Electrofluorination apparatus and method for producing perfluorobutylsulfonyl fluoride

Abstract

The application discloses an electrolytic fluorination reaction device and a method for producing perfluorobutylsulfonyl fluoride, which comprises an electrolytic tank and a feed buffer tank, an anode chamber and a cathode chamber are arranged in the electrolytic tank, the electrolytic tank comprises a separation plate for separating the anode chamber and the cathode chamber, a diaphragm is arranged on the separation plate, an anode plate is arranged on the anode chamber, a cathode plate is arranged on the cathode chamber, a feed pipe is arranged on the top of the feed buffer tank, a pipeline of an outlet end of the feed buffer tank is connected to the inside of the anode chamber, and an electrolyte circulating element is arranged on the electrolytic tank, so that the electrolyte in the cathode chamber is circulated back to the anode chamber through the electrolyte circulating element. The feed buffer tank is designed to meet the continuous small-flow input of fresh raw materials, the anode plate is arranged in a small-angle inclined mode in the anode chamber, and the special structure design of the plate surface groove and the scale-like convex is adopted to realize sufficient electrolytic fluorination reaction. The application has the advantages of high electrolytic fluorination efficiency, effective flushing and removal of tar by-products and the like.

Description

Technical Field

[0001] This invention relates to the field of chemical product production equipment technology, and more specifically, to an electrolytic fluorination reaction apparatus and a method for producing perfluorobutyl sulfonyl fluoride. Background Technology

[0002] The production of perfluorobutyl sulfonyl fluoride using electrochemical fluorination is a mainstream industrial method. However, current industrial applications suffer from a series of problems, such as low anodic reaction efficiency, high levels of byproduct tar, and easy residue buildup. Based on these practical production conditions, it is necessary to design a dedicated reaction equipment and method for the production of perfluorobutyl sulfonyl fluoride using electrochemical fluorination to meet production demands. Summary of the Invention

[0003] The purpose of this invention is to address the needs of the prior art by providing an electrolytic fluorination reaction apparatus and a method for producing perfluorobutyl sulfonyl fluoride. This invention features a feed buffer tank designed to accommodate a continuous, low-flow input of fresh raw materials. The anode plate is installed at a small angle in the anode chamber, and the special structural design of grooves and fish-scale protrusions on the plate surface enables a full electrolytic fluorination reaction. This invention has the advantages of high electrolytic fluorination efficiency and effective flushing and removal of tar byproducts.

[0004] To achieve the above objectives, the present invention adopts the following technical solution:

[0005] An electrolytic fluorination reactor includes an electrolytic cell and a feed buffer tank. The electrolytic cell has an anode chamber and a cathode chamber. The electrolytic cell includes a separation plate separating the anode chamber and the cathode chamber. A diaphragm is installed on the separation plate, allowing electrolyte to flow between the anode chamber and the cathode chamber. An anode plate is installed in the anode chamber, and a cathode plate is installed in the cathode chamber. A feed inlet is installed at the top of the feed buffer tank, and an outlet pipe of the feed buffer tank is connected to the interior of the anode chamber. A first exhaust pipe is connected to the top of the anode chamber, and a second exhaust pipe is connected to the top of the cathode chamber. An electrolyte circulation element is installed in the electrolytic cell to circulate the electrolyte from the cathode chamber back to the anode chamber.

[0006] Furthermore, the cathode plate is installed vertically in the cathode chamber, and the anode plate is installed at an angle in the anode chamber. The angle of the anode plate is set to 5-8 degrees. The lower end of the anode plate is installed at an angle close to the separation plate. The anode chamber and the cathode chamber are filled with electrolyte. The tops of the anode plate and the cathode plate are both above the highest electrolyte level.

[0007] Furthermore, the separation plate is vertically installed and fixed, and the diaphragm is installed at the bottom of the separation plate. The diaphragm is a porous PTFE diaphragm, and the diaphragm is set at the bottom of the anode plate and the cathode plate.

