An electrolytic cell for preparing perfluorobutyryl fluoride gas

Abstract

The present invention discloses an electrolytic cell for preparing perfluorobutyryl fluoride gas, which belongs to the technical field of perfluorobutyryl fluoride gas preparation, and comprises a cell body, wherein a cover plate which is slidably sealed with the inner wall of the cell body is arranged inside the cell body, an electric push rod is installed on the outer side of the cover plate, and the top end of the electric push rod is installed to the inner top wall of the cell body, an exhaust pipe is installed on the cover plate, a collection component is arranged on the outer side of the exhaust pipe, and a delivery pump is arranged on the outer side of the cell body, and the output end and input end of the delivery pump are fixedly connected with a fixed pipe. The invention can pre-mix the input materials to improve the subsequent mixing effect and work efficiency, and before the gas collection process, the excess gas in the electrolytic cell can be discharged to ensure the concentration of the gas generated by electrolysis after collection. After use, it is convenient to process the precipitation inside the electrolytic cell to improve the cleaning effect and facilitate the next use.

Description

Technical Field

[0001] The invention relates to the technical field of perfluorobutyryl fluoride gas preparation, and more specifically to an electrolytic cell for preparing perfluorobutyryl fluoride gas. Background Art

[0002] The electrolytic cell is mainly used for industrial production of high-purity metals. It is a device that converts electrical energy into chemical energy (composed of: external power supply, electrolyte solution, positive and negative electrodes). The current passes through the electrolyte solution or molten electrolyte to cause reduction and oxidation reactions at the positive and negative electrodes. In the process of preparing perfluorobutyryl fluoride gas, anhydrous hydrogen fluoride and n-butyryl fluoride need to be electrolytically reacted through the electrolytic cell to obtain perfluorobutyryl fluoride gas. After the collection is completed, the perfluorobutyryl fluoride is introduced into the hydrolysis tower kettle, the temperature in the kettle is maintained at 50-55°C, and it is absorbed with a 50% potassium hydroxide aqueous solution. When the pH value reaches 6-7, Stop introducing perfluorobutyryl fluoride gas, keep warm at 50-55°C for two hours, cool to 20-25°C, filter, transfer the filtrate into a distillation kettle for distillation, add ethyl acetate to recrystallize the mother liquor after it crystallizes, filter to obtain a wet product, recover ethyl acetate from the mother liquor, dry the wet product to obtain an intermediate potassium perfluorobutyrate, add the obtained potassium perfluorobutyrate and concentrated sulfuric acid into a reactor at room temperature, stir to dissolve, heat to 100°C, distill under slightly reduced pressure to collect the intermediate perfluorobutyric acid, add perfluorobutyric acid, concentrated sulfuric acid and methanol into a reactor, heat to 60°C, keep warm for 9-10 hours, and collect the fractions by atmospheric distillation to obtain perfluorobutyryl fluoride gas.

[0003] The existing electrolytic cells have the following defects during use:

[0004] 1. When collecting the gas generated by electrolysis, it is inevitable that air and bubbles inside the electrolyte will enter, which may affect the concentration of the collected gas;

[0005] 2. It does not have the function of pre-mixing materials, and the materials need to be mixed after being put in, which affects the work efficiency;

[0006] 3. The internal part of the electrolytic cell is cleaned by flushing and manual scrubbing, which is not convenient for handling sediments, and the cleaning effect is average, which may easily affect the next use. Summary of the invention

[0007] In view of the problems existing in the prior art, the object of the present invention is to provide an electrolytic cell for preparing perfluorobutyryl fluoride gas to overcome the defects of the background technology.

[0008] To solve the above problems, the present invention adopts the following technical solutions.

