Perfluorotributylamine production device capable of realizing deep fluorination and production method of perfluorotributylamine production device

Abstract

The invention relates to the technical field of perfluorotributylamine preparation, in particular to a perfluorotributylamine production device capable of deep fluorination and a production method thereof.The perfluorotributylamine production device structurally comprises an electrolytic bath body, a mother liquor inlet pipe outwards arranged on one side of the electrolytic bath body, and a heat exchange device used for conducting circulating refrigeration on materials in the electrolytic bath body; a multi-pipeline heat exchange pipe is replaced by a single-pipeline heat exchange pipe, the flowing path is simple, fluid flows in the same pipeline, the flowing speed is uniform, and the phenomenon that in the multi-pipeline design, due to uneven flow distribution, the flowing speed of some pipelines is too low, and local deposition is caused is avoided; and the product flows along the curve of the pipeline, the disturbance and turbulivity of the fluid are increased, the disturbance flow is beneficial to preventing electrolytic products from being deposited on the inner wall of the pipeline, and because the turbulent flow can improve the shearing force of the fluid, effectively washes away sediments, prevents substances from being accumulated in the pipeline, and effectively ensures the heat exchange uniformity and efficiency.

Description

Technical Field

[0001] The invention relates to the technical field of perfluorotributylamine preparation, in particular to a perfluorotributylamine production device capable of deep fluorination and a production method thereof. Background Art

[0002] 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.

[0003] The most widely used technology for preparing perfluorotributylamine is the electrolytic fluorination method. A mother liquor composed of tributylamine and hydrogen fluoride is fed with low-voltage direct current in an electrolytic cell to generate free fluorine atoms to directly replace the hydrogen atoms in tributylamine, and then the perfluorotributylamine product is obtained through a simple purification process. The electrolysis process is in an exothermic state, and the mother liquor and the product need to be circulated through a corresponding refrigeration heat exchanger to cool the mother liquor and the product to prevent the mother liquor and the product from gasifying due to temperature rise during the electrolysis process. In actual application, the following deficiencies still exist: the existing heat exchange pipeline adopts a multi-pipeline simultaneous heat exchange method, which is easy to cause the electrolysis product to stagnate, and the refrigerant is usually injected from the top of the heat exchange tank and flows directly downward during heat exchange. Inside the heat exchange tank, the refrigerant may flow faster along certain channels, while the flow rate in other areas is slower. There are dead zones in the heat exchange process. Due to uneven flow rate, some refrigerants may have a shorter contact time with the heat exchange tube when flowing through the heat exchange tube, and fail to fully absorb the heat of the tube wall, resulting in poor cooling effect and low heat exchange efficiency; There is also a bigger problem: as the heat exchanger is used for a longer time, scaling substances in the refrigerant (such as scale, rust, etc.) and other sediments will accumulate on the tube walls of the heat exchanger, thereby reducing the efficiency of heat exchange and electrolysis reaction, and even damaging the equipment. If the heat exchange tubes of the heat exchanger are dismantled and cleaned, the electrolytic cell needs to be shut down, which will also affect the production process. Summary of the invention

[0004] The present invention provides a perfluorotributylamine production device capable of deep fluorination and a production method thereof, which can effectively solve the above problems.

