A continuous production device and method for perfluorotributylamine

Abstract

The invention relates to a continuous production device and method of perfluorotributylamine, and belongs to the field of perfluorotributylamine preparation and fluid working system. In the process, tributylamine and hydrogen fluoride are in a mass ratio of 24-30kg:200-230kg, hydrogen fluoride is first added to an electrolytic cell, and then tributylamine is added; before the reaction, the air in the electrolytic cell is replaced by nitrogen, and the air is replaced by nitrogen for preliminary mixing and preparing electrolyte; then a low-voltage current is passed to carry out an electrolytic replacement reaction, and the reaction pressure is controlled at 0.1-1.5MPa and the temperature is controlled at 5-15°C; by controlling the reflux distribution of the circulating liquid and the single circulation path, the product with a large specific gravity is deposited in the pipeline equipment, the reaction activity, the fluorination efficiency and the conversion rate are improved, and the electrolytic fluorination method is adopted, the reaction is mild and controllable, the process is simple, the efficiency is high, the impurities are few and easy to separate, and the scheme also provides a perfluorotributylamine preparation device, which is adapted to the preparation process thereof, and a perfluorotributylamine crude product with a purity of more than 80% is obtained under the conditions of simple reaction raw materials and simple reaction device.

Description

Technical Field

[0001] The invention belongs to the technical field of perfluorotributylamine preparation and fluid working system, and specifically relates to a continuous production device and method of perfluorotributylamine. Background Art

[0002] At present, perfluorotributylamine is mainly used in anti-corrosion transmission fluids of instruments and meters, dielectric insulating fluids, electronic components, device leak detection fluids, perfluorocarbon artificial plasma, etc.; perfluorotributylamine can be used as a blood substitute and is also an excellent dielectric insulating fluid. In addition, it can also be used as a thermal conductive coolant, antioxidant lubricant, chemical reaction stabilizing diluent, etc.

[0003] Perfluorotributylamine molecule is an important perfluoro tertiary amine compound. Due to its many excellent physical, chemical and physiological properties, it has been widely used in modern civilized society. Perfluorotributylamine is a colorless and transparent liquid at room temperature, with almost no amine smell. It is insoluble in water and ethanol, and its solubility in organic solvents such as butanone, ether, chloroform, dioxane, ethyl acetate, benzene and petroleum ether is also very small, but it can be miscible with chlorofluoroalkanes. Perfluorotributylamine is completely non-toxic to the human body and can dissolve and carry a large amount of oxygen and carbon dioxide. It is one of the main components of artificial plasma used in the field of modern medicine. It is also used as an anti-corrosion transmission fluid, dielectric insulation fluid, and electronic component and device leak detection fluid for instruments and meters. The production of perfluorotributylamine is of great significance to the country's scientific progress and development.

[0004] In the existing technology for preparing perfluorotributylamine, such as using fluorine gas and tributylamine to directly react, this preparation method has the following disadvantages: low reaction efficiency, complex process, difficult reaction control, high risk factor, etc., which violates the development trend of energy-saving, clean, environmentally friendly and efficient fine chemical industry. The reaction formula of this preparation is as follows: Figure 1 As shown; There is also an electrochemical combined fluorination process in the existing technology for preparing perfluorotributylamine, using low-boiling carbon compounds and high-boiling amine compounds as two raw materials to be fluorinated, dissolving the combination of the two raw materials to be fluorinated in anhydrous hydrogen fluoride, and conducting a combined electrolytic fluorination reaction to simultaneously obtain corresponding low-boiling perfluorocarbon compounds and high-boiling perfluoroamine compounds. This preparation method has the following disadvantages: complex reaction conditions, complex and diverse reaction products and tail gases, high difficulty and high cost in separation, uncontrollable reaction direction, etc., which is not conducive to industrial production; The most widely used method for preparing perfluorotributylamine is the electrolytic fluorination method, in which tributylamine and hydrogen fluoride are fed into a low-voltage direct current in an electrolytic cell to generate free fluorine atoms to directly replace the hydrogen atoms in tributylamine, but this method still has the following disadvantages: low reaction activity, low fluorination efficiency, low conversion rate, large raw material loss, etc., and the overall production capacity is limited.

[0005] Therefore, this solution proposes a continuous production device and method for perfluorotributylamine that can solve the above problems. Summary of the invention

[0006] In view of the deficiencies in the prior art, the technical problem to be solved by the present invention is to provide a continuous production device and method for perfluorotributylamine, which can.

