidirectional telescopic rod is fixedly connected to an adjustment shell, and the sliding rheostat is located in the adjustment shell.

[0007] Preferably, sliding grooves are provided on the inner walls on both sides of the electrolytic cell, and the inner walls of the sliding grooves are slidably connected with connecting telescopic rods, and the fixed ends of the connecting telescopic rods are embedded with first permanent magnet blocks, and the telescopic ends of the connecting telescopic rods are fixedly connected to the outer walls of the protective shell, and the outer walls on both sides of the preparation box are fixedly connected with extension plates, and the bottom ends of the extension plates are fixedly connected with the first electric telescopic rods, and the telescopic ends of the first electric telescopic rods are fixedly connected with the second permanent magnet blocks that are magnetically attracted to the first permanent magnet blocks, and the electrical signal of the infrared thermometer is connected with the PLC controller to form a detection loop.

[0008] Preferably, the sliding rheostat includes a resistance plate fixedly connected to the inner top wall of the adjusting shell, a second electric telescopic rod is fixedly connected to the inner wall of the adjusting shell, a conductive sheet that is in sliding contact with the resistance plate is fixedly connected to the telescopic end of the second electric telescopic rod, the resistance plate and the conductive sheet form an adjustment loop, and during the sliding process of the conductive sheet on the resistance plate toward and away from the second electric telescopic rod, the resistance of the sliding rheostat in the adjustment loop gradually increases, and the PLC controller is electrically connected to the second electric telescopic rod and the first motor to form a control loop.

[0009] Preferably, the gas supply mixing mechanism also includes a gas storage box fixedly connected to the outer wall of the preparation box, and fluorine gas is stored in the gas storage box, the bottom end of the preparation box is fixedly connected to a second motor, the output end of the second motor is fixedly connected to a second rotating plate, the top 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 exhaust end of the exhaust pump is fixedly connected to an intake ring, the outer wall of the intake ring is rotatably connected to a connecting ring, the inner wall of the connecting ring is fixedly connected to an exhaust pipe, the other end of the exhaust pipe passes through the outer wall of the preparation box and is connected to the inside of the gas storage box.

[0010] Preferably, it also includes a temperature control mechanism, which also includes a cooling groove opened inside the first rotating plate, the inner wall of the cooling groove is provided with a refrigeration pipe, the top of the second rotating plate is fixedly connected with a water pump, the drainage end of the water pump passes through the exhaust hood and the first rotating plate and is connected with one end of the refrigeration pipe, the other end of the refrigeration pipe is fixedly connected with a drainage pipe, and the drainage pipe passes through the first rotating plate and the exhaust hood and extends to the inner bottom of the preparation box.

[0011] Preferably, a semiconductor refrigeration plate is embedded in the inner bottom wall of the preparation box, and the cooling end of the semiconductor refrigeration plate faces the inside of the preparation box, and the heating end of the semiconductor refrigeration plate faces the bottom of the preparation box, and cooling water is poured between the preparation box and the electrolytic cell. The PLC controller is connected to the exhaust pump and the semiconductor refrigeration plate with electrical signals to form a control loop.

[0012] Preferably, the top of the support plate is fixedly connected to a preparation device, the preparation device and the top of the preparation box are jointly provided with a discharge port, and a first sealing plug is arranged in the discharge port, the bottom end of the support plate is fixedly connected to a first feeding pump, the feeding end of the first feeding pump is fixedly connected to a feeding pipe connected to the outlet of the preparation device, the discharge end of the first feeding pump is fixedly connected to the discharge pipe, and the other end of the discharge pipe is above the electrolytic cell, a cleaning port is opened on the outer wall of the preparation box, and a second sealing plug is arranged in the cleaning port, the outer wall of the preparation box is fixedly connected to a gas collector, the gas collector and the preparation box are jointly fixedly connected with an air outlet pipe, the outer wall of the preparation box is fixedly connected to a collecting box, the outer wall of the preparation box is fixedly connected to a second feeding pump, the feeding end of the second feeding pump is connected to the inside of the electrolytic cell, the discharge end of the second feeding pump is connected to the collecting box, and the bottom end of the preparation box is fixedly connected to a support frame.