[0008] Furthermore, the feed buffer tank includes a first tank and a second tank. The first tank is vertically stacked and connected above the second tank. The first tank and the second tank are interconnected. The diameter of the first tank is smaller than that of the second tank. Two feed inlets are installed on the top of the first tank. A spiral plate is installed inside the first tank. A discharge pipe is connected to the bottom of the second tank. The discharge pipe extends into the anode chamber. The outlet end of the discharge pipe faces the top of the anode plate. A flow limiting plate is fixedly installed at the outlet end of the discharge pipe. The surface of the flow limiting plate is densely covered with several small through holes.

[0009] Furthermore, a first level gauge is installed on the top of the anode chamber, and a second level gauge is installed on the top of the cathode chamber. The first and second level gauges are radar level gauges, and the liquid level in the anode chamber is higher than the liquid level in the cathode chamber.

[0010] Furthermore, the electrolyte circulation element includes a circulation pump, a suction pipe, and a return pipe. The circulation pump is installed outside the cathode chamber. The suction pipe is connected to the inlet end of the circulation pump and extends into the electrolyte in the cathode chamber. The return pipe is connected to the outlet end of the circulation pump and extends into the anode chamber. The outlet end of the return pipe faces the top of the anode plate.

[0011] Furthermore, the anode plate has several parallel and concave grooves on its surface. These grooves extend vertically along the installation height of the anode plate. Between two adjacent grooves, several rows of fish-scale protrusions are formed on the plate surface. Adjacent rows of fish-scale protrusions are staggered. Each fish-scale protrusion includes a midpoint of an arc and a straight line segment. The midpoint of the arc is the highest protrusion height of the fish-scale protrusion. The straight line segment is flush with the surface of the anode plate, and the protrusion height gradually narrows from the midpoint of the arc towards the straight line segment.

[0012] Furthermore, it also includes a cooling circulation system, which includes a chiller unit, a condenser, a first cooling jacket, and a second cooling jacket. The condenser is integrated and installed on the first exhaust pipe. The first cooling jacket is installed on the outer side of the anode chamber, and the second cooling jacket is installed on the outer side of the cathode chamber. The chiller unit is connected to the condenser, the first cooling jacket, and the second cooling jacket in sequence via pipelines. The outlet pipeline of the second cooling jacket is connected back to the chiller unit.

[0013] Furthermore, the bottom of the anode chamber is sunken to form a conical section, and the bottom of the conical section is connected to a waste discharge pipe, which is equipped with a control valve.

[0014] A method for producing perfluorobutylsulfonyl fluoride, using an electrolytic fluorination reactor, includes the following steps:

[0015] S1: Pre-load the anode and cathode chambers with electrolyte;

[0016] S2: Start the electrolysis operation. The electrolyte in the cathode chamber is circulated and pumped out of the anode chamber through the electrolyte circulation element. Fresh raw materials and anhydrous hydrogen fluoride are added to the feed buffer tank. After the fresh raw materials and anhydrous hydrogen fluoride are mixed, fresh liquid is output. The fresh liquid and the electrolyte circulation return liquid converge at the top of the anode plate and wash the surface of the anode plate to complete the electrolytic fluorination reaction.

[0017] S3: The gas generated by the fluorination reaction contains the target component of perfluorobutyl sulfonyl fluoride. The gas is drawn out from the first exhaust pipe at the top of the anode chamber. The electrolyte in the anode chamber flows to the cathode chamber through the diaphragm. Under the electrolysis of the cathode plate, fluoride ions and hydrogen are decomposed. The hydrogen is drawn out separately through the second exhaust pipe of the cathode chamber. The fluorine-rich electrolyte formed in the cathode chamber is circulated and drawn out of the anode chamber through the electrolyte circulation element.