[0007] In order to solve the above technical problems, the technical solution adopted by the present invention is: a continuous production device of perfluorotributylamine, comprising an electrolytic component, a cooling component and a water circulation component, wherein the electrolytic component comprises two electrolytic cells stacked up and down, a cover body and a plurality of electrolytic plate kits, wherein the cover body is sealed and covered on the electrolytic cell located at the top, wherein the electrolytic cell has a reaction chamber, wherein the cover body has a liquid inlet chamber, and adjacent reaction chambers and liquid inlet chambers and reaction chambers are blocked by a blocking plate, wherein the blocking plate has a liquid inlet hole; wherein the plurality of electrolytic plate kits are located in the reaction chamber and are arranged at intervals on the left and right;

[0008] The water circulation assembly includes two pump bodies, an intermediate cylinder, a plurality of swing plates and a circulation pipeline. The two pump bodies are respectively located at one side of the liquid inlet end and the liquid outlet end of the electrolytic assembly. The intermediate cylinder is located between the two pump bodies. The circulation pipeline is located between the intermediate cylinder and the pump body and between the electrolytic assembly and the pump body. The swing plate is located in the electrolytic cell. The swing plate is used to drive the liquid in the electrolytic cell to move toward the electrolytic plate set. The liquid passes through the reaction chamber, the circulation pipeline, the intermediate cylinder, the circulation pipeline, the liquid passage chamber and the reaction chamber in sequence for circulation electrolysis.

[0009] The cooling component is used to cool the liquid in the circulation pipeline.

[0010] Furthermore, the electrolytic plate kit includes multiple groups of reaction plates and cover frames arranged in sequence on the left and right, the reaction plates include anode plates and cathode plates, and a liquid inlet channel is provided between the anode plates and the cathode plates. The cover frame is arranged above the multiple groups of reaction plates, and multiple strip-shaped liquid holes are formed on the cover frame, and the lower openings of the multiple liquid holes respectively correspond to the upper openings of the multiple liquid inlet channels.

[0011] Furthermore, the width of the lower opening of the liquid passage hole is greater than the width of the upper opening of the liquid inlet channel, and the lower opening of the liquid passage hole is an arc-shaped opening.

[0012] Furthermore, the swing plate is located on both sides of the plurality of reaction plates, the swing direction of the swing plate is toward the side opening of the liquid inlet channel, and both sides of the swing plate are rotatably connected to the inner wall of the reaction chamber.

[0013] Furthermore, an opening is provided on the swing plate, and a one-way opening and closing plate is provided in the opening. The one-way opening and closing plate is closed when it approaches the reaction plate, and is opened when it moves away from the reaction plate.

[0014] Furthermore, the bottom of the reaction chamber located at the bottom is an arc-shaped bottom or a conical bottom.

[0015] Furthermore, the cooling component includes a cooling tower, in which a plurality of baffles are arranged at intervals up and down, and the plurality of baffles are connected to the left and right sides of the inner wall of the cooling tower. The coolant path in the cooling tower is in the shape of a vertically arranged equal-amplitude oscillation curve, and the circulation pipeline in the cooling tower is arranged in a spiral manner.

[0016] A method for continuously producing perfluorotributylamine adopts a continuous production device for perfluorotributylamine, comprising the following steps: S1, replacing the air in the reaction chamber of an electrolytic cell with nitrogen, first adding hydrogen fluoride into the electrolytic cell body, then adding tributylamine, and forming an electrolyte after preliminary mixing, and starting a pump body for circulation, so that the electrolyte fills 60%-80% of the total volume of the intermediate cylinder and multiple reaction chambers;

[0017] S2. Perform low-pressure electrolysis, control the reaction pressure at 0.1MPa-1.5MPa, and the temperature at 5℃-15℃. The pump body starts to operate. The pump body near the liquid inlet of the electrolytic cell controls the volume of the electrolyte in the reaction chamber near it to account for 70-80% of the volume of the reaction chamber. The pump body near the liquid outlet of the electrolytic cell controls the volume of the electrolyte in the reaction chamber near it to account for 70-80% of the volume of the reaction chamber.

[0018] S3. During the electrolyte circulation process, the electrolyte flushes the surface of the anode plate and the cathode plate in three directions;

[0019] S4. After the cyclic electrolysis is completed, a crude product of perfluorotributylamine with a purity of more than 80% is obtained.

[0020] Furthermore, the specific steps in S3 are as follows: the electrolyte flows in from the liquid inlet of the partition, the electrolyte is pressurized, and then enters the liquid hole of the cover frame, the liquid hole corresponds to the liquid inlet channel, the electrolyte in the liquid hole rushes into the liquid inlet channel to flush the anode plate and the cathode plate, and during the electrolysis process, the swing plates located on both sides of the electrolysis component swing toward the electrolysis component in a cyclic manner, driving the electrolyte to flow toward the liquid inlet channel between the anode plate and the cathode plate, thereby achieving double flushing.