[0005] The present invention is achieved in that: A perfluorotributylamine production device capable of deep fluorination, the structure of which comprises: an electrolytic cell body, a mother liquid inlet pipe is arranged outwardly on one side of the electrolytic cell body, and a heat exchange device for circulating and cooling the material in the electrolytic cell body, the heat exchange device comprises a heat exchange tank body, a circulating liquid conduit is arranged in the heat exchange tank body, one end of the circulating liquid conduit is connected to the top of the heat exchange tank body and is pumped to the bottom of the electrolytic cell body through a circulating feed pipe, and the other end is connected to the bottom of the heat exchange tank body and is connected to the top of the bottom of the electrolytic cell body through a circulating discharge pipe, the circulating feed pipe is connected to the product discharge pipe outwardly through a three-way valve, and a densitometer for detecting material density is installed at the bottom of the electrolytic cell body; the circulating liquid conduit comprises an input pipe connected to the top of the heat exchange tank body, an output pipe connected to the bottom of the heat exchange tank body, and a heat exchange circulation pipe in the heat exchange tank body and connected between the input pipe and the output pipe, the heat exchange circulation pipe extends downward in a spiral shape; a refrigerant feed pipe is arranged on the top of the left side of the heat exchange tank body The heat exchange tank body is provided with a plurality of groups of flow guide devices connected with the heat exchange tank body on both sides, each group of flow guide devices includes an inlet and a drain, and a feeding pump arranged between the inlet and the drain, the inlet end of the inlet is connected with the heat exchange tank body, and the outlet end is connected with the feed port of the feeding pump, the inlet end of the drain is connected with the discharge port of the feeding pump, and the outlet end is connected with the heat exchange tank body, and the inlet of the top flow guide device on the right side is arranged correspondingly with the refrigerant feed pipe, the drain on the right side is arranged correspondingly with the inlet of the left flow guide device, the inlet of the left flow guide device is arranged correspondingly with the drain of the right flow guide device, and the drain of the bottom flow guide device on the left side is arranged correspondingly with the refrigerant discharge pipe; it also includes a cleaning mechanism for cleaning the surface of the heat exchange circulation pipe; the cleaning mechanism is arranged in the heat exchange tank body, and when the refrigerant enters the heat exchange tank body through the refrigerant feed pipe to cool the heat exchange circulation pipe, the cleaning mechanism moves up and down along the heat exchange circulation pipe for cleaning.

[0006] As a further improvement, the inlet and outlet both include a box body, the box body is provided with a first connecting port connected to the heat exchange tank body, the box body is connected to a second connecting port connected to a feed pump, a plurality of diverter plates extending from the first connecting port to the second connecting port are provided in the box body, and a filter net is provided on the first connecting port.

[0007] As a further improvement, the cleaning mechanism includes a rotating shaft coaxially arranged with the heat exchange circulation tube, a connecting tube is sleeved on the surface of the rotating shaft, a transmission screw sleeved in the rotating shaft is fixed in the heat exchange tank body, the transmission screw is provided with a track corresponding to the spiral of the heat exchange circulation tube, a vertically extending guide rail is provided on the rotating shaft, a guide column matching the guide rail and the transmission screw track is provided on the inner side of the connecting tube, the connecting tube is connected to the outside with a ring through a connecting rod, the ring is correspondingly sleeved on the outside of the heat exchange circulation tube, a cleaning brush is provided in the ring, a reduction motor is provided on the top of the heat exchange tank body, and the output shaft of the reduction motor is fixedly connected to the rotating shaft.

[0008] As a further improvement, the cleaning brush includes an annular frame coaxially installed in the ring, a plurality of brush head assemblies are evenly distributed on the inner side of the annular frame, a positioning plate extending outward is provided on one side of the annular frame, first transmission teeth are evenly distributed on the inner side of the positioning plate, a transmission rod is sleeved on the connecting rod, a second transmission tooth is provided on one side of the guide rail, a first gear meshing with the first transmission tooth is provided at one end of the transmission rod, and a second gear meshing with the second transmission tooth is provided at the other end.

[0009] As a further improvement, the brush head assembly includes a driving shaft distributed in a ring shape on the annular frame, a brush head is fixed to one end of the driving shaft facing the inner side of the annular frame, and a third gear is fixed to the other end, and the ring is provided with a third transmission tooth that cooperates with the third gear.

[0010] As a further improvement, the electrolytic cell body is provided with anode plates and cathode plates for electrolytic reaction, and the anode plates and cathode plates are arranged vertically alternately. A circulating liquid distributor connected to a circulating discharge pipe is provided at the top of the electrolytic cell body, and a plurality of circulating liquid discharge outlets are provided at the bottom of the circulating liquid distributor.

[0011] As a further improvement, the product discharge pipe is connected to a corresponding intermediate tank, and the intermediate tank is pumped to the feed end of the distillation device.

[0012] As a further improvement, a tail gas exhaust pipe is connected to the top of the electrolytic cell body.

[0013] As a further improvement, a nitrogen replacement pipe is connected to the left side of the electrolytic cell body, and the nitrogen replacement pipe is connected to an external nitrogen source.