[0018] In summary, the present invention has the following beneficial effects:

[0019] This invention designs a feed buffer tank to meet the continuous low-flow input of fresh raw materials. The anode plate is installed at a small angle in the anode chamber, and the special structural design of the plate surface grooves and fish scale protrusions achieves a full electrolytic fluorination reaction. This invention has the advantages of high electrolytic fluorination efficiency and effective flushing and removal of tar by-products, and can well meet the industrial production needs of perfluorobutyl sulfonyl fluoride products. Attached Figure Description

[0020] Figure 1 This is a schematic diagram of the structure of an electrolytic fluorination reaction apparatus according to this embodiment;

[0021] Figure 2 This is a schematic diagram of the internal structure of the electrolytic cell in this embodiment;

[0022] Figure 3 This is a front view of the anode plate in this embodiment;

[0023] Figure 4 This is a schematic diagram of the internal structure of the feed buffer tank in this embodiment;

[0024] Figure 5 This is a schematic diagram of the outlet position structure of the discharge pipe in this embodiment;

[0025] Figure 6 This is a schematic diagram of the connection principle of the cooling circulation system in this embodiment.

[0026] Figure label:

[0027] Electrolytic cell 1, anode chamber 11, first exhaust pipe 111, first level gauge 112, conical section 113, waste discharge pipe 114, control valve 115, cathode chamber 12, second exhaust pipe 121, second level gauge 122, separation plate 13, diaphragm 14, anode plate 2, groove 21, fish scale protrusion 22, arc midpoint 221, straight section 222, cathode plate 3, feed buffer tank 4, first tank body 41, feed inlet 411, spiral plate 412, second tank body 42, discharge pipe 421, flow limiting plate 422, small through hole 423, third level gauge 43, electrolyte circulation element 5, circulation pump 51, liquid extraction pipe 52, return pipe 53, cooling circulation system 6, chiller unit 61, condenser 62, first cooling jacket 63, second cooling jacket 64. Detailed Implementation

[0028] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0029] like Figures 1 to 6As shown, this embodiment discloses an electrolytic fluorination reaction apparatus, including an electrolytic cell 1 and a feed buffer tank 4. The electrolytic cell 1 has an anode chamber 11 and a cathode chamber 12, which are separated by a separation plate 13 installed within the electrolytic cell 1. The anode chamber 11 and cathode chamber 12 are filled with an electrolyte (mainly composed of anhydrous HF). To facilitate electrolyte flow, a diaphragm 14 is installed on the separation plate 13. The diaphragm 14 is installed between the electrolyte in the anode chamber 11 and cathode chamber 12. Below this level, the diaphragm 14 is a porous PTFE (polytetrafluoroethylene) diaphragm. The diaphragm 14 has a microporous structure, allowing the electrolyte to flow but blocking the passage of gases generated by the reactions in the anode chamber 11 and cathode chamber 12 (the anode chamber 11 produces a gas mainly composed of perfluorobutyl sulfonyl fluoride, and the cathode chamber 12 produces hydrogen). The diaphragm 14 allows electrolyte flow between the anode chamber 11 and cathode chamber 12. In this invention, the liquid level in the anode chamber 11 is designed to be higher than the liquid level in the cathode chamber 12. Under hydrostatic pressure, the anode chamber 11... The electrolyte flows naturally into the cathode chamber 12. An anode plate 2 is installed in the anode chamber 11, and a cathode plate 3 is installed in the cathode chamber 12. The anode plate 2 and cathode plate 3, in a conductive state, meet the requirements for electrolytic fluorination production. The raw material input of this invention is achieved through a feed buffer tank 4. The top of the feed buffer tank 4 is equipped with a feed inlet 411 (two types of raw materials are input, fed through two separate feed inlets 411). The outlet pipe of the feed buffer tank 4 is connected to the interior of the anode chamber 11. The feed buffer tank 4 serves as a buffer and mixing tank for the input of raw materials. The mixed raw materials are input into the anode chamber 11 and flow onto the energized anode plate 2 to carry out the electrolytic fluorination reaction, thereby obtaining perfluorobutylsulfonyl fluoride. The perfluorobutylsulfonyl fluoride product is a gas. This invention has a first exhaust pipe 111 connected to the top of the anode chamber 11. The first exhaust pipe 111 creates a negative pressure suction effect to carry out the gaseous perfluorobutylsulfonyl fluoride product. The cathode chamber 12, through the conductive cathode plate 3, achieves the effect of electrolytic separation of fluoride ions (reaction formula: 2HF + 2e). - = H2 + 2F -During this process, hydrogen gas is also produced as a byproduct. A second exhaust pipe 121 is connected to the top of the cathode chamber 12. The second exhaust pipe 121 creates a negative pressure suction effect to remove the hydrogen gas. Since there is a safety risk (explosion risk) when hydrogen gas mixes with the perfluorobutylsulfonyl fluoride product gas, the anode chamber 11 and the cathode chamber 12 are gas-isolated from each other, and the generated gases are extracted separately (the separation plate 13 physically separates them, and the diaphragm 14 is below the liquid surface and forms a gas barrier through a special material). The electrolytic fluorination reaction of the anode plate 2 consumes fluoride ions in the electrolyte to generate the perfluorobutylsulfonyl fluoride product. Therefore, the fluoride content of the electrolyte in the anode chamber 11 decreases. The ionization effect of the cathode plate 3 is to separate and produce fluoride ions. Thus, the cathode chamber 12 is a fluoride-rich electrolyte. The electrolyte in the cathode chamber 12 is drawn into the anode chamber 11 to replenish the fluoride ions. For this purpose, the present invention is equipped with an electrolyte circulation element 5 for the electrolytic cell 1. The electrolyte circulation element 5 is used to circulate the electrolyte in the cathode chamber 12 back to the anode chamber 11 to replenish the fluoride ions required for the electrolytic fluorination reaction. Under the above design, the present invention forms a closed loop of electrolytic fluorination reaction, which can continuously produce perfluorobutyl sulfonyl fluoride gas products.