[0013] Compared with the known prior art, the technical solution provided by the present invention has the following beneficial effects:

[0014] 1. The temperature of the electrode surface is monitored in real time by an infrared thermometer, and the concentration of trifluoromethylsulfonamide is fed back. The electrolysis conditions are automatically adjusted according to the temperature change to prevent the electrolysis reaction from being too intense 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 resistor plate, thereby changing the current and voltage between the electrodes, and then controls the first motor to drive the rotation of the bidirectional screw and the coordination of the limit rod, dynamically adjusting 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 trifluoromethylsulfonamide, thereby optimizing the electrolysis conditions and improving the reaction efficiency and product selection.

[0015] 2. According to the concentration of trifluoromethylsulfonamide fed back by the real-time temperature monitoring, 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 concentrations of fluorine gas and other reactants need to be balanced during the electrolysis process. As the concentration of trifluoromethylsulfonamide decreases, the electrolysis reaction rate may decrease. Therefore, by slowly reducing the injection rate of fluorine gas, the chemical balance can be maintained to ensure that the electrolysis reaction is carried out under optimal conditions, thereby improving the reaction efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the prior art descriptions are briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention, and for ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0017] Figure 1 The three-dimensional structure of the present invention is shown in FIG. Figure 1 ;

[0018] Figure 2 The three-dimensional structure of the present invention is shown in FIG. Figure 2 ;

[0019] Figure 3 It is a schematic diagram of a cross-sectional three-dimensional structure of the present invention;

[0020] Figure 4 It is a schematic diagram of the internal part cross-section three-dimensional structure of the present invention;

[0021] Figure 5 It is a schematic diagram of a cross-sectional three-dimensional structure of a connecting shell portion of the present invention;

[0022] Figure 6 It is a schematic diagram of a partial internal three-dimensional structure of the present invention;

[0023] Figure 7 It is a schematic diagram of the three-dimensional structure of the electrolytic cell of the present invention;

[0024] Figure 8 It is a schematic diagram of the cross-sectional three-dimensional structure of the first rotating plate of the present invention.

[0025] 1. Preparation box; 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. Limit rod; 364. Threaded block; 365. Bidirectional telescopic rod; 366. Adjusting 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. Resistor plate; 315. Second electric telescopic rod; 4. Gas supply mixer Combination mechanism; 41, exhaust pump; 42, first rotating plate; 43, air inlet pipe; 44, air storage box; 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, drainage pipe; 495, semiconductor refrigeration plate; 410, air inlet ring; 411, connecting ring; 412, air extraction pipe; 5, preparation device; 6, discharge port; 7, first extraction pump; 8, extraction pipe; 9, discharge pipe; 10, cleaning port; 11, gas collector; 12, air outlet pipe; 13, collection box; 14, second extraction pump; 15, support frame. DETAILED DESCRIPTION

[0026] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0027] The present invention will be further described below in conjunction with the embodiments.

[0028] Example: Refer to Figures 1 to 8 , an electrolytic fluorination device for trifluoromethylsulfonamide, comprising: a preparation box 1, an inner wall of which is fixedly connected an electrolytic cell 2; The voltage and current of the electrodes can be adaptively adjusted according to the concentration of the electrolytic raw materials by the adaptive electrolysis adjustment mechanism 3. Figures 1 to 5The adaptive electrolysis regulating 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, an infrared thermometer 35 is fixedly connected to the inner wall of the connecting shell 34, the anode 31 and the cathode 32 are electrically connected to a sliding rheostat, and the adaptive electrolysis regulating mechanism 3 also includes an electrode regulating component 36 for adjusting the distance between the anode 31 and the cathode 32, wherein there is no electrolyte between the protective shell 33 and the connecting shell 34; Among them, the electrode adjustment component 36 includes a first motor 361 fixedly connected to the outer wall of the preparation box 1, a bidirectional screw 362 is fixedly connected to the output end of the first motor 361, a limiting rod 363 is fixedly connected to the inner wall of the preparation box 1, both ends of the bidirectional screw 362 are threadedly connected to thread blocks 364, and the limiting rod 363 slides through the two thread blocks 364, the bottom ends of the two thread blocks 364 are respectively fixedly connected to the top of the cathode 32 and the anode 31, a bidirectional telescopic rod 365 is fixedly connected between the two thread blocks 364, the top of the bidirectional telescopic rod 365 is fixedly connected to the adjustment shell 366, and the sliding rheostat is in the adjustment shell 366, the threads on both sides of the bidirectional screw 362 are opposite, so that the two thread blocks 364 can move in opposite directions.