[0014] A production method of perfluorotributylamine comprises the following specific steps: S, replacing air in an electrolytic cell body with nitrogen before reaction, replacing the air with nitrogen for preliminary mixing and preparing electrolyte in the electrolytic cell body; S2, preparing tributylamine and hydrogen fluoride in a mass ratio of 24-30kg:200-230kg, first adding hydrogen fluoride into the electrolytic cell body, and then adding tributylamine; S3, passing low-voltage current for electrolytic replacement reaction, the reaction pressure of the electrolytic cell is controlled at 0.1-1.5MP, and the temperature is controlled at 5-15°C; S5, after the electrolysis is completed, the tributylamine is electrolytically fluorinated and converted into perfluorotributylamine, and the material is discharged from the bottom of the electrolytic cell body to obtain the product perfluorotributylamine.

[0015] The beneficial effects of the present invention are: The present invention replaces the multi-pipe heat exchange tube with a single-pipe type, the flow path is relatively simple, the fluid flows in the same pipeline, the flow rate is relatively uniform, and the phenomenon of slow flow rate in some pipelines due to uneven flow distribution in the multi-pipe design is avoided, causing local siltation. At the same time, a spiral downward extension is adopted to make the product flow along the curve of the pipeline, increase the disturbance and turbulence of the fluid, and this disturbed flow helps to prevent the electrolysis product from being deposited on the inner wall of the pipeline, because turbulence can increase the shear force of the fluid, effectively wash away the sediment, avoid the accumulation of materials in the pipeline, and effectively ensure the uniformity and efficiency of heat exchange. The present invention is provided with a flow guide device, so that the refrigerant adopts a baffled flow mode in the heat exchange tank body, changes the flow direction of the refrigerant, and promotes the refrigerant to repeatedly contact the surface of the heat exchange circulation tube for many times, so that the residence time of the refrigerant in the heat exchanger is increased, so that there is more time for heat exchange with the heat exchange surface, further improves the efficiency of heat exchange, avoids uneven flow of the refrigerant, and ensures that the refrigerant flows evenly through the heat exchange tube in the heat exchanger. The present invention is provided with a cleaning mechanism, so that structural substances (such as dirt, grease, scaling, etc.) accumulated on the surface of the heat flow pipe in the refrigerant can be removed without stopping the machine, thereby ensuring heat exchange efficiency. BRIEF DESCRIPTION OF THE DRAWINGS In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for use in the embodiments will be briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without paying creative work.

[0016] Figure 1 This is a schematic structural diagram of a perfluorotributylamine production device capable of deep fluorination provided by the present invention; Figure 2 It is a structural schematic diagram of the heat exchange device provided by the present invention; Figure 3 is a schematic diagram of the structure of the heat exchange device provided by the present invention in a front cross-sectional view; Figure 4 is a schematic diagram of the structure of the heat exchange device provided by the present invention in a front cross-sectional view; Figure 5 It is a schematic diagram of the cross-sectional structure of the flow inlet and the flow discharger provided by the present invention when viewed from above; Figure 6 It is a structural schematic diagram of the cleaning mechanism provided by the present invention; Figure 7 It is a structural schematic diagram of the cleaning mechanism provided by the present invention; Figure 8 It is a schematic structural diagram of a cross-section of a connecting tube, a connecting rod, and a sleeve ring provided by the present invention; Fig. 9 It is a schematic structural diagram of a cross-section of a connecting tube, a connecting rod, and a sleeve ring provided by the present invention; Fig.10 It is a schematic diagram of the structure of the cleaning brush provided by the present invention; Fig.11 It is a schematic structural diagram of a partial cross-section of the cleaning mechanism provided by the present invention; Fig.12 It is a structural schematic diagram of the electrolytic cell body provided by the present invention.

[0017] In the figure: electrolytic cell body-1, mother liquid inlet pipe-2, heat exchange device-3, heat exchange tank body-31, circulating liquid conduit-32, circulating feed pipe-4, circulating discharge pipe-5, three-way valve-6, product discharge pipe-7, density meter-8, input pipe-321, output pipe-322, heat exchange circulation pipe-323, refrigerant feed pipe-33, refrigerant discharge pipe-34, flow guide device-35, inlet device-351, drain device-352, feed pump-353, cleaning mechanism-9, box body-354, first connecting port-355, second connecting port-356, diverter plate-357, filter screen-358, rotating shaft-91, connecting cylinder-92, transmission Moving screw-93, guide rail-94, guide column-95, connecting rod-96, collar-97, cleaning brush-98, reduction motor-99, ring frame-981, brush head assembly-982, positioning plate-983, first transmission tooth-984, transmission rod-985, second transmission tooth-986, first gear-987, second gear-988, drive shaft-9821, brush head-9822, third gear-9823, third transmission tooth-9824, anode plate-101, cathode plate-102, circulating liquid uniform distributor-103, circulating liquid discharge port-104, intermediate tank-10, exhaust gas exhaust pipe-11, nitrogen replacement pipe-12. DETAILED DESCRIPTION