[0030] like Figure 4 As shown, the feed buffer tank 4 of the present invention includes a first tank body 41 and a second tank body 42. The first tank body 41 is vertically erected and stacked on top of the second tank body 42. The first tank body 41 and the second tank body 42 are interconnected. Two feed ports 411 are installed on the top of the first tank body 41 for feeding the raw material butyl sulfonyl fluoride and the solvent anhydrous HF (hydrogen fluoride), respectively. A spiral plate 412 is installed inside the first tank body 41. The spiral plate 412 is located below the feed ports 411 and forms a spiral liquid guiding path. The butyl sulfonyl fluoride and the solvent anhydrous HF fall under the guidance of the spiral plate 412 and form a premixing effect. The spiral plate 412 forms a spiral liquid guiding path. The swirling mixing effect allows butyl sulfonyl fluoride and anhydrous HF solvent to be premixed without stirring. The diameter of the first tank 41 is smaller than that of the second tank 42, which forms an expansion chamber. The premixed raw material liquid is collected in the second tank 42, which stabilizes the output flow rate and buffers the feed pressure. A discharge pipe 421 is connected to the bottom of the second tank 42, extending into the anode chamber 11. The discharge pipe 421 is used to output fresh raw material liquid, with its outlet facing the top of the anode plate 2, creating a top-down liquid flow scouring effect on the anode plate 2. Figure 5As shown, a flow limiting plate 422 is fixedly installed at the outlet end of the discharge pipe 421. The surface of the flow limiting plate 422 is densely covered with several small through holes 423, which are used to output fresh raw material liquid. The flow limiting plate 422 restricts the output flow rate. The fresh raw material is pre-stored in the second tank 42. Under the action of the flow limiting plate 422, the output flow rate of the discharge pipe 421 is small, stable and continuous, achieving the effect of continuous flushing of the anode plate 2 with a small flow rate, thereby stably and efficiently producing perfluorobutyl sulfonyl fluoride gas product. In this invention, a third liquid level gauge 43 is installed on the top of the second tank 42. The third liquid level gauge 43 is a radar liquid level gauge, which monitors the liquid level of the second tank 42 without contact, ensuring that the output of fresh raw material liquid is continuous. A valve is installed on the discharge pipe 421, and the valve needs to be open during production.