[0009] An electrolytic cell for preparing perfluorobutyryl fluoride gas comprises a cell body, wherein a cover plate which is slidably sealed with the inner wall of the cell body is arranged inside the cell body, an electric push rod is installed on the outer side of the cover plate, the top end of the electric push rod is installed to the inner top wall of the cell body, an exhaust pipe is installed on the cover plate, a collection component is arranged on the outer side of the exhaust pipe, a delivery pump is arranged on the outer side of the cell body, the output end and the input end of the delivery pump are both fixedly connected with fixed pipes, the ends of the two fixed pipes away from the delivery pump are respectively penetrated and fixedly connected to the left and right sides of the cell body, the two fixed pipes are both installed with a feed pipe, the interiors of the two fixed pipes are both rotatably connected with a rotating shaft, the top end of the rotating shaft is penetrated and rotated A stirring blade at the bottom end of the feed pipe is dynamically connected, a transmission mechanism is arranged between the two rotating shafts, a connecting shaft is installed on the transmission mechanism, the bottom end of the connecting shaft passes through and is fixedly connected with a scraper in contact with the bottom wall of the pool body, an air guide component is arranged inside the pool body, a group of annular cavities are opened inside the pool body, a group of conduits are installed inside the pool body, two adjacent annular cavities are connected through the conduits therebetween, the right end of the conduit on the right side passes through and is fixedly connected to the outside of the pool body, a group of vibration rods are installed on the inner bottom wall of the pool body, the top end of the vibration rods extends to the inside of the scraper, and the inside of the annular cavity is rotatably connected with a striking fan in contact with the outside of the vibration rod.

[0010] As a further description of the above technical solution:

[0011] The collection component includes a docking joint, a collection tube, two connecting tubes, a piston disk and a solenoid valve. The opposite ends of the two connecting tubes pass through and are fixedly connected to the interior of the collection tube. The connecting tube at the bottom is connected to the exhaust pipe through a docking joint fixedly installed on the outside. The outer side of the piston disk is slidably connected to the interior of the collection tube. The solenoid valve is installed on the bottom connecting tube.

[0012] As a further description of the above technical solution:

[0013] A metal ring is embedded on the outer side of the piston disc, and a magnetic ring is sleeved on the outer side of the collection tube.

[0014] As a further description of the above technical solution:

[0015] The transmission mechanism comprises a synchronous belt and three synchronous wheels. The three synchronous wheels are respectively mounted on two rotating shafts and a connecting shaft. The synchronous belt is mounted on the outer sides of the three synchronous wheels.

[0016] As a further description of the above technical solution:

[0017] A guide plate is arranged on the outer side of the rotating shaft on the right side, and one side of the guide plate is installed in a fixed pipe located on the right side of the pool body.

[0018] As a further description of the above technical solution:

[0019] A group of baffles are slidably mounted inside the scraper, and arc portions are arranged at the bottoms of the front and back sides of the baffles, and the top end of the vibration rod contacts the bottom of the baffles.

[0020] As a further description of the above technical solution:

[0021] The left and right sides of the baffle are both fixedly connected with counterweight blocks, and the outer side of the counterweight block is slidably connected to the inside of the scraper.

[0022] As a further description of the above technical solution:

[0023] The air guide assembly includes an N-shaped rod, a piston plate and an air pipe, both ends of the N-shaped rod penetrate and are slidably connected to the interior of the pool body, one end of the N-shaped rod is fixedly connected to the top of the cover plate, and the other end of the N-shaped rod is fixedly connected to the top of the piston plate. An air cavity is opened on the left side of the interior of the pool body, and the outer side of the piston plate is slidably connected to the interior of the air cavity. The air pipe is embedded in the interior of the pool body, the top end of the air pipe is connected to the air cavity, and the right end of the air pipe is connected to the left annular cavity.

[0024] As a further description of the above technical solution:

[0025] A control panel is installed on the front side of the pool body.

[0026] As a further description of the above technical solution:

[0027] Discharge pipes are installed on the right side of the pool body and the outer fixed pipe, and valves are installed on the two discharge pipes and the feed pipe.

[0028] Compared with the prior art, the advantages of the present invention are:

[0029] (1) This solution uses a stirring blade to break up the introduced materials at intervals, and then uses a circulating electrolyte to perform pre-mixing. It is then combined with a scraper inside the cell body for secondary mixing to improve the mixing effect and work efficiency.

[0030] (2) This solution uses the extrusion exhaust of the scraper and the vibration exhaust of the vibration rod to reduce the gas content inside the pool body, thereby improving the concentration of the collected reaction gas.