[0018] In order to make the embodiments of the present invention, all belong to the scope of protection of the present invention. Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the invention claimed for protection, but merely represents the selected embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work belong to the scope of protection of the present invention.

[0019] In the description of the present invention, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as referring to the purpose, technical solutions and advantages of the methods. To be more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work indicate or imply relative importance or implicitly indicate the number of indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, the meaning of "multiple" is two or more, unless otherwise clearly and specifically defined.

[0020] The existing heat exchange pipeline adopts a multi-pipeline heat exchange method, which is easy to cause the electrolysis product to accumulate. In addition, during heat exchange, the refrigerant is usually injected from the top of the heat exchange tank and flows directly downward. Inside the heat exchange tank, the refrigerant may flow faster along certain channels and slower in other areas. There are dead zones in the heat exchange process. Due to uneven flow rate, some refrigerants may have a short contact time with the heat exchange tube when flowing through the heat exchange tube, and fail to fully absorb the heat of the tube wall, resulting in poor cooling effect and low heat exchange efficiency. In order to solve the above technical problems, this case proposes the following technical solutions: Reference Figures 1 to 12As shown, a perfluorotributylamine production device capable of deep fluorination, the structure of which includes: an electrolytic cell body 1, a mother liquid inlet pipe 2 is arranged outwardly on one side of the electrolytic cell body 1, and a heat exchange device 3 for circulating refrigeration of the material in the electrolytic cell body 1, the heat exchange device 3 includes a heat exchange tank body 31, a circulating liquid conduit 32 is arranged in the heat exchange tank body 31, one end of the circulating liquid conduit 32 is connected to the top of the heat exchange tank body 31 and is pumped to the bottom of the electrolytic cell body 1 through a circulating feed pipe 4, and the other end is connected to the bottom of the heat exchange tank body 31 and is connected to the bottom of the electrolytic cell body 1 through a circulating discharge pipe 5. The top of the heat exchange tank body 31 is connected to the product discharge pipe 7 through the three-way valve 6, and a densitometer 8 for detecting material density is installed at the bottom of the electrolytic cell body 1; the circulating liquid conduit 32 includes an input pipe 321 connected to the top of the heat exchange tank body 31, an output pipe 322 connected to the bottom of the heat exchange tank body 31, and a heat exchange circulation pipe 323 located in the heat exchange tank body 31 and connected between the input pipe 321 and the output pipe 322, and the heat exchange circulation pipe 323 extends downward in a spiral shape; a refrigerant feed pipe 33 is provided at the top of the left side of the heat exchange tank body 31, and a refrigerant discharge pipe 34 is provided at the bottom of the right side; The present invention replaces the multi-pipe heat exchange tube with a single-pipe type, the flow path is relatively simple, the fluid flows in the same pipe with a relatively uniform flow rate, and the phenomenon of slow flow rate in some pipes due to uneven flow distribution in the multi-pipe design, which causes local siltation, is avoided. At the same time, a spiral downward extension is adopted to make the product flow along the curve of the pipe, increasing the disturbance and turbulence of the fluid. This disturbed flow helps to prevent the electrolysis products from depositing on the inner wall of the pipe, because turbulence can increase the shear force of the fluid, effectively wash away the sediment, avoid the accumulation of substances in the pipe, and effectively ensure the uniformity and efficiency of heat exchange. The heat exchange tank 31 is provided with a plurality of groups of flow guide devices 35 connected to the heat exchange tank 31 on both sides, each group of flow guide devices 35 includes an inlet 351 and an outlet 352, and a feed pump 353 arranged between the inlet 351 and the outlet 352. The inlet end of the inlet 351 is connected to the heat exchange tank 31, and the outlet end is connected to the feed port of the feed pump 353. The inlet end of the outlet 352 is connected to the outlet of the feed pump 353. The outlet end is connected with the heat exchange tank body 31, and the inlet 351 of the uppermost flow guide device 35 on the right side is arranged correspondingly with the refrigerant feed pipe 33, the drain 352 on the right side is arranged correspondingly with the inlet 351 of the left flow guide device 35, the inlet 351 of the left flow guide device 35 is arranged correspondingly with the drain 352 of the right flow guide device 35, and the drain 352 of the lowermost flow guide device 35 on the left side is arranged correspondingly with the refrigerant discharge pipe 34; like Figure 4As shown, when in use, the refrigerant enters the heat exchange tank body 31 through the refrigerant feed pipe 33, and at the same time flows toward the inlet 351 of the right-hand guide device 35, and is transported to the discharger 352 by the feed pump 353, and finally returns to the heat exchange tank body 31, and flows toward the inlet 351 of the left-hand guide device 35, and is transported to the discharger 352 by the feed pump 353 of the left-hand guide device 35, and returns to the heat exchange tank body 31 again, and circulates in sequence until it is discharged from the discharger 352 at the bottom of the left side and then discharged outwardly through the refrigerant discharge pipe 34, so that the refrigerant adopts a baffled flow mode in the heat exchange tank body 31, changes the flow direction of the refrigerant, and promotes the refrigerant to repeatedly contact the surface of the heat exchange circulation tube 323 for multiple times, so that the residence time of the refrigerant in the heat exchanger is increased, so that there is more time for heat exchange with the heat exchange surface, further improves the efficiency of heat exchange, avoids uneven refrigerant flow, and ensures that the refrigerant flows evenly through the heat exchange tube in the heat exchanger.