[0031] The three cathode plates ionize and release fluoride ions and hydrogen gas, but have no other special function. Therefore, as... Figure 2 As shown, the cathode plate 3 is vertically installed in the cathode chamber 12, while the electrolytic fluorination reaction of the anode plate 2 requires continuous flushing of the feed liquid to meet production needs. Therefore, this invention designs the anode plate 2 to be installed at an angle of 5-8 degrees in the anode chamber 11, with the lower end of the anode plate 2 close to the separation plate 13. The inclined installation method of the anode plate 2 adapts to the electrolyte flow direction, forming an efficient path scheme that drives the feed liquid to flush the high-efficiency anode plate 2. In this invention, the separation plate 13 is vertically installed and fixed, and the diaphragm 14 is installed at the bottom of the separation plate 13. The diaphragm 14 is set at the bottom of the anode plate 2 and the cathode plate 3. Since the diaphragm 14 is installed at a low position, a top-to-bottom electrolyte fluid path is naturally formed in the anode chamber 11, which is exactly... The raw material liquid is carried downward along the inclined high-efficiency anode plate 2 to fully and efficiently produce perfluorobutyl sulfonyl fluoride gas products. In this invention, the tops of both the anode plate 2 and the cathode plate 3 extend beyond the highest liquid level of the electrolyte. The extended portions of the anode plate 2 and the cathode plate 3 can guide the gas generated by the reaction to float upward and be discharged, so that the generated gas is not trapped in the electrolyte. In this invention, a first liquid level gauge 112 is installed on the top of the anode chamber 11, and a second liquid level gauge 122 is installed on the top of the cathode chamber 12. The first liquid level gauge 112 and the second liquid level gauge 122 are radar liquid level gauges, forming a non-contact liquid level monitoring. In this invention, the liquid level of the anode chamber 11 needs to be designed to be higher than that of the cathode chamber 12, so that under the action of static pressure, the electrolyte in the anode chamber 11 naturally flows to the cathode chamber 12.

[0032] The fluoride ions consumed in the production of perfluorobutyl sulfonyl fluoride gas in the anode chamber 11 need to be replenished through the cathode chamber 12. This replenishment is achieved using the electrolyte circulation element 5. Figure 1 and Figure 2As shown, the electrolyte circulation element 5 includes a circulation pump 51, a suction pipe 52, and a return pipe 53. The circulation pump 51 is installed outside the cathode chamber 12. The suction pipe 52 is connected to the inlet end of the circulation pump 51 and extends into the electrolyte in the cathode chamber 12. The circulation pump 51 generates a reflux suction force, and the suction pipe 52 draws the fluorine-rich electrolyte from the cathode chamber 12. The return pipe 53 is connected to the outlet end of the circulation pump 51 and extends into the anode chamber 11. The outlet end faces the top of the anode plate 2. The reflux pipe 53 refluxes the fluorine-rich electrolyte from the cathode chamber 12. The reflux liquid and the fresh raw material liquid converge at the top of the anode plate 2 and together flush the surface of the anode plate 2 to replenish the fluoride ions required for the electrolytic fluorination reaction. Since the fresh raw material liquid is input at a small flow rate, the flow rate of the reflux liquid is designed to be greater than that of the fresh raw material liquid. After the two converge, the fresh raw material liquid can be carried down by the fluorine-rich reflux liquid, thereby improving the effect of the fresh raw material liquid flushing the anode plate 2.