[0031] (3) This solution uses a vibration rod to separate the sediment from the pool body, and uses a scraper to scrape off the sediment to improve the cleaning effect of the pool body. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 It is a structural schematic diagram of the present invention;

[0033] Figure 2 It is a front cross-sectional schematic diagram of the structure of the present invention;

[0034] Figure 3 The structure of the present invention Figure 2 A is an enlarged schematic diagram;

[0035] Figure 4 The structure of the present invention Figure 2 A magnified schematic diagram of B;

[0036] Figure 5 The structure of the present invention Figure 2 A magnified schematic diagram of middle C;

[0037] Figure 6 It is a bottom-up stereoscopic schematic diagram of the striking fan structure of the present invention;

[0038] Figure 7 The structure of the present invention Figure 2 A magnified schematic diagram of D in the middle;

[0039] Figure 8 It is a bottom-up cross-sectional schematic diagram of the rotating shaft and stirring blade structure of the present invention;

[0040] Fig. 9 It is a side perspective schematic diagram of the baffle structure of the present invention.

[0041] Description of the numbers in the figure:

[0042] 1. Pool body; 2. Cover plate; 3. Electric push rod; 4. Exhaust pipe; 5. Collection component; 51. Docking joint; 52. Collection pipe; 53. Connecting pipe; 54. Piston plate; 55. Solenoid valve; 6. Delivery pump; 7. Fixed pipe; 8. Air guide component; 81. N-shaped rod; 82. Piston plate; 83. Air pipe; 9. Transmission mechanism; 91. Synchronous belt; 92. Synchronous wheel; 10. Discharge pipe; 11. Rotating shaft; 12. Stirring blade; 13. Feed pipe; 14. Annular cavity; 15. Conduit; 16. Vibrating rod; 17. Beating fan; 18. Metal ring; 19. Magnetic ring; 20. Connecting shaft; 21. Scraper; 22. Guide plate; 23. Baffle; 24. Counterweight; 25. Air cavity. DETAILED DESCRIPTION

[0043] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the accompanying drawings in the embodiments of the present invention;

[0044] See also Figure 1-9, an electrolytic cell for preparing perfluorobutyryl fluoride gas, comprising a cell body 1, a cover plate 2 which is slidably sealed with the inner wall of the cell body 1 is arranged inside the cell body 1, an electric push rod 3 is installed on the outer side of the cover plate 2, the top of the electric push rod 3 is installed to the inner top wall of the cell body 1, an exhaust pipe 4 is installed on the cover plate 2, a collection component 5 is arranged on the outer side of the exhaust pipe 4, a delivery pump 6 is arranged on the outer side of the cell body 1, the output end and the input end of the delivery pump 6 are fixedly connected with fixed pipes 7, the ends of the two fixed pipes 7 away from the delivery pump 6 are respectively penetrated and fixedly connected to the left and right sides of the cell body 1, a feed pipe 13 is installed on the two fixed pipes 7, the interiors of the two fixed pipes 7 are rotatably connected with a rotating shaft 11, the top of the rotating shaft 11 is penetrated and rotatably connected with a feed pipe 13 in the feed pipe 13, A stirring blade 12 is provided at the bottom end of the tube 13, and a transmission mechanism 9 is arranged between the two rotating shafts 11, and a connecting shaft 20 is installed on the transmission mechanism 9. The bottom end of the connecting shaft 20 passes through and is fixedly connected with a scraper 21 in contact with the inner bottom wall of the pool body 1, and an air guide component 8 is arranged inside the pool body 1. A group of annular cavities 14 are opened inside the pool body 1, and a group of conduits 15 are installed inside the pool body 1. Two adjacent annular cavities 14 are connected through the conduits 15 therebetween, and the right end of the right conduit 15 passes through and is fixedly connected to the outside of the pool body 1, and a group of vibration rods 16 are installed on the inner bottom wall of the pool body 1, and the top end of the vibration rod 16 extends to the inside of the scraper 21, and the inside of the annular cavity 14 is rotatably connected with a striking fan 17 in contact with the outside of the vibration rod 16.