[0021] Among them, the inlet 351 and the drain 352 both include a box body 354, the box body 354 is provided with a first connecting port 355 connected to the heat exchange tank body 31, and a second connecting port 356 connected to the feed pump 353. A plurality of diverter plates 357 extending from the first connecting port 355 to the second connecting port 356 are provided in the box body 354, and a filter screen 358 is provided on the first connecting port 355. When in use, the refrigerant of the inlet 351 enters the box body 354 through the first connecting port 355 from the heat exchange tank body 31 and quickly flows to the second connecting port 356 through the channel of the diverter plate 357, thereby entering the feed pump 353 to be transported to the drain 352, while the refrigerant of the drain 352 is transported to the second connecting port 356 through the feed pump 353, enters the box body 354, and quickly returns to the heat exchange tank body 31 toward the first connecting port 355 through the channel of the diverter plate 357. In order to ensure the cleanliness of the surface of the heat exchange circulation tube 323 and prevent the structural substances in the refrigerant (such as dirt, grease, scaling, etc.) from accumulating on the surface of the heat exchange circulation tube 323, a cleaning mechanism 9 is also included to clean the surface of the heat exchange circulation tube 323; the cleaning mechanism 9 is arranged in the heat exchange tank body 31. When the refrigerant enters the heat exchange tank body 31 through the refrigerant feed pipe 33 to cool the heat exchange circulation tube 323, the cleaning mechanism 9 moves up and down along the heat exchange circulation tube 323 to clean, thereby ensuring that the heat exchange efficiency is not affected and avoiding the reduction of heat transfer efficiency or equipment failure due to sediment accumulation.

[0022] The cleaning mechanism 9 includes a rotating shaft 91 coaxially arranged with the heat exchange circulation pipe 323, a connecting tube 92 is sleeved on the surface of the rotating shaft 91, a transmission screw 93 sleeved in the rotating shaft 91 is fixed in the heat exchange tank body 31, the transmission screw 93 is provided with a track corresponding to the spiral of the heat exchange circulation pipe 323, a vertically extending guide rail 94 is provided on the rotating shaft 91, a guide column 95 matching with the guide rail 94 and the track of the transmission screw 93 is provided on the inner side of the connecting tube 92, the connecting tube 92 is connected to the outside with a collar 97 through a connecting rod 96, the collar 97 is sleeved on the outside of the heat exchange circulation pipe 323, a cleaning brush 98 is provided in the collar 97, a reduction motor 99 is provided on the top of the heat exchange tank body 31, and the output shaft of the reduction motor 99 is fixedly connected to the rotating shaft 91; Therefore, when in use, the reduction motor 99 drives the rotating shaft 91 to rotate in the heat exchange tank body 31. At the same time, since the connecting tube 92 is slidably connected to the rotating shaft 91, and the guide column 95 on the connecting tube 92 cooperates with the guide rail 94 and the transmission screw 93 track respectively, when the rotating shaft 91 rotates, it drives the connecting tube 92 to move up and down along the heat exchange circulation tube 323 spirally. The connecting tube 92 drives the cleaning brush 98 on the ring 97 through the connecting rod 96 to remove dirt, oil stains, sediments and other impurities deposited on the surface of the heat exchange circulation tube 323, so as to avoid their accumulation on the surface of the pipeline, affecting the heat exchange effect, and avoiding the decrease in heat exchange efficiency due to dirt accumulation.