[0021] Furthermore, the mass ratio of tributylamine to hydrogen fluoride in step S1 is 24-30kg:200-230kg.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] 1. The invention provides a process for preparing perfluorotributylamine. The mass ratio of tributylamine to hydrogen fluoride is 24-30kg:200-230kg. Hydrogen fluoride is first added to an electrolytic cell, and then tributylamine is added. Before the reaction, the air in the electrolytic cell is replaced by nitrogen, and the air is replaced by nitrogen for preliminary mixing and preparing an electrolyte. Then, a low-voltage current is passed to carry out an electrolytic replacement reaction, and the reaction pressure is controlled at 0.1-1.5MPa and the temperature is controlled at 5-15°C. By controlling the reflux distribution of the circulating liquid and the single circulation path, the product with a large specific gravity is placed in the pipeline equipment to improve the reaction activity, fluorination efficiency, and conversion rate. The electrolytic fluorination method has mild and controllable reaction, simple process, high efficiency, less impurities and easy separation. Moreover, the present invention also provides a continuous production device for perfluorotributylamine, wherein the electrolytic cell is configured as an electrolytic cell that can be stacked up and down, and the number of electrolytic plate sets provided in the electrolytic cell is reduced. By configuring the electrolytic cell, the length of the electrolytic cell can be reduced, and the space above the electrolytic cell can be fully utilized. Compared with the existing electrolytic cell device, the electrolytic cell occupies less space, and the length of the electrolytic cell is shortened, and the circulation speed of the electrolyte is faster (reducing the distance between the electrolyte and the liquid outlet), thereby improving the electrolysis efficiency. Since the electrolytic cell is stacked up and down, in order to ensure the electrolysis rate, the volume of the electrolyte in the reaction chamber needs to account for 70% of the volume of the reaction chamber. %, the reaction chamber located at the top is controlled by the pump body close to one side thereof. When the electrolyte in the upper reaction chamber is insufficient, the pump body accelerates the operation, so that the electrolyte in the middle cylinder flows into the upper reaction chamber faster; the reaction chamber located at the bottom is controlled by the pump body close to one side thereof. When the electrolyte in the lower reaction chamber is insufficient, the pump body reduces the operation speed, so that the electrolyte flows out of the lower reaction chamber more slowly. The above arrangement enables the control of the electrolyte volume in the reaction chamber. The electrolytic cells, pump bodies, middle cylinders and circulation pipelines stacked up and down form a fluid working system dedicated to this scheme.

[0024] 2. The cooling components and circulation components in this solution use a single circulation pipeline for flow circulation and heat exchange, which can avoid the accumulation of electrolysis products.

[0025] 3. The bottom of the electrolytic reaction chamber is an arc-shaped bottom or a conical bottom, so that the products produced by electrolysis can be fully circulated.

[0026] 4. In order to flush away the tar attached to the surface of the plate produced during the electrolysis process, the electrolyte of this scheme will be pressurized when entering from the liquid inlet of the separator, and then flow into the liquid hole of the cover frame. The liquid hole corresponds to the opening on the liquid inlet channel between the anode plate and the cathode plate. The electrolyte will rush into the liquid inlet channel at a faster speed. This impact force can flush off the tar on the surface of the anode plate and the cathode plate. Since the lower part of the liquid inlet channel is connected to the reaction chamber of the electrolytic cell, the electrolyte will flow out to both sides after entering the liquid inlet channel, so the speed of the electrolyte entering the liquid inlet channel is gradually reduced. This may lead to incomplete cleaning of tar adhesion under the anode plate and the cathode plate, so the present scheme also adds two swinging plates, which are located on both sides of the liquid inlet channel, and the swinging plates reciprocate to push the electrolyte into the liquid inlet channel. The driving force of the electrolyte toward the liquid inlet channel can reduce the tendency of the electrolyte that has just flowed into the liquid inlet channel to flow outward, so that the electrolyte that has just flowed into the liquid inlet channel can maintain a relatively high speed to rush into the bottom of the anode plate and the cathode plate, ensuring comprehensive flushing, and the swinging plate pushes the electrolyte to move into the liquid inlet channel, which can also flush the surface of the anode plate and the cathode plate. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 is the chemical formula for the direct reaction of fluorine gas and tributylamine in the background technology of the present invention;

[0028] Figure 2 This is a schematic diagram of the principle structure of a continuous production device of perfluorotributylamine in the present invention;

[0029] Figure 3 It is a schematic diagram of the three-dimensional structure of the electrolytic component in the present invention;

[0030] Figure 4 It is a schematic diagram of the split structure of the electrolytic component in the present invention;

[0031] Figure 5 It is a schematic diagram of the split structure of the electrolytic component in another direction of the present invention;

[0032] Figure 6 It is a schematic cross-sectional view of the electrolytic component in the present invention;