[0029] The following structure can feedback the concentration change of electrolytic raw materials, refer to Figure 4 The inner walls of both sides of the electrolytic cell 2 are provided with sliding grooves 37, and the inner walls of the sliding grooves 37 are slidably connected with connecting telescopic rods 38, and the fixed ends of the connecting telescopic rods 38 are embedded with first permanent magnets. The telescopic ends of the connecting telescopic rods 38 are fixedly connected to the outer walls of the protective shell 33, and the outer walls of the preparation box 1 are fixedly connected with extension plates 39, and the bottom ends of the extension plates 39 are fixedly connected with the first electric telescopic rod 310, and the telescopic ends of the first electric telescopic rod 310 are fixedly connected with the second permanent magnet 311 that is magnetically attracted to the first permanent magnet. The infrared thermometer 35 is electrically connected to the PLC controller to form a detection loop. 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 pre-set to move slowly downward, and can automatically and slowly reset after moving downward to the point where it cannot move, thereby circulating.

[0030] Among them, the sliding rheostat includes a resistor plate 314 fixedly connected to the inner top wall of the adjusting shell 366, the inner wall of the adjusting shell 366 is fixedly connected to the second electric telescopic rod 315, 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 resistor plate 314, the resistor plate 314 and the conductive sheet 313 form an adjustment loop, and during the sliding process of the conductive sheet 313 on the resistor plate 314 toward and away from the second electric telescopic rod 315, the resistance of the sliding rheostat in the adjustment loop gradually increases, and the PLC controller is electrically connected to the second electric telescopic rod 315 and the first motor 361 to form a control loop.

[0031] The required gas can be supplied and adjusted in real time by the gas supply mixing mechanism 4. Figure 6 , Figure 7 The gas supply 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 provided on the inner wall of the rotating groove for airtight rotation. A plurality of air inlet pipes 43 are embedded in the interior of the first rotating plate 42, and a one-way valve is provided in the air inlet pipe 43. The one-way valve can prevent the electrolyte from entering the air inlet pipe 43.

[0032] Among them, the gas supply mixing mechanism 4 also includes a gas storage box 44 fixedly connected to the outer wall of the preparation box 1, and fluorine gas is stored in the gas storage box 44, the bottom end of the preparation box 1 is fixedly connected to a second motor 45, and the second motor 45 is waterproof, the output end of the second motor 45 is fixedly connected to a second rotating plate 46, the top 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 exhaust 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 connected to an exhaust pipe 412, and the other end of the exhaust pipe 412 passes through the outer wall of the preparation box 1 and is connected to the inside of the gas storage box 44.

[0033] The electrolysis temperature can be controlled by the temperature control mechanism 49, see Figure 8 The temperature control mechanism 49 also includes a cooling groove 491 opened inside the first rotating plate 42, and 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 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 connected to 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.

[0034] Among them, a semiconductor refrigeration plate 495 is embedded in the inner bottom wall of the preparation box 1, and the cooling end of the semiconductor refrigeration plate 495 is facing the inside of the preparation box 1, and the heating end of the semiconductor refrigeration plate 495 is facing the bottom of the preparation box 1, and cooling water is poured between the preparation box 1 and the electrolytic cell 2. The PLC controller is connected to the exhaust pump 41 and the semiconductor refrigeration plate 495 by electrical signals to form a control loop.

[0035] The top of the support plate 312 is fixedly connected to a preparation device 5, and the top of the preparation device 5 and the preparation box 1 are jointly provided with a discharge port 6, and a first sealing plug is provided in the discharge port 6, and the bottom of the support plate 312 is fixedly connected to a first pumping pump 7, and the pumping end of the first pumping pump 7 is fixedly connected to a pumping pipe 8 connected to the outlet of the preparation device 5, and the discharge end of the first pumping pump 7 is fixedly connected to a discharge pipe 9, and the other end of the discharge pipe 9 is located above the electrolytic cell 2, and the outer wall of the preparation box 1 is provided with a cleaning port 10 , and a second sealing plug is provided in the cleaning port 10, a gas collector 11 is fixedly connected to the outer wall of the preparation box 1, and the gas collector 11 and the preparation box 1 are fixedly connected with an outlet pipe 12, a collecting box 13 is fixedly connected to the outer wall of the preparation box 1, a second extraction pump 14 is fixedly connected to the outer wall of the preparation box 1, a extraction end of the second extraction pump 14 is connected to the inside of the electrolytic cell 2, a discharge end of the second extraction pump 14 is connected to the collecting box 13, and a support frame 15 is fixedly connected to the bottom end of the preparation box 1.