[0023] Furthermore, the cleaning brush 98 includes an annular frame 981 coaxially mounted in the collar 97, a plurality of brush head assemblies 982 are evenly distributed on the inner side of the annular frame 981, a positioning plate 983 extending outward is provided on one side of the annular frame 981, and first transmission teeth 984 are evenly distributed on the inner side of the positioning plate 983, a transmission rod 985 is sleeved on the connecting rod 96, a second transmission tooth 986 is provided on one side of the guide rail 94, and a first gear 987 meshing with the first transmission tooth 984 is provided at one end of the transmission rod 985, and a first gear 987 meshing with the first transmission tooth 984 is provided at the other end of the transmission rod 985. A second gear 988 meshing with the second transmission tooth 986 is provided at the end. Therefore, when in use, as the connecting tube 92 moves up and down along the rotating shaft 91, the second gear 988 cooperates with the second transmission tooth 986, thereby driving the transmission rod 985 and the first gear 987 to rotate, thereby prompting the first gear 987 to drive the positioning plate 983 to rotate in the ring 97 through the first transmission tooth 984, and the annular frame 981 drives the brush head assembly 982 to rotate around the surface of the heat exchange circulation tube 323, further improving the cleaning effect of the heat exchange circulation tube 323.

[0024] In addition, the brush head assembly 982 includes a driving shaft 9821 distributed in a ring shape on the annular frame 981, a brush head 9822 is fixed to one end of the driving shaft 9821 facing the inner side of the annular frame 981, and a third gear 9823 is fixed to the other end. The collar 97 is provided with a third transmission tooth 9824 cooperating with the third gear 9823. Therefore, as the annular frame 981 rotates in the collar 97, the third gear 9823 drives the driving shaft 9821 to rotate through the third transmission tooth 9824, prompting the brush head 9822 to rotate around the driving shaft 9821 for cleaning, and the surface of the heat exchange circulation tube 323 is cleaned through multiple rotation directions, thereby improving the thoroughness of cleaning and ensuring the cleaning effect.

[0025] The electrolytic cell body 1 is provided with an anode plate 101 and a cathode plate 102 for electrolysis reaction, and the anode plate 101 and the cathode plate 102 are arranged vertically alternately. A circulating liquid uniform distributor 103 connected to the circulating discharge pipe 5 is provided on the top of the electrolytic cell body 1, and a plurality of circulating liquid discharge ports 104 are provided at the bottom of the circulating liquid uniform distributor 103. By setting the circulating liquid uniform distributor 103, the surface of the plate can be flushed. Tar and the like generated during the electrolysis process will adhere to the surface of the plate, affecting the electrolysis. At the same time, the incompletely fluorinated products are fully contacted with the fluorine atoms generated by the electrolysis, so that the fluorination is more thorough and the reaction efficiency is improved.

[0026] The product discharge pipe 7 is connected to a corresponding intermediate tank 10, which is pumped to the feed end of the distillation equipment.

[0027] A tail gas exhaust pipe 11 is connected to the top of the electrolytic cell body 1 .

[0028] A nitrogen replacement pipe 12 is connected to the left side of the electrolytic cell body 1, and the nitrogen replacement pipe 12 is connected to an external nitrogen source.