[0033] Figure 7 For the present invention Figure 6 A schematic diagram of the local enlarged structure at point A in the middle;

[0034] Figure 8 It is a schematic cross-sectional view of the electrolytic component in another direction of the present invention;

[0035] Fig. 9 For the present invention Figure 8 A schematic diagram of the local enlarged structure at B in the middle;

[0036] Fig.10 It is a schematic diagram of the three-dimensional structure of the swing plate in the present invention;

[0037] Fig.11 It is a partial cross-sectional structural schematic diagram of the swing plate in the present invention;

[0038] Fig.12 It is a schematic diagram of the three-dimensional structure of the electrolytic plate set in the present invention;

[0039] Fig.13 It is a partial side view structural schematic diagram of the electrolytic plate set in the present invention;

[0040] Fig.14 It is a schematic cross-sectional view of the electrolytic plate set in the present invention;

[0041] Fig.15 It is a schematic diagram of the three-dimensional structure of the electrolytic cell located at the top in the present invention;

[0042] Fig.16 It is a schematic diagram of the three-dimensional structure of the partition in the present invention;

[0043] Fig.17 It is a schematic diagram of the three-dimensional structure of the electrolytic cell located at the bottom in the present invention;

[0044] Fig.18 It is a schematic diagram of the principle structure of the cooling component in the present invention.

[0045] Markings in the figure: 1. electrolytic assembly; 11. electrolytic cell; 111. reaction chamber; 12. cover; 121. liquid inlet chamber; 13. electrolytic plate set; 131. fixed column; 132. reaction plate; 1321. anode plate; 1322. cathode plate; 1323. liquid inlet channel; 133. left fixed plate; 134. right fixed plate; 135. middle plate; 136. power supply column; 137. cover frame; 1371. liquid through hole; 1372. inclined guide platform; 14. partition; 141. liquid inlet hole; 2. cooling assembly; 21. cooling tower; 21 1. Baffle; 3. Water circulation assembly; 31. Pump body; 32. Intermediate cylinder; 33. Swing plate; 331. One-way opening and closing plate; 332. Swing limit block; 333. Opening; 334. Limit convex strip; 34. Circulation pipeline; 341. First pipeline; 3411. First solenoid valve; 342. Second pipeline; 3421. Second solenoid valve; 343. Third pipeline; 3431. Third solenoid valve; 344. Fourth pipeline; 3441. Fourth solenoid valve; 345. Fifth pipeline; 3451. Fifth solenoid valve; 4. Exhaust treatment assembly. DETAILED DESCRIPTION

[0046] In order to make the above features and advantages of the present invention more obvious and easy to understand, embodiments are given below with reference to the accompanying drawings for detailed description as follows.

[0047] like Figure 1-Figure 18 As shown, this embodiment provides a continuous production device of perfluorotributylamine, including an electrolysis component 1, a cooling component 2, a water circulation component 3 and an exhaust gas treatment component 4.

[0048] like Figure 3-Figure 9 and Figure 15-17 As shown, the electrolytic assembly 1 includes two electrolytic cells 11 stacked up and down, a cover body 12, a fixing column 131, and two electrolytic plate sets 13. The reaction chamber 111 of the upper electrolytic cell 11 has upper and lower openings 333, and the reaction chamber 111 of the lower electrolytic cell 11 has an upper opening 333. The cover body 12 is sealed and covered on the uppermost electrolytic cell 11. A partition 14 is arranged between the cover body 12 and the electrolytic cell 11. A first limiting step is arranged at the opening 333 on the lower surface of the cover body 12. The partition 14 is sealed and embedded in the first limiting step. The cover body 12 and the partition 14 surround and form a liquid inlet cavity. Chamber 121, a partition 14 is also provided between the electrolytic cell 11 and the electrolytic cell 11, a reaction chamber 111 is provided in the electrolytic cell 11, the reaction chamber 111 of the electrolytic cell 11 located at the top is formed by the upper and lower partitions 14 and the inner wall of the electrolytic cell 11, the reaction chamber 111 of the electrolytic cell 11 located at the bottom is formed by the partition 14 and the inner wall of the electrolytic cell 11, the bottom of the reaction chamber 111 located at the bottom is an arc bottom or a conical bottom, this scheme adopts an arc bottom, and the bottom of the electrolysis reaction chamber 111 is set to be an arc bottom or a conical bottom, so that the products produced by electrolysis can be fully circulated. A first density meter for measuring the nitrogen density in the reaction area is provided in the middle of the circumference of the electrolytic cell 11, and a second density meter for measuring the density of the electrolyte after the reaction is provided below the electrolytic cell 11. A nitrogen inlet and an electrolyte raw material inlet are also provided on the side wall of the electrolytic cell 11 body.