[0036] The working principle of the present invention is as follows:

[0037] First, the raw materials trifluoromethylsulfonic acid and ammonia for preparing trifluoromethylsulfonamide are put into the preparation device 5 through the discharge port 6, the preparation of trifluoromethylsulfonamide is completed by the preparation device 5, and the trifluoromethylsulfonamide is converted into liquid, the liquid trifluoromethylsulfonamide in the preparation device 5 is extracted by the first extraction pump 7, the liquid trifluoromethylsulfonamide is discharged into the electrolytic cell 2 through the discharge pipe 9, the electrolyte is discharged into the electrolytic cell 2 through the cleaning port 10, and then the second sealing plug is re-inserted into the cleaning port 10.

[0038] The fluorine gas in the air storage box 44 is extracted by the exhaust pump 41, and the fluorine gas is discharged into the exhaust hood 48 through the connecting pipe 47, and the fluorine gas is discharged into the electrolyte and liquid trifluoromethylsulfonamide in the electrolytic cell 2 through the air intake pipe 43, and the second motor 45 is started to drive the second rotating plate 46 to rotate, and the exhaust pump 41 is driven to rotate synchronously through the second rotating plate 46, and then the exhaust hood 48 is driven to rotate synchronously, and 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, and the first rotating plate 42 is slowly rotated. Rotate to mix the electrolyte with trifluoromethylsulfonamide, and make the fluorination more uniform in the subsequent electrolytic fluorination process. At the same time, it is necessary to start the semiconductor refrigeration plate 495 to cool the cooling water in the preparation box 1, and then start the water pump 493 to discharge the cooling water into the cooling pipe 492 through the water pump 493, so that the cooling pipe 492 cools the electrolyte to about -10°C. This temperature can ensure that the fluorination reaction is carried out under efficient and controllable conditions, while reducing the occurrence of side reactions; By energizing the sliding rheostat, and then energizing the anode 31 and the cathode 32, the trifluoromethylsulfonamide is electrolytically fluorinated. At the same time, the concentration of trifluoromethylsulfonamide is gradually reduced by the electrolytic fluorination of trifluoromethylsulfonamide. Therefore, the insufficient supply of reactants, coupled with the higher voltage and current intensity, may cause the electrolysis conditions to be too intense, promote unnecessary side reactions, and increase the side reactions. The selectivity of the target product is reduced, the by-products increase, and the purity of the final product is affected. Therefore, the electrolysis of trifluoromethylsulfonamide requires real-time regulation of voltage and current intensity. As the electrolytic concentration of trifluoromethylsulfonamide decreases, electrolysis with high voltage and current intensity will lead to excessive energy input, especially when the concentration of trifluoromethylsulfonamide is low, the electrolytic reaction rate decreases, and the effect of converting energy into reactants is reduced. The excess energy will cause the electrolyte temperature to rise, and this temperature is most obvious on the electrode surface. The reason is that the electrolytic fluorination reaction is most intense near the electrode. Therefore, by starting the first electric telescopic rod 310, the second permanent magnet block 311 is pushed to slide slowly downward by the first electric telescopic rod 310, thereby driving the second permanent magnet block 311 and the connecting telescopic rod 38 to move synchronously, thereby driving 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 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 increases, it means that the concentration of trifluoromethylsulfonamide has decreased, so the voltage and current need to be adjusted; The measured temperature data is transmitted to the PLC controller through the infrared thermometer 35, and then the second electric telescopic rod 315 is controlled to start through the PLC controller, and the conductive sheet 313 is pushed forward by the second electric telescopic rod 315 (the moving distance of the conductive sheet 313 is proportional to the temperature measured by infrared rays), and the conductive sheet 313 moves on the resistor plate 314, thereby changing the current passed into the electrode, and then changing the current intensity and voltage intensity, so as to adjust the current and voltage passed into the electrode in real time according to the concentration of trifluoromethylsulfonamide, so as to ensure that the electrolytic fluorination 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 power of the exhaust pump 41 is gradually reduced through the PLC controller to slowly reduce the fluorine gas injected into the electrolytic cell 2. The reason is that during the electrolysis process, the concentrations of fluorine gas and other reactants need to maintain a certain balance. The reduction in the concentration of trifluoromethylsulfonamide may cause the electrolysis reaction rate to decrease, so it is necessary to slowly reduce the injection rate of fluorine gas to maintain chemical balance.