[0029] A production method of perfluorotributylamine comprises the following specific steps: S1, before the reaction, the air in an electrolytic cell body 1 is replaced by nitrogen, and the air is replaced by nitrogen for preliminary mixing to prepare an electrolyte in the electrolytic cell body 1; S2, tributylamine and hydrogen fluoride are prepared in a mass ratio of 24-30kg:200-230kg, the hydrogen fluoride is first added to the electrolytic cell body 1, and then the tributylamine is added; S3, a low-voltage current is passed to carry out an electrolytic replacement reaction, and the reaction pressure of the electrolytic cell is controlled at 0.1-1.5MP and the temperature is controlled at 5-15°C; S5, after the electrolysis is completed, the tributylamine is electrolytically fluorinated and converted into perfluorotributylamine, and the material is discharged from the bottom of the electrolytic cell body 1 to obtain the product perfluorotributylamine.

[0030] The electrolytic cell body 1 in this embodiment adopts the electrolytic cell body 1 of the prior art, and its electrolysis means are also the prior art, so it will not be described in detail here, and the structure of the electrolytic cell body 1 will not be expanded in the figure. 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.

[0031] The method and the device can improve the fluorination degree in the reaction process, and obtain a crude perfluorotributylamine with a purity of more than 80% under the conditions of simple reaction raw materials and simple reaction devices.

[0032] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A perfluorotributylamine production device capable of deep fluorination, the structure of which comprises: An electrolytic cell body (1) is provided with a mother liquid inlet pipe (2) on one side of the electrolytic cell body (1) and a heat exchange device (3) for circulating and cooling the material in the electrolytic cell body (1), characterized in that: the heat exchange device (3) comprises a heat exchange tank body (31), a circulating liquid conduit (32) is provided in the heat exchange tank body (31), one end of the circulating liquid conduit (32) is connected to the top of the heat exchange tank body (31) and is pumped to the bottom of the electrolytic cell body (1) through a circulating feed pipe (4), and the other end is connected to the bottom of the heat exchange tank body (31) and is connected to the top of the bottom of the electrolytic cell body (1) through a circulating discharge pipe (5), and the circulating feed pipe (4) is connected to the bottom of the electrolytic cell body (1) through a three-way valve. (6) is connected to the outside with a product discharge pipe (7), and a densitometer (8) for detecting material density is installed at the bottom of the electrolytic cell body (1); the circulating liquid conduit (32) includes an input pipe (321) connected to the top of the heat exchange tank body (31), an output pipe (322) connected to the bottom of the heat exchange tank body (31), and a heat exchange circulation pipe (323) located in the heat exchange tank body (31) and connected between the input pipe (321) and the output pipe (322), and the heat exchange circulation pipe (323) extends downward in a spiral shape; a refrigerant feed pipe (33) is provided at the top of the left side of the heat exchange tank body (31), and a refrigerant discharge pipe (34) is provided at the bottom of the right side; the heat exchange tank body (31) is divided into two sides. A plurality of groups of flow guide devices (35) are provided which are connected to the heat exchange tank body (31). Each group of flow guide devices (35) includes a flow inlet (351) and a flow discharger (352), and a feed pump (353) arranged between the flow inlet (351) and the flow discharger (352). The inlet end of the flow inlet (351) is connected to the heat exchange tank body (31), and the outlet end is connected to the feed port of the feed pump (353). The inlet end of the flow discharger (352) is connected to the discharge port of the feed pump (353), and the outlet end is connected to the heat exchange tank body (31). The flow inlet (351) of the uppermost flow guide device (35) on the right side is arranged corresponding to the refrigerant feed pipe (33). The flow discharger (352) on the right side is connected to the feed port of the feed pump (353). The heat exchange tank body (31) is provided with a heat exchanger (323) and a cooling medium (323) disposed on the heat exchange tank body (31). The heat exchanger (323) is provided with a cooling medium (323) and a cooling medium (323) disposed on the heat exchange tank body (31). The cooling medium ...

2. A perfluorotributylamine production device capable of deep fluorination as claimed in claim 1, characterized in that: The inlet (351) and the outlet (352) both comprise a box body (354); the box body (354) is provided with a first connecting port (355) connected to the heat exchange tank body (31); the box body (354) is provided with a second connecting port (356) connected to the feed pump (353); a plurality of flow dividers (357) extending from the first connecting port (355) to the second connecting port (356) are provided in the box body (354); and a filter screen (358) is provided on the first connecting port (355).