[0049] The two electrolytic plate kits 13 are located in the reaction chamber 111 and are spaced apart from each other on the left and right sides. The same fixing column 131 passes through the two electrolytic plate kits 13 and the two ends are respectively connected to the two inner walls of the reaction chamber 111 for fixation. Preferably, a mounting groove can be provided on the side wall of the reaction chamber 111 for positioning and installing the fixing column 131. The optimal number of electrolytic plate kits 13 is 2-4, which is set according to actual conditions. The electrolytic plate kit 13 includes seven groups of reaction plates 132, cover frames 137, left fixed plates 133, right fixed plates 134 and adjacent intermediate plates 135, which are arranged in sequence. The reaction plates 132, left fixed plates 133, right fixed plates 134 and adjacent intermediate plates 135 are connected by bolts. The adjacent intermediate plates 135 are located between adjacent reaction plates 132. The left fixed plate 133 and the right fixed plate 134 are respectively located on the leftmost and rightmost sides of the entire electrolytic plate kit 13. The electrolytic plate kit 13 is also penetrated by two power supply poles 136, one of which is used to supply power to the anode plate 1321 in the reaction plate 132, and the other power supply pole 136 is used to supply power to the cathode plate 1322 in the reaction plate 132. One side of the two power supply poles 136 passes through the side wall of the electrolytic cell 11. The number of reaction plates 132 is set according to actual needs. The above structure is implemented using the common settings in existing electrolysis devices, which will not be repeated again.

[0050] The reaction plate 132 includes an anode plate 1321, a cathode plate 1322 and an ion diaphragm, the ion diaphragm is located between the anode plate 1321 and the cathode plate 1322, a liquid inlet channel 1323 is formed between the anode plate 1321 and the cathode plate 1322, the distance between the anode plate 1321 and the cathode plate 1322 is 50mm-120mm, in this solution, the distance between the anode plate 1321 and the cathode plate 1322 is 100mm, and the distance between the anode plate 1321 and the cathode plate 1322 is set according to the actual situation with reference to the number of electrolytic plate sets 13 and the volume of the reaction chamber 111. Figure 12-14As shown, the cover frame 137 is covered on the plurality of reaction plates 132, and a plurality of strip-shaped liquid holes 1371 are formed on the cover frame 137, and the lower openings 333 of the plurality of liquid holes 1371 correspond to the upper openings 333 of the plurality of liquid inlet channels 1323, respectively. Specifically, the upper surface of the cover frame 137 is in contact with the lower surface of the partition 14, and the partition 14 is provided with a plurality of liquid inlet holes 141, and the positions and numbers of the liquid inlet holes 141 correspond to the liquid inlet holes 1371, and the upper opening 333 of the liquid inlet is formed with an expanded opening, and the liquid inlet holes 1371 correspond to the upper opening 333 of the liquid inlet. The upper opening 333 of 71 is provided with a V-shaped expansion, and the lower opening 333 of the liquid hole 1371 has an arc shape in vertical section, that is, an arc-shaped opening 333. The lower opening 333 of the liquid hole 1371 covers the upper opening 333 of the liquid inlet channel 1323. The material of the cover frame 137 is an insulating material. In this solution, the cover frame 137 is made of plastic. The liquid inlet hole 141 and the liquid hole 1371 are provided to ensure that the electrolyte enters the liquid inlet channel 1323 after being pressurized during the circulation process to flush the surface of the electrode plate. Specifically, inclined guide platforms 1372 are further provided on both sides of the inner wall of the cover frame 137 facing the side of the liquid inlet channel 1323. Because the cover frame 137 can only cover the outer periphery of the left fixed plate 133 and the right fixed plate 134, there is still a gap between the inner wall of the cover frame 137 and the electrode plate. When the electrolyte flows out from the liquid hole 1371, it will directly flow out from both sides of the liquid inlet channel 1323. In order to ensure that the electrolyte enters the liquid inlet channel 1323, an inclined guide platform 1372 is provided. The side wall of the inclined guide platform 1372 is pressed against the side wall of the reaction plate 132, so that the electrolyte will enter the liquid inlet channel 1323 when it flows out from the liquid hole 1371.