[0033] During the electrolytic fluorination reaction, anode plate 2 forms heavy byproducts, primarily tar. Tar buildup on the plate causes a series of problems, including reduced current efficiency, current imbalance, accelerated electrode corrosion, and shortened electrode life. This invention first addresses this by installing anode plate 2 at an inclined angle to accelerate electrolyte flushing, thereby reducing the probability of tar buildup. Figure 3 As shown, the present invention also provides several parallel and concave grooves 21 on the surface of the anode plate 2. The grooves 21 extend vertically along the installation height of the anode plate 2. The electrolyte flow rate is fastest at the location of the grooves 21, which is beneficial for quickly flushing away the tar byproducts. Several rows of fish-scale protrusions 22 are formed on the surface between two adjacent grooves 21. The two adjacent rows of fish-scale protrusions 22 are staggered. Each fish-scale protrusion 22 includes a midpoint 221 of an arc and a straight segment 222. The fish-scale protrusions 22 are all set with the midpoint 221 of the arc facing upwards. The midpoint 221 of the arc is the highest protrusion height of the fish-scale protrusion 22. The straight segment 222 is flush with the surface of the anode plate 2 and extends from the midpoint 221 of the arc towards the straight segment 222. The line segment 222 gradually narrows towards the height of the protrusion. The midpoint 221 of the arc of the fish-scale protrusion 22 faces the direction of electrolyte flow. The fish-scale protrusion 22 can divert the electrolyte. Through the continuous diversion of the electrolyte by the densely distributed fish-scale protrusions 22, the electrolyte has sufficient time and stroke to contact the surface of the anode plate 2 during the diversion process, thereby improving the efficiency of the electrolytic fluorination reaction and the product yield. At the same time, the arc segment of the fish-scale protrusion 22 can also cause the by-product tar to be flushed off without forming a plate-hanging phenomenon. The staggered and dense distribution of the fish-scale protrusions 22 can also create chaotic turbulence in the area where the fish-scale protrusions 22 are set. The turbulence can stir up the by-product tar, which helps it to be flushed off the groove 21. Figure 2As shown, in this invention, a conical section 113 is formed at the bottom of the anode chamber 11. Tar and other heavy component by-products are washed off the anode plate 2 and naturally sink to the bottom of the conical section 113 to collect. The bottom of the conical section 113 is connected to a waste discharge pipe 114. A control valve 115 is installed on the waste discharge pipe 114. The control valve 115 is normally closed. After the equipment has worked a fixed shift, the control valve 115 is opened to discharge the heavy component waste (which is placed in a safety container).

[0034] The electrolytic fluorination reaction of this invention requires a cooling environment; therefore, this invention also includes a cooling circulation system 6. The cooling circulation system 6 includes a chiller unit 61, a condenser 62, a first cooling jacket 63, and a second cooling jacket 64. The chiller unit 61 is used to circulate cooling water. The condenser 62 is integrated into the first exhaust pipe 111. The first exhaust pipe 111 uses negative pressure to exhaust the gas generated in the anode chamber 11. The gas generated in the anode chamber 11 is mainly perfluorobutyl sulfonyl fluoride product gas, and also includes some evaporated HF gas. The condenser 62 is used to process the HF gas. The condensation of the gas causes HF gas to condense into liquid HF, which then flows back to the anode chamber 11 for use. Perfluorobutyl sulfonyl fluoride gas undergoes a series of processes including washing, drying, and purification to obtain the finished product. The first cooling jacket 63 is installed on the outside of the anode chamber 11 to provide a reaction cooling environment. The second cooling jacket 64 is installed on the outside of the cathode chamber 12 to provide a reaction cooling environment. In this invention, the required condensation temperature for the condenser 62 is -15 to -10°C, the cooling temperature for the anode chamber 11 is -10 to 0°C, and the required condensation temperature for the cathode chamber 12 is 0 to 5°C, thus meeting the continuous temperature requirements. Therefore, this invention designs a chiller unit 61 with sequential piping connecting the condenser 62, the first cooling jacket 63, and the second cooling jacket 64. The temperature difference is used to rationally arrange the cooling water flow, satisfying all production needs in a single cycle. The outlet pipe of the second cooling jacket 64 is connected back to the chiller unit 61 to complete the closed-loop flow.

[0035] A method for producing perfluorobutylsulfonyl fluoride, using an electrolytic fluorination reactor, includes the following steps:

[0036] S1: Pre-load the anode chamber 11 and cathode chamber 12 with electrolyte (the anode chamber 11 and cathode chamber 12 are designed with pre-filled liquid inlets), and the liquid level in the anode chamber 11 is preset to be higher than the liquid level in the cathode chamber 12;

[0037] S2: Start the electrolysis operation. The electrolyte in the cathode chamber 12 is circulated and pumped out of the anode chamber 11 through the electrolyte circulation element 5. Fresh raw materials and anhydrous hydrogen fluoride are added to the feed buffer tank 4. After the fresh raw materials and anhydrous hydrogen fluoride are mixed, fresh liquid is output. The fresh liquid is continuously output at a small flow rate. The fresh liquid and the electrolyte circulation return liquid converge at the top of the anode plate 2 and flush the surface of the anode plate 2 to complete the electrolytic fluorination reaction. The return liquid replenishes the fluoride ions required for the reaction.