3. A perfluorotributylamine production device capable of deep fluorination as claimed in claim 1 or 2, characterized in that: The cleaning mechanism (9) comprises a rotating shaft (91) coaxially arranged with the heat exchange circulation tube (323); a connecting tube (92) is sleeved on the surface of the rotating shaft (91); a transmission screw (93) sleeved in the rotating shaft (91) is fixed in the heat exchange tank body (31); a track corresponding to the spiral of the heat exchange circulation tube (323) is provided on the transmission screw (93); a guide rail (94) extending vertically is provided on the rotating shaft (91); a guide column (95) cooperating with the guide rail (94) and the track of the transmission screw (93) is provided on the inner side of the connecting tube (92); a sleeve ring (97) is connected to the outside of the connecting tube (92) through a connecting rod (96); the sleeve ring (97) is sleeved on the outer side of the heat exchange circulation tube (323); a cleaning brush (98) is provided in the sleeve ring (97); a reduction motor (99) is provided on the top of the heat exchange tank body (31); an output shaft of the reduction motor (99) is fixedly connected to the rotating shaft (91).

4. A perfluorotributylamine production device capable of deep fluorination as claimed in claim 3, characterized in that: The cleaning brush (98) comprises an annular frame (981) coaxially mounted inside a collar (97), a plurality of brush head assemblies (982) being evenly distributed inside the annular frame (981), a positioning plate (983) extending outwardly being provided on one side of the annular frame (981), first transmission teeth (984) being evenly distributed on the inner side of the positioning plate (983), a transmission rod (985) being sleeved on the connecting rod (96), a second transmission tooth (986) being provided on one side of the guide rail (94), a first gear (987) meshing with the first transmission tooth (984) being provided at one end of the transmission rod (985), and a second gear (988) meshing with the second transmission tooth (986) being provided at the other end of the transmission rod (985).

5. A perfluorotributylamine production device capable of deep fluorination as claimed in claim 4, characterized in that: The brush head assembly (982) comprises a driving shaft (9821) distributed in an annular shape on the annular frame (981); a brush head (9822) is fixed to one end of the driving shaft (9821) facing the inner side of the annular frame (981); a third gear (9823) is fixed to the other end; and the collar (97) is provided with a third transmission tooth (9824) cooperating with the third gear (9823).

6. A perfluorotributylamine production device capable of deep fluorination as claimed in claim 1, characterized in that: The electrolytic cell body (1) is provided with an anode plate (101) and a cathode plate (102) for electrolytic reaction, wherein the anode plate (101) and the cathode plate (102) are arranged vertically and alternately, and a circulating liquid uniform distributor (103) connected to a circulating discharge pipe (5) is provided at the top of the electrolytic cell body (1), and a plurality of circulating liquid discharge ports (104) are provided at the bottom of the circulating liquid uniform distributor (103).

7. A perfluorotributylamine production device capable of deep fluorination as claimed in claim 1, characterized in that: The product discharge pipe (7) is connected to a corresponding intermediate tank (10), which is pumped to the feed end of the distillation equipment.

8. A perfluorotributylamine production device capable of deep fluorination as claimed in claim 1, characterized in that: The top of the electrolytic cell body (1) is connected to a tail gas exhaust pipe (11).

9. A perfluorotributylamine production device capable of deep fluorination as claimed in claim 1, characterized in that: A nitrogen replacement pipe (12) is connected to the left side of the electrolytic cell body (1), and the nitrogen replacement pipe (12) is connected to an external nitrogen source.

10. A method for producing perfluorotributylamine, based on the perfluorotributylamine production device capable of deep fluorination as claimed in any one of claims 1 to 9, characterized in that: The method comprises the following specific steps: S1, replacing air in the electrolytic cell body (1) with nitrogen before the reaction, and preliminarily mixing the replaced air with nitrogen to prepare an electrolyte in the electrolytic cell body (1); S2, preparing tributylamine and hydrogen fluoride in a mass ratio of 24-30 kg:200-230 kg, respectively, first adding hydrogen fluoride to the electrolytic cell body (1), and then adding tributylamine; S3, passing a low-voltage current to carry out an electrolytic replacement reaction, wherein the reaction pressure of the electrolytic cell is controlled at 0.1-1.5 MPa and the temperature is controlled at 5-15°C; S5, after the electrolysis is completed, the tributylamine is electrolytically fluorinated and converted into perfluorotributylamine, and the material is discharged from the bottom of the electrolytic cell body (1) to obtain the product perfluorotributylamine.

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