[0051] like Figure 1 , Figure 7 and Fig.10As shown, the water circulation component 3 includes two pump bodies 31, an intermediate cylinder 32, a plurality of swing plates 33 and a circulation pipeline 34. The two pump bodies 31 are respectively located on the liquid inlet and liquid outlet sides of the electrolytic component 1, the intermediate cylinder 32 is located between the two pump bodies 31, and the circulation pipeline 34 is located between the intermediate cylinder 32 and the pump body 31 and between the electrolytic component 1 and the pump body 31. The liquid passes through the reaction chamber 111, the circulation pipeline 34, the intermediate cylinder 32, the circulation pipeline 34, the liquid passage chamber and the reaction chamber 111 in sequence for circulation electrolysis. Specifically, the circulation pipeline 34 includes a first pipeline 341, a second pipeline 342, a third pipeline 343, a fourth pipeline 344 and a fifth pipeline 345. The first pipeline 341 is located below the electrolytic cell 11 and between the pump body 31. A first solenoid valve 3411 is provided on the first pipeline 341. The two ends of the second pipeline 342 are respectively connected to the pump body 31 and the third pipeline 343. A second solenoid valve 3421 is provided on the second pipeline 342. The other end of the third pipeline 343 is connected to the fourth pipeline 344. The third pipeline 343 passes through the cooling component 2. A third solenoid valve 3431 is provided on the third pipeline 343. The other end of the fourth pipeline 344 is connected to the liquid inlet end of the intermediate tank. A fourth solenoid valve 3441 is provided on the fourth pipeline 344. The two ends of the fifth pipeline 345 are respectively connected to the intermediate tank and the cover body 12. A fifth solenoid valve 3451 is provided on the fifth pipeline 345. The second pipeline 342 may be provided with a liquid outlet pipe to transfer the finished product after electrolysis out through the liquid outlet pipe.

[0052] like Figure 7 , Fig.10 and Fig.11 As shown, the swing plate 33 is located in the electrolytic cell 11, and the swing plate 33 is used to drive the liquid in the electrolytic cell 11 to move toward the electrolytic plate set 13. Specifically, the swing plate 33 is located on both sides of the reaction plate 132, and the swing direction of the swing plate 33 is toward the side opening 333 of the liquid inlet channel 1323. Both sides of the swing plate 33 are rotatably connected to the inner wall of the reaction chamber 111. The axial end of the swing plate 33 is located on the upper side, and one side of the axial end of the swing plate 33 passes through the side wall of the electrolytic cell 11 and is driven by a motor. Preferably, an opening 333 is provided on the swing plate 33, and a one-way opening and closing plate 331 is provided in the opening 333. The one-way opening and closing plate 331 is closed when it is close to the reaction plate 132, and is opened when it is away from the reaction plate 132. Specifically, as shown in FIG. Fig.11 As shown, a limiting convex strip 334 is formed in the opening 333, and the surface of the one-way opening and closing plate 331 abuts against the limiting convex strip 334. When the one-way opening and closing plate 331 is close to the reaction plate 132, the one-way opening and closing plate 331 is in a closed state because the surface of the one-way opening and closing plate 331 and the limiting convex strip 334 abut against each other. When the one-way opening and closing plate 331 is away from the reaction plate 132, the one-way opening and closing plate 331 opens under the resistance of the electrolyte. The one-way opening and closing plate 331 is provided to reduce the resistance when the swing plate 33 is reset. Further, as shown in FIG. Figure 7 As shown, two swing limit blocks 332 are formed on the side wall of the electrolytic cell 11, and the two swing limit blocks 332 are respectively located at the two ends of the lower position of the axial end of the swing plate 33, and are used to limit the swing angle of the swing plate 33. It is mentioned here that the axial end of the swing plate 33 is set below the electrolytic cell 11 or two swing plates 33 are set to open and close and swing, which can be applied to this solution.

[0053] like Fig.18 As shown, the cooling component 2 is used to cool the liquid in the circulation pipeline 34. The cooling component 2 includes a cooling tower 21. The cooling liquid inlet of the cooling tower 21 is at the upper end of the cooling tower 21, and the cooling liquid outlet of the cooling tower 21 is at the lower end of the cooling tower 21. A plurality of baffles 211 are arranged at intervals up and down in the cooling tower 21. The plurality of baffles 211 are connected to the left and right sides of the inner wall of the cooling tower 21. The cooling liquid path in the cooling tower 21 is in the shape of a vertically arranged equal-amplitude oscillation curve. The third pipeline 343 in the circulation pipeline 34 in the cooling tower 21 is arranged in a spiral manner.

[0054] The tail gas treatment component 4 is used to collect and process the gas in the electrolytic cell 11. Specifically, the electrolytic cell 11 is connected to the tail gas treatment component 4 through an exhaust pipe. The tail gas treatment component 4 adopts the tail gas treatment component 4 commonly used in the perfluorotributylamine preparation process in the prior art, which will not be described in detail here.

[0055] This embodiment also provides a method for continuous production of perfluorotributylamine, which adopts the above-mentioned continuous production device of perfluorotributylamine for production, and comprises the following steps:

[0056] S1. Replace the air in the reaction chamber 111 of the electrolytic cell 11 with nitrogen, first add hydrogen fluoride into the electrolytic cell 11 body, then add tributylamine, and form an electrolyte after preliminary mixing, start the pump body 31 for circulation, so that the electrolyte fills 60%-80% of the total volume of the intermediate cylinder 32 and the two reaction chambers 111, wherein the mass ratio of tributylamine to hydrogen fluoride is 24-30kg:200-230kg.