[0045] The air guide assembly 8 includes an N-shaped rod 81, a piston plate 82 and an air pipe 83. Both ends of the N-shaped rod 81 pass through and are slidably connected to the interior of the pool body 1. One end of the N-shaped rod 81 is fixedly connected to the top of the cover plate 2, and the other end of the N-shaped rod 81 is fixedly connected to the top of the piston plate 82. An air cavity 25 is opened on the left side of the interior of the pool body 1. The outer side of the piston plate 82 is slidably connected to the interior of the air cavity 25. The air pipe 83 is embedded in the interior of the pool body 1. The top end of the air pipe 83 is connected to the air cavity 25, and the right end of the air pipe 83 is connected to the left annular cavity 14.

[0046] The cell body 1 plays a supporting role for the entire device. Before the electrolysis operation is performed, the user can start the delivery pump 6 to allow the electrolyte to circulate along the two fixed tubes 7. During the flow, anhydrous hydrogen fluoride and n-butyryl fluoride are introduced along the two feed tubes 13 respectively. During the introduction process, the flowing electrolyte will drive the stirring blade 12 on the rotating shaft 11 to rotate, so that the material is put into the fixed tube 7 at intervals, which is more dispersed. In the process of being introduced into the interior of the cell body 1 by the fixed tube 7, the electrolyte is pre-mixed. At the same time, after the rotating shaft 11 rotates, the transmission mechanism 9 will drive the connecting shaft 20 to rotate, so that the scraper 21 rotates accordingly, and the material inside the cell body 1 is mixed and stirred with the electrolyte. Then, after the material mixing is completed, the user can start the electric push rod 3 to push the cover plate 2 to move downward until the bottom of the cover plate 2 contacts the electrolyte level. During this process, the gas between the electrolyte level and the cover plate 2 will be discharged along the exhaust pipe 4, and the N-shaped rod 81 will be driven downward, so that the piston plate 82 squeezes the gas inside the air cavity 25, and the gas is introduced into the left annular cavity 14 along the air pipe 83. At this time, the gas will push the striking fan 17 to rotate, so that the striking fan 17 during the rotation will continue to strike the vibration rod 16 for a short period of time, and the bubbles attached to the electrolyte will be shaken out by vibration, so that they are discharged along the exhaust pipe 4. Then the user can turn on the power to perform electrolysis operations. At this time, the collection component 5 can be connected to the exhaust pipe 4. After use, the user can also use the scraper 21 in combination with the vibration rod 16 to vibrate and scrape the sediment on the bottom wall of the cell body 1 to improve the cleaning effect. After the cover plate 2 is reset in the later stage, the piston plate 82 draws the external gas back into the air cavity 25.

[0047] See also Figure 1-4 , wherein: the collection component 5 includes a docking joint 51, a collection tube 52, two connecting tubes 53, a piston disc 54 and a solenoid valve 55, the opposite ends of the two connecting tubes 53 are both penetrated and fixedly connected to the inside of the collection tube 52, the bottom connecting tube 53 is connected to the exhaust pipe 4 through the docking joint 51 fixedly installed on the outside, the outer side of the piston disc 54 is slidably connected to the inside of the collection tube 52, and the solenoid valve 55 is installed on the bottom connecting tube 53.

[0048] The user can insert the docking joint 51 into the top of the exhaust pipe 4 to connect the exhaust pipe 4 with the bottom connecting pipe 53. The gas generated by the electrolysis operation will then be introduced into the collection pipe 52 along the bottom connecting pipe 53, pushing the piston plate 54 upward. At this time, the gas inside the collection pipe 52 will be discharged along the top connecting pipe 53. After the collection operation is completed, the solenoid valve 55 can be closed to ensure the collection effect.

[0049] See also Figure 1-2 , wherein: a metal ring 18 is embedded on the outer side of the piston disc 54 , and a magnetic ring 19 is sleeved on the outer side of the collection tube 52 .

[0050] When the collected gas needs to be introduced, the solenoid valve 55 can be opened, and then the magnetic ring 19 can be moved to drive the metal ring 18 and the piston disk 54 to move, thereby improving the gas introduction efficiency.