[0039] As the concentration of trifluoromethylsulfonamide decreases, the ion concentration in the electrolyte will also decrease, which will cause the resistance to increase (the reason is that the decrease in ion concentration and mobility in the electrolyte leads to a decrease in conductivity, which in turn causes an increase in resistance). In order to maintain an appropriate electric field strength, the electrode distance needs to be adjusted to ensure that the reaction continues to proceed efficiently. Therefore, the distance between the two electrodes is controlled in real time by the PLC controller according to the feedback temperature. As the concentration of trifluoromethylsulfonamide gradually decreases, the distance between the two electrodes is gradually brought closer. 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 first motor 361 is controlled to start by the PLC controller, and the bidirectional screw 362 is driven to rotate by the first motor 361. Then, the two threaded blocks 364 are limited by the limit rod 363, so that the two threaded blocks 364 drive the two electrodes to slowly approach and move to a suitable position (adjusted according to the feedback temperature), and then the second motor 45 is stopped.

[0040] During the electrolysis process, the gas generated is collected by the gas collector 11. When the electrolysis is completed (based on previous electrolysis experience), the electrolyte in the electrolytic cell 2 is extracted by the second extraction pump 14 and discharged into the collection box 13 for subsequent processing.

[0041] 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 aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or make equivalent replacements for some of the technical features therein. However, 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 embodiments of the present invention.

Claims

1. An electrolytic fluorination device for trifluoromethylsulfonamide, characterized in that: include: A preparation box (1), wherein an electrolytic cell (2) is fixedly connected to the inner wall of the preparation box (1); An adaptive electrolysis regulating mechanism (3), the adaptive electrolysis regulating mechanism (3) comprising an anode (31) and a cathode (32) for electrolysis treatment, the outer walls of the anode (31) and the cathode (32) being in airtight sliding contact with a protective shell (33), the outer wall of the protective shell (33) being fixedly connected to a connecting shell (34), a connecting port being provided between the connecting shell (34) and the protective shell (33), an infrared thermometer (35) being fixedly connected to the inner wall of the connecting shell (34), the anode (31) and the cathode (32) being electrically connected together with a sliding rheostat, the adaptive electrolysis regulating mechanism (3) further comprising an electrode regulating assembly (36) for adjusting the distance between the anode (31) and the cathode (32); A gas supply mixing mechanism (4), the gas supply mixing mechanism (4) comprising an exhaust pump (41) for injecting fluorine gas into the electrolytic cell (2), the inner bottom wall of the electrolytic cell (2) being provided with a rotating groove, the inner wall of the rotating groove being provided with a first rotating plate (42) for airtight rotation, a plurality of air inlet pipes (43) being embedded in the interior of the first rotating plate (42), and a one-way valve being provided in the air inlet pipe (43).

2. The electrolytic fluorination equipment of trifluoromethylsulfonamide according to claim 1, characterized in that: The electrode adjustment assembly (36) comprises a first motor (361) fixedly connected to the outer wall of the preparation box (1); a bidirectional screw (362) is fixedly connected to the output end of the first motor (361); a limiting rod (363) is fixedly connected to the inner wall of the preparation box (1); both ends of the bidirectional screw (362) are threadedly connected to thread blocks (364); the limiting rod (363) slides through the two thread blocks (364); the bottom ends of the two thread 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 thread blocks (364); the top end of the bidirectional telescopic rod (365) is fixedly connected to an adjustment shell (366), and the sliding rheostat is located in the adjustment shell (366).

3. The electrolytic fluorination device of trifluoromethylsulfonamide according to claim 2, characterized in that: The inner walls of both sides of the electrolytic cell (2) are provided with sliding grooves (37), the inner walls of the sliding grooves (37) are slidably connected with connecting telescopic rods (38), the fixed ends of the connecting telescopic rods (38) are embedded with first permanent magnets, the telescopic ends of the connecting telescopic rods (38) are fixedly connected to the outer walls of the protective shell (33), the outer walls of both sides of the preparation box (1) are fixedly connected with extension plates (39), the bottom ends of the extension plates (39) are fixedly connected with first electric telescopic rods (310), the telescopic ends of the first electric telescopic rods (310) are fixedly connected with second permanent magnets (311) that are magnetically attracted to the first permanent magnets, and the infrared thermometer (35) is electrically connected to a PLC controller to form a detection circuit.