[0057] S2. Perform low-pressure electrolysis, control the reaction pressure at 0.1MPa-1.5MPa, and control the temperature at 5℃-15℃. The pump body 31 starts to operate, and the volume of the electrolyte in the intermediate cylinder 32 accounts for 60% of the volume of the intermediate cylinder 32. The pump body 31 near the liquid inlet of the electrolytic cell 11 controls the volume of the electrolyte in the reaction chamber 111 near it to account for 80% of the volume of the reaction chamber 111. The pump body 31 near the liquid outlet of the electrolytic cell 11 controls the volume of the electrolyte in the reaction chamber 111 near it to account for 80% of the volume of the reaction chamber 111. The volume of the reaction chamber 111 accounts for 80% of the volume of the reaction chamber 111. The specific steps are as follows: when the electrolyte in the upper reaction chamber 111 is insufficient, the pump body 31 accelerates the operation, so that the electrolyte in the middle cylinder 32 flows into the upper reaction chamber 111 faster; the reaction chamber 111 located below is controlled by one side of the pump body 31 close to it. When the electrolyte in the lower reaction chamber 111 is insufficient, the operation speed of the pump body 31 is reduced, so that the electrolyte flows out of the lower reaction chamber 111 more slowly.

[0058] S3. During the electrolyte circulation process, the electrolyte flushes the surfaces of the anode plate 1321 and the cathode plate 1322 in three directions. The specific steps are as follows: the electrolyte flows in from the liquid inlet of the partition 14, the electrolyte is pressurized, and then enters the liquid hole 1371 of the cover frame 137. The liquid hole 1371 corresponds to the liquid inlet channel 1323. The electrolyte in the liquid hole 1371 flushes into the liquid inlet channel 1323 to flush the anode plate 1321 and the cathode plate 1322. During the electrolysis process, the swing plates 33 located on both sides of the electrolysis component 1 swing toward the electrolysis component 1 in a cyclic manner, driving the electrolyte to flow into the liquid inlet channel 1323 between the anode plate 1321 and the cathode plate 1322, thereby achieving double flushing.

[0059] S4. After the cyclic electrolysis is completed, a crude product of perfluorotributylamine with a purity of more than 80% is obtained.

[0060] In step S1, this embodiment also provides several relatively excellent mass ratios of tributylamine and hydrogen fluoride. The mass ratio of tributylamine and hydrogen fluoride is 25kg:210kg.

[0061] The present invention aims to overcome the shortcomings of the prior art such as low reaction activity, low fluorination efficiency, low conversion rate, and large raw material loss. In order to break this technical barrier, a perfluorotributylamine deep fluorination device with simple reaction, high reaction activity, high fluorination degree, and high conversion rate is developed to achieve efficient and high-purity industrial production of perfluorotributylamine. The electrolytic fluorination method is adopted, and hydrogen fluoride and tributylamine are electrolyzed under the action of additives to achieve the purpose of replacing hydrogen atoms with fluorine atoms. The reaction mechanism is as follows:

[0062] Electrode reaction:

[0063] At cathode: H++e ─→ H H+H ─→ H2↑

[0064] At the anode: F--e ─→ F C-H+F ─→ C-F+H.

[0065] Through the process and apparatus of this embodiment, a crude perfluorotributylamine with a purity of more than 80% can be obtained under the conditions of simple reaction raw materials and simple reaction apparatus. The process and apparatus can increase the degree of fluorination in the reaction process from the original 70% to 80%, and the reaction raw materials and reaction apparatus are relatively simple, which is more conducive to the industrial production of perfluorotributylamine.

[0066] The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The above embodiments and descriptions are only for illustrating the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which shall fall within the scope of the present invention to be protected. The scope of protection of the present invention is defined by the attached claims and their equivalents.