[0038] S3: The gas generated by the fluorination reaction contains the target component of perfluorobutyl sulfonyl fluoride. The gas is extracted and discharged from the first exhaust pipe 111 at the top of the anode chamber 11. The electrolyte in the anode chamber 11 flows to the cathode chamber 12 through the diaphragm 14. Under the electrolysis of the cathode plate 3, fluoride ions and hydrogen are decomposed. The hydrogen is extracted and discharged separately through the second exhaust pipe 121 of the cathode chamber 12. The fluorine-rich electrolyte formed in the cathode chamber 12 is circulated and pumped out of the anode chamber 11 through the electrolyte circulation element 5.

[0039] The electrolytic fluorination production of perfluorobutyl sulfonyl fluoride products continues with the ongoing operation of steps S2 and S3.

[0040] The above description is merely a preferred embodiment of the present invention. The scope of protection of the present invention is not limited to the above embodiments. All technical solutions falling within the scope of the present invention's concept are within the scope of protection of the present invention. It should be noted that for those skilled in the art, any improvements and modifications made without departing from the principles of the present invention should also be considered within the scope of protection of the present invention.

Claims

1. An electrolytic fluorination reaction apparatus, characterized in that, The system includes an electrolytic cell (1) and a feed buffer tank (4). The electrolytic cell (1) has an anode chamber (11) and a cathode chamber (12). The electrolytic cell (1) includes a separation plate (13) separating the anode chamber (11) and the cathode chamber (12). A diaphragm (14) is installed on the separation plate (13) to allow electrolyte to flow between the anode chamber (11) and the cathode chamber (12). An anode plate (2) is installed in the anode chamber (11), and a cathode plate is installed in the cathode chamber (12). (3) The feed buffer tank (4) is equipped with a feed inlet (411) at the top. The outlet pipe of the feed buffer tank (4) is connected to the inside of the anode chamber (11). The top of the anode chamber (11) is connected to a first exhaust pipe (111). The top of the cathode chamber (12) is connected to a second exhaust pipe (121). The electrolytic cell (1) is equipped with an electrolyte circulation element (5). The electrolyte circulation element (5) allows the electrolyte in the cathode chamber (12) to circulate back to the anode chamber (11).

2. The electrolytic fluorination reaction apparatus according to claim 1, characterized in that, The cathode plate (3) is installed vertically in the cathode chamber (12), and the anode plate (2) is installed at an angle in the anode chamber (11). The angle of the anode plate (2) is set to 5-8 degrees. The lower end of the anode plate (2) is installed at an angle close to the separation plate (13). The anode chamber (11) and the cathode chamber (12) are filled with electrolyte. The tops of the anode plate (2) and the cathode plate (3) are both above the highest liquid level of the electrolyte.

3. The electrolytic fluorination reaction apparatus according to claim 1, characterized in that, The separation plate (13) is installed vertically and fixedly. The diaphragm (14) is installed at the bottom of the separation plate (13). The diaphragm (14) is a porous PTFE diaphragm. The diaphragm (14) is set at the bottom of the anode plate (2) and the cathode plate (3).

4. The electrolytic fluorination reaction apparatus according to claim 1, characterized in that, The feed buffer tank (4) includes a first tank body (41) and a second tank body (42). The first tank body (41) is vertical and stacked on top of the second tank body (42). The first tank body (41) and the second tank body (42) are interconnected. The diameter of the first tank body (41) is smaller than that of the second tank body (42). Two feed inlets (411) are installed on the top of the first tank body (41). A spiral plate (412) is installed inside the first tank body (41). A discharge pipe (421) is connected to the bottom of the second tank body (42). The discharge pipe (421) extends into the anode chamber (11). The outlet end of the discharge pipe (421) faces the top of the anode plate (2). A flow limiting plate (422) is fixedly installed at the outlet end of the discharge pipe (421). The surface of the flow limiting plate (422) is densely covered with several small through holes (423).