[0051] See also Figure 1-7 , wherein: the transmission mechanism 9 includes a synchronous belt 91 and three synchronous wheels 92 , the three synchronous wheels 92 are respectively installed on two rotating shafts 11 and a connecting shaft 20 , and the synchronous belt 91 is installed on the outer sides of the three synchronous wheels 92 .

[0052] When the rotating shaft 11 rotates, the synchronous wheel 92 connected thereto will rotate accordingly, so that the synchronous belt 91 drives the middle synchronous wheel 92 to move, and the connecting shaft 20 is driven.

[0053] See also Figure 1-8 , wherein: a guide plate 22 is arranged on the outer side of the right rotating shaft 11 , and one side of the guide plate 22 is installed in the fixed pipe 7 on the right side of the pool body 1 .

[0054] The guide plate 22 is arranged so that the electrolyte can avoid the middle part of the stirring blade 12 during the flow process, thereby ensuring the normal rotation of the stirring blade 12 and reducing the occurrence of stuck or non-rotating phenomena.

[0055] See also Figure 1-9 , wherein: a group of baffles 23 are slidably installed inside the scraper 21 , and arc portions are provided at the bottom of the front and back sides of the baffles 23 , and the top end of the vibration rod 16 contacts the bottom of the baffles 23 .

[0056] Since the bottom of the front and back sides of the baffle 23 are both provided with arc-shaped portions, the baffle 23 can perform adaptive interlaced motion with the vibration rod 16 during the rotation of the scraper 21 without affecting the normal motion of the vibration rod 16 and the scraper 21 .

[0057] See also Figure 1-5 , wherein: the left and right sides of the baffle 23 are fixedly connected with a counterweight block 24 , and the outer side of the counterweight block 24 is slidably connected to the inside of the scraper 21 .

[0058] By adopting the arrangement of the counterweight block 24 , after the baffle plate 23 is separated from the vibration rod 16 , gravity can be used to drive the baffle plate 23 to quickly return downward, thereby ensuring the contact effect with the inner bottom wall of the pool body 1 .

[0059] See also Figure 1-3 , wherein: a control panel is installed on the front of the pool body 1.

[0060] Users can use the control panel to control the electrical components inside the entire device.

[0061] See also Figure 1-2, wherein: a discharge pipe 10 is installed on the right side of the pool body 1 and the outer fixed pipe 7, and valves are installed on the two discharge pipes 10 and the feed pipe 13.

[0062] After the feeding operation is completed, the corresponding valve can be closed. After use, the valves on the two discharge pipes 10 can be opened to discharge the sediment and the electrode liquid.

[0063] It should be noted that the electrical devices in this application are common devices in the market, and can be selected according to specific needs during use. The circuit connection relationships of the devices are all simple series and parallel connection circuits. There is no innovation in the circuit connection. Those skilled in the art can easily implement it. It belongs to the existing technology and will not be elaborated on.