Claims

1. A continuous production device for perfluorotributylamine, characterized in that: It comprises an electrolytic assembly, a cooling assembly and a water circulation assembly, wherein the electrolytic assembly comprises two electrolytic cells stacked up and down, a cover body and a plurality of electrolytic plate kits, wherein the cover body is sealed and covered on the electrolytic cell located at the top, wherein the electrolytic cell has a reaction chamber, wherein the cover body has a liquid inlet chamber, and the adjacent reaction chambers and the liquid inlet chamber and the reaction chamber are blocked by a blocking plate, wherein the blocking plate has a liquid inlet hole; the plurality of electrolytic plate kits are located in the reaction chamber and are spaced apart from each other on the left and right sides; The water circulation assembly includes two pump bodies, an intermediate cylinder, a plurality of swing plates and a circulation pipeline. The two pump bodies are respectively located at one side of the liquid inlet end and the liquid outlet end of the electrolytic assembly. The intermediate cylinder is located between the two pump bodies. The circulation pipeline is located between the intermediate cylinder and the pump body and between the electrolytic assembly and the pump body. The swing plate is located in the electrolytic cell. The swing plate is used to drive the liquid in the electrolytic cell to move toward the electrolytic plate set. The liquid passes through the reaction chamber, the circulation pipeline, the intermediate cylinder, the circulation pipeline, the liquid passage chamber and the reaction chamber in sequence for circulation electrolysis. The cooling component is used to cool the liquid in the circulation pipeline.

2. A continuous production device for perfluorotributylamine according to claim 1, characterized in that: The electrolytic plate kit includes multiple groups of reaction plates and cover frames arranged in sequence on the left and right, the reaction plates include anode plates and cathode plates, and a liquid inlet channel is provided between the anode plates and the cathode plates. The cover frame is arranged above the multiple groups of reaction plates, and multiple strip-shaped liquid holes are formed on the cover frame, and the lower openings of the multiple liquid holes respectively correspond to the upper openings of the multiple liquid inlet channels.

3. A continuous production device for perfluorotributylamine according to claim 2, characterized in that: The width of the lower opening of the liquid passage hole is greater than the width of the upper opening of the liquid inlet channel, and the lower opening of the liquid passage hole is an arc-shaped opening.

4. A continuous production device for perfluorotributylamine according to claim 2, characterized in that: The swing plate is located at both sides of the plurality of reaction plates, the swinging direction of the swing plate is toward the side opening of the liquid inlet channel, and both sides of the swing plate are rotatably connected to the inner wall of the reaction chamber.

5. A continuous production device for perfluorotributylamine according to claim 4, characterized in that: The swing plate is provided with an opening, and a one-way opening and closing plate is provided in the opening. The one-way opening and closing plate is closed when it approaches the reaction plate, and is opened when it is away from the reaction plate.

6. The continuous production device of perfluorotributylamine according to claim 1, characterized in that: The bottom of the reaction chamber located at the bottom is an arc-shaped bottom or a conical bottom.

7. The continuous production device of perfluorotributylamine according to claim 1, characterized in that: The cooling assembly includes a cooling tower, in which a plurality of baffles are arranged at intervals up and down, and the plurality of baffles are connected to the left and right sides of the inner wall of the cooling tower. The coolant path in the cooling tower is in the shape of a vertically arranged equal-amplitude oscillation curve, and the circulation pipeline in the cooling tower is arranged in a spiral manner.

8. A continuous production method of perfluorotributylamine, characterized in that: The continuous production device of perfluorotributylamine as claimed in any one of claims 1 to 7 is used for production, comprising the following steps: S1, replacing the air in the reaction chamber of the electrolytic cell with nitrogen, first adding hydrogen fluoride into the electrolytic cell body, then adding tributylamine, and forming an electrolyte after preliminary mixing, and starting the pump body for circulation, so that the electrolyte fills 60%-80% of the total volume of the intermediate cylinder and the multiple reaction chambers; S2. Perform low-pressure electrolysis, control the reaction pressure at 0.1MPa-1.5MPa, and the temperature at 5℃-15℃. The pump body starts to operate. The pump body near the liquid inlet of the electrolytic cell controls the volume of the electrolyte in the reaction chamber near it to account for 70-80% of the volume of the reaction chamber. The pump body near the liquid outlet of the electrolytic cell controls the volume of the electrolyte in the reaction chamber near it to account for 70-80% of the volume of the reaction chamber. S3. During the electrolyte circulation process, the electrolyte flushes the surface of the anode plate and the cathode plate in three directions; S4. After the cyclic electrolysis is completed, a crude product of perfluorotributylamine with a purity of more than 80% is obtained.

9. The continuous production method of perfluorotributylamine according to claim 8, characterized in that: The specific steps in S3 are as follows: the electrolyte flows in from the liquid inlet of the partition, the electrolyte is pressurized, and then enters the liquid hole of the cover frame, the liquid hole corresponds to the liquid inlet channel, the electrolyte in the liquid hole rushes into the liquid inlet channel to flush the anode plate and the cathode plate, and during the electrolysis process, the swing plates located on both sides of the electrolysis component swing toward the electrolysis component in a circular manner, driving the electrolyte to flow toward the liquid inlet channel between the anode plate and the cathode plate, thereby achieving double flushing.

10. The method for continuous production of perfluorotributylamine according to claim 8, characterized in that: The mass ratio of tributylamine to hydrogen fluoride in step S1 is 24-30kg:200-230kg.

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