5. The electrolytic fluorination reaction apparatus according to claim 1, characterized in that, A first level gauge (112) is installed on the top of the anode chamber (11), and a second level gauge (122) is installed on the top of the cathode chamber (12). The first level gauge (112) and the second level gauge (122) are radar level gauges. The liquid level in the anode chamber (11) is higher than the liquid level in the cathode chamber (12).

6. The electrolytic fluorination reaction apparatus according to claim 1, characterized in that, The electrolyte circulation element (5) includes a circulation pump (51), a suction pipe (52), and a return pipe (53). The circulation pump (51) is installed outside the cathode chamber (12). The suction pipe (52) is connected to the inlet end of the circulation pump (51) and extends into the electrolyte in the cathode chamber (12). The return pipe (53) is connected to the outlet end of the circulation pump (51) and extends into the anode chamber (11). The outlet end of the return pipe (53) faces the top of the anode plate (2).

7. The electrolytic fluorination reaction apparatus according to claim 1, characterized in that, The anode plate (2) has several parallel grooves (21) that are all concave. The grooves (21) run vertically along the installation height of the anode plate (2). Several rows of fish scale protrusions (22) are formed on the plate surface between two adjacent grooves (21). The two adjacent rows of fish scale protrusions (22) are staggered. The fish scale protrusions (22) include the midpoint of the arc (221) and the straight line segment (222). The fish scale protrusions (22) are all set with the midpoint of the arc (221) facing upwards. The midpoint of the arc (221) is the highest protrusion height of the fish scale protrusions (22). The straight line segment (222) is flush with the plate surface of the anode plate (2). The protrusion height gradually narrows from the midpoint of the arc (221) towards the straight line segment (222).

8. The electrolytic fluorination reaction apparatus according to claim 1, characterized in that, It also includes a cooling circulation system (6), which includes a chiller (61), a condenser (62), a first cooling jacket (63) and a second cooling jacket (64). The condenser (62) is integrated into the first exhaust pipe (111). The first cooling jacket (63) is installed on the outside of the anode chamber (11). The second cooling jacket (64) is installed on the outside of the cathode chamber (12). The chiller (61) is connected to the condenser (62), the first cooling jacket (63) and the second cooling jacket (64) in sequence. The outlet pipe of the second cooling jacket (64) is connected back to the chiller (61).

9. The electrolytic fluorination reaction apparatus according to claim 1, characterized in that, The bottom of the anode chamber (11) sinks to form a conical section (113), and the bottom of the conical section (113) is connected to a waste discharge pipe (114), and a control valve (115) is installed on the waste discharge pipe (114).

10. A method for producing perfluorobutylsulfonyl fluoride, implemented using an electrolytic fluorination apparatus as described in any one of claims 1-9, characterized in that, Includes the following steps: S1: Pre-load the anode chamber (11) and cathode chamber (12) with electrolyte; S2: Start the electrolysis operation. The electrolyte in the cathode chamber (12) is circulated and pumped out of the anode chamber (11) through the electrolyte circulation element (5). Fresh raw materials and anhydrous hydrogen fluoride are added to the feed buffer tank (4). After the fresh raw materials and anhydrous hydrogen fluoride are mixed, fresh liquid is output. The fresh liquid and the electrolyte circulation return liquid converge at the top of the anode plate (2) and flush the surface of the anode plate (2) to complete the electrolytic fluorination reaction. S3: The gas generated by the fluorination reaction contains the target component of perfluorobutyl sulfonyl fluoride. The gas is extracted and discharged from the first exhaust pipe (111) at the top of the anode chamber (11). The electrolyte in the anode chamber (11) flows to the cathode chamber (12) through the diaphragm (14). Under the electrolysis of the cathode plate (3), fluoride ions and hydrogen are decomposed. The hydrogen is extracted separately through the second exhaust pipe (121) of the cathode chamber (12). The fluorine-rich electrolyte formed in the cathode chamber (12) is circulated and pumped out of the anode chamber (11) through the electrolyte circulation element (5).

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