[0064] The above is only a preferred specific implementation of the present invention; however, the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical solution and its improved conception within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. An electrolytic cell for preparing perfluorobutyryl fluoride gas, comprising a cell body (1), characterized in that: The interior of the pool body (1) is provided with a cover plate (2) which is slidably sealed with the inner wall thereof; an electric push rod (3) is installed on the outer side of the cover plate (2); the top end of the electric push rod (3) is installed to the inner top wall of the pool body (1); an exhaust pipe (4) is installed on the cover plate (2); a collection assembly (5) is installed on the outer side of the exhaust pipe (4); a delivery pump (6) is installed on the outer side of the pool body (1); the output end and the input end of the delivery pump (6) are both fixedly connected to fixed pipes (7); the ends of the two fixed pipes (7) away from the delivery pump (6) respectively penetrate and are fixedly connected to the left and right sides of the interior of the pool body (1); a feed pipe (13) is installed on the two fixed pipes (7); the interiors of the two fixed pipes (7) are rotatably connected to a rotating shaft (11); the top end of the rotating shaft (11) penetrates and is rotatably connected to a stirring blade (12) at the bottom end of the feed pipe (13); the two fixed pipes (7) are connected to the inner sides of the two fixed pipes (7); A transmission mechanism (9) is arranged between the rotating shafts (11), a connecting shaft (20) is installed on the transmission mechanism (9), the bottom end of the connecting shaft (20) penetrates and is fixedly connected to a scraper (21) in contact with the inner bottom wall of the pool body (1), an air guide component (8) is arranged inside the pool body (1), a group of annular cavities (14) are opened inside the pool body (1), a group of conduits (15) are installed inside the pool body (1), two adjacent annular cavities (14) are connected through the conduits (15) therebetween, the right end of the right conduit (15) penetrates and is fixedly connected to the outer side of the pool body (1), a group of vibration rods (16) are installed on the inner bottom wall of the pool body (1), the top end of the vibration rod (16) extends to the inside of the scraper (21), and the inside of the annular cavity (14) is rotatably connected to a striking fan (17) in contact with the outer side of the vibration rod (16); The air guide assembly (8) comprises an N-shaped rod (81), a piston plate (82) and an air pipe (83); both ends of the N-shaped rod (81) penetrate through and are slidably connected to the interior of the pool body (1); one end of the N-shaped rod (81) is fixedly connected to the top of the cover plate (2); the other end of the N-shaped rod (81) is fixedly connected to the top of the piston plate (82); an air cavity (25) is provided on the left side of the interior of the pool body (1); the outer side of the piston plate (82) is slidably connected to the interior of the air cavity (25); the air pipe (83) is embedded in the interior of the pool body (1); the top end of the air pipe (83) is in communication with the air cavity (25); and the right end of the air pipe (83) is in communication with the left annular cavity (14).

2. An electrolytic cell for preparing perfluorobutyryl fluoride gas according to claim 1, characterized in that: The collection assembly (5) comprises a butt joint (51), a collection tube (52), two connecting tubes (53), a piston disc (54) and a solenoid valve (55); opposite ends of the two connecting tubes (53) penetrate through and are fixedly connected to the interior of the collection tube (52); the bottom connecting tube (53) is butt-jointed with the exhaust pipe (4) via a butt joint (51) fixedly mounted on the outside; the outside of the piston disc (54) is slidably connected to the interior of the collection tube (52); and the solenoid valve (55) is mounted on the bottom connecting tube (53).

3. An electrolytic cell for preparing perfluorobutyryl fluoride gas according to claim 2, characterized in that: A metal ring (18) is embedded on the outer side of the piston disc (54), and a magnetic ring (19) is sleeved on the outer side of the collection tube (52).

4. An electrolytic cell for preparing perfluorobutyryl fluoride gas according to claim 1, characterized in that: The transmission mechanism (9) comprises a synchronous belt (91) and three synchronous wheels (92); the three synchronous wheels (92) are respectively mounted on two rotating shafts (11) and a connecting shaft (20); and the synchronous belt (91) is mounted on the outside of the three synchronous wheels (92).

5. An electrolytic cell for preparing perfluorobutyryl fluoride gas according to claim 1, characterized in that: A guide plate (22) is provided on the outer side of the right rotating shaft (11), and one side of the guide plate (22) is installed in a fixed pipe (7) located on the right side of the tank body (1).

6. An electrolytic cell for preparing perfluorobutyryl fluoride gas according to claim 1, characterized in that: A group of baffles (23) are slidably mounted inside the scraper (21), and arc-shaped portions are provided at the bottom of the front and back sides of the baffles (23), and the top end of the vibration rod (16) contacts the bottom of the baffles (23).

7. An electrolytic cell for preparing perfluorobutyryl fluoride gas according to claim 6, characterized in that: The left and right sides of the baffle plate (23) are both fixedly connected with a counterweight block (24), and the outer side of the counterweight block (24) is slidably connected to the inside of the scraper plate (21).

8. An electrolytic cell for preparing perfluorobutyryl fluoride gas according to claim 1, characterized in that: A control panel is installed on the front of the pool body (1).

9. An electrolytic cell for preparing perfluorobutyryl fluoride gas according to claim 1, characterized in that: A discharge pipe (10) is installed on the right side of the tank body (1) and the outer fixed pipe (7), and valves are installed on the two discharge pipes (10) and the feed pipe (13).

Images