4. The electrolytic fluorination device of trifluoromethylsulfonamide according to claim 3, characterized in that: The sliding rheostat comprises a resistor plate (314) fixedly connected to the inner top wall of an adjustment shell (366); a second electric telescopic rod (315) is fixedly connected to the inner wall of the adjustment shell (366); a conductive sheet (313) in sliding contact with the resistor plate (314) is fixedly connected to the telescopic end of the second electric telescopic rod (315); the resistor plate (314) and the conductive sheet (313) together form an adjustment loop; during the sliding process of the conductive sheet (313) on the resistor plate (314) away from the second electric telescopic rod (315), the resistance of the sliding rheostat in the adjustment loop gradually increases; and the PLC controller is electrically signal-connected to the second electric telescopic rod (315) and the first motor (361) to form a control loop.

5. The electrolytic fluorination equipment of trifluoromethylsulfonamide according to claim 3, characterized in that: The gas supply mixing mechanism (4) further comprises a gas storage box (44) fixedly connected to the outer wall of the preparation box (1), wherein fluorine gas is stored in the gas storage box (44), a second motor (45) is fixedly connected to the bottom end of the preparation box (1), an output end of the second motor (45) is fixedly connected to a second rotating plate (46), a top end of the second rotating plate (46) is fixedly connected to the exhaust pump (41), an output end of the exhaust pump (41) is fixedly connected to a connecting pipe (47), and the connecting pipe (47) is fixedly connected to the exhaust pump (41). The output end of the preparation box (7) 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 exhaust end of the exhaust pump (41) is fixedly connected to an air intake ring (410), the outer wall of the air intake ring (410) is rotatably connected to a connecting ring (411), the inner wall of the connecting ring (411) is fixedly connected to an exhaust pipe (412), the other end of the exhaust pipe (412) passes through the outer wall of the preparation box (1) and is connected to the interior of the air storage box (44).

6. The electrolytic fluorination equipment of trifluoromethylsulfonamide according to claim 5, characterized in that: It also includes a temperature control mechanism (49), the temperature control mechanism (49) also includes a cooling groove (491) opened inside the first rotating plate (42), the inner wall of the cooling groove (491) is provided with a refrigeration pipe (492), the top 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 connected to 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).

7. The electrolytic fluorination equipment of trifluoromethylsulfonamide according to claim 6, characterized in that: A semiconductor refrigeration plate (495) is embedded in the inner bottom wall of the preparation box (1), and the cooling end of the semiconductor refrigeration plate (495) faces the inside of the preparation box (1), and the heating end faces the bottom of the preparation box (1), and cooling water is poured between the preparation box (1) and the electrolytic cell (2), and the PLC controller is electrically connected to the exhaust pump (41) and the semiconductor refrigeration plate (495) to form a control loop.

8. The electrolytic fluorination equipment of trifluoromethylsulfonamide according to claim 4, characterized in that: The inner wall of the preparation box (1) is fixedly connected to a support plate (312), the top of the support plate (312) is fixedly connected to a preparation device (5), the preparation device (5) and the top of the preparation box (1) are provided with a discharge port (6), and a first sealing plug is provided in the discharge port (6), the bottom end of the support plate (312) is fixedly connected to a first material extraction pump (7), the extraction end of the first material extraction pump (7) is fixedly connected to a material extraction pipe (8) connected to the outlet of the preparation device (5), the discharge end of the first material extraction pump (7) is fixedly connected to a discharge pipe (9), and the other end of the discharge pipe (9) is located above the electrolytic cell (2), and the preparation box (1) 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 to a gas collector (11); the gas collector (11) and the preparation box (1) are fixedly connected to a gas outlet pipe (12); the outer wall of the preparation box (1) is fixedly connected to a collecting box (13); the outer wall of the preparation box (1) is fixedly connected to a second material extraction pump (14); the extraction end of the second material extraction pump (14) is connected to the inside of the electrolytic cell (2); the discharge end of the second material extraction pump (14) is connected to the collecting box (13); and the bottom end of the preparation box (1) is fixedly connected to a support frame (15).

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