An automatic liquid replenishment continuous production device and process for perfluorotripropylamine

Abstract

The invention relates to an automatic liquid replenishment continuous production device and process for perfluorotripropylamine, belonging to the field of perfluorotripropylamine preparation and fluid working system. An electrolytic component adopts an electrolytic fluorination method, cooperates with a water circulation component, an automatic liquid replenishment component and a liquid density detection component to work together, monitors the liquid level of the electrolytic component through a liquid level monitor to detect the liquid level for liquid replenishment, detects the solution density at the liquid inlet and liquid outlet of the electrolytic component through a density detector to judge whether the electrolysis is completed, and after complete electrolysis, the solution is concentratedly recovered through an intermediate cylinder, and the electrolytic component performs liquid replenishment and continuous operation, and the crude perfluorotripropylamine in the intermediate cylinder is discharged for double distillation recovery and distillation purification, thereby realizing efficient and high-purity industrial production of perfluorotripropylamine.

Description

Technical Field

[0001] The invention belongs to the technical field of perfluorotripropylamine preparation and fluid working system, and specifically relates to an automatic liquid replenishment continuous production device and process for perfluorotripropylamine. Background Art

[0002] Perfluorotripropylamine 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. Perfluorotripropylamine 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 acetone, ether, chloroform, dioxane, ethyl acetate, benzene and petroleum ether is also very small, but it can be miscible with chlorofluoroalkanes. Perfluorotripropylamine 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 perfluorotripropylamine is of great significance to the country's scientific progress and development. The most widely used technology for preparing perfluorotripropylamine is the electrolytic fluorination method. Low-voltage direct current is passed through tripropylamine and hydrogen fluoride in an electrolytic cell to generate free fluorine atoms to directly replace hydrogen atoms in tripropylamine, and then the perfluorotripropylamine product is obtained through simple purification. However, this method still has the following disadvantages: the reaction process is intermittent, the reaction stops when discharging, and the efficiency is low; the product and the mother liquor are separated due to different densities, the discharging process cannot be accurately quantified, and the process is unreasonable; the loss of hydrogen fluoride is large; the risk factor is high, etc. In view of this, the present scheme was created. Summary of the invention

[0003] In view of the deficiencies of the prior art, the technical problem to be solved by the present invention is to provide an automatic liquid replenishment continuous production device and process for perfluorotripropylamine, which can produce high-purity perfluorotripropylamine.

[0004] In order to solve the above technical problems, the technical solution adopted by the present invention is: an automatic liquid replenishment continuous production device for perfluorotripropylamine, comprising an electrolytic component, a water circulation component, an automatic detection liquid replenishment component and a liquid density detection component; the electrolytic component has a liquid inlet, a liquid outlet and a mother liquid inlet;

[0005] The automatic detection of liquid replenishment includes a liquid level detector and a mother liquid driver, wherein the liquid level detector is used to detect the liquid level in the electrolytic component, and the mother liquid driver is used to drive the mother liquid to be replenished into the electrolytic component;

[0006] The water circulation assembly includes two pump bodies, an intermediate cylinder and a circulation pipeline, wherein the intermediate cylinder is connected to the circulation pipeline, and the two ends of the circulation pipeline are respectively connected to the liquid inlet and the liquid outlet of the electrolytic assembly, and the two pump bodies are connected to the circulation pipeline and are located at the two ends of the circulation pipeline; one of the liquid density detection assemblies is located between the liquid outlet of the electrolytic assembly and one of the pump bodies, and the other liquid density detection assembly is located between the liquid inlet of the electrolytic assembly and the other pump body;

[0007] The liquid density detection assembly includes a density detector, a liquid pumping cylinder and a detection body, wherein the detection body has a volume cavity, the detection body is connected to the circulation pipeline through a shunt pipe, the liquid pumping cylinder is used to pump liquid from the shunt pipe into or out of the volume cavity, and the density detector is used to detect the density of the liquid in the volume cavity;

[0008] The liquid passes through the electrolysis component, the circulation pipeline, the intermediate cylinder, the circulation pipeline and the electrolysis component in sequence for circulation electrolysis and the liquid fills the shunt tube.

[0009] Furthermore, the density detector uses a gravity sensor or an ultrasonic sensor for detection.

[0010] Furthermore, the detection body and the volume cavity are prismatic, the detection body is made of glass, a pull-out block is provided at the output end of the liquid pumping cylinder, the pull-out block is adapted to and sealed with the volume cavity, the ultrasonic sensor includes a transmitter and a receiver, the transmitter and the receiver are respectively fixed on two corresponding side walls of the detection body, and the transmitting end of the transmitter and the receiving end of the receiver are facing each other.

[0011] Furthermore, the electrolytic assembly includes an electrolytic cell, a cover body and a plurality of electrolytic plate kits, the cover body is sealed over the electrolytic cell, the electrolytic cell has a reaction chamber, the cover body has a liquid inlet chamber, adjacent reaction chambers and between the liquid inlet chamber and the reaction chamber are blocked by a blocking plate, the blocking plate has a liquid inlet hole; the plurality of electrolytic plate kits are located in the reaction chamber and are spaced apart on the left and right.

[0012] 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 multiple lower openings of the liquid holes correspond to the upper openings of the multiple liquid inlet channels respectively; the multiple upper openings of the liquid holes correspond to the lower openings of the multiple liquid inlets respectively, and a sealing plate is formed on the lower surface of the cover frame, and the sealing plate is located on both sides of the multiple liquid holes, and the sealing plate is used to close the sides of the multiple reaction plates.

[0013] 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.

[0014] An automatic liquid replenishment continuous production process of perfluorotripropylamine adopts an automatic liquid replenishment continuous production device of perfluorotripropylamine for production, comprising the following steps:

[0015] S1. Replace the air in the electrolytic component with nitrogen, mix hydrogen fluoride and tripropylamine into a mother liquid and inject it into the electrolytic component, so that the mother liquid fills 60%-80% of the total volume of the intermediate cylinder and the inner cavity of the electrolytic component;

[0016] S2. The electrolytic component is passed through a low-voltage current to perform an electrolytic replacement reaction. The reaction pressure is normal pressure and the temperature is controlled at 0-5°C. The mother liquid in the electrolytic component is controlled to account for 70%-80% of the total volume of the inner cavity of the electrolytic component through the input and output of two pump bodies;

[0017] S3. During the electrolysis process, the reaction pressure is adjusted to 0.01MPa-0.03MPa, and the electrolysis current is gradually increased;

[0018] S4. After 5-10 days of electrolysis, two liquid density detection components detect the liquid density at the liquid inlet and liquid outlet of the electrolysis component. Starting from the 5th day of electrolysis, the two liquid density detection components are tested twice a day until the detection values ​​of the two liquid density detection components reach or exceed the predetermined value, and the error of the detection values ​​of the two liquid density detection components is less than 0.2kg / m³;

[0019] S5. After the electrolysis is completed, the crude perfluorotripropylamine in the circulation pipeline, the intermediate cylinder and the electrolysis assembly is discharged;

[0020] S6. When the liquid level detector detects that the liquid in the electrolytic component is lower than the rated value, the valve between the intermediate cylinder and the electrolytic component is closed, and liquid is automatically added to the electrolytic component. After the crude perfluorotripropylamine in the intermediate cylinder is completely discharged, the valve between the intermediate cylinder and the electrolytic component is opened for the next liquid replenishment electrolysis.

[0021] Furthermore, the mass ratio of tripropylamine to hydrogen fluoride in step S1 is 20-30kg:200-240kg.

[0022] Furthermore, in step S3, the electrolysis current is gradually increased to 500A-600A.

[0023] Furthermore, in steps S5 and S6, the crude perfluorotripropylamine is discharged into a double distillation device for distillation.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] 1. The present invention provides an automatic liquid replenishment continuous production device and process for perfluorotripropylamine. The method comprises the following steps: firstly, tripropylamine and hydrogen fluoride are prepared into a mother liquid in a mass ratio of 22-30kg:200-230kg, and then the mother liquid is pumped into an electrolytic component, wherein the mother liquid fills 60%-80% of the sum of the volume of the intermediate cylinder and the inner cavity of the electrolytic component; before the reaction, the air in the electrolytic component is replaced with nitrogen, and after the reaction, a low-voltage current is passed to perform an electrolytic replacement reaction, wherein the reaction pressure is normal pressure and the temperature is controlled at 0-5°C; the mother liquid is transported toward the intermediate cylinder by a pump body at a liquid outlet of the electrolytic component, and the mother liquid is transported toward the electrolytic component by a pump body at a liquid inlet of the electrolytic component, so as to realize an electrolytic cycle; after 5-10 days of electrolysis, two liquid density detection components detect the liquid density of the electrolytic component. The liquid density at the liquid inlet and the liquid outlet, specifically, after 5 days of electrolysis, the two liquid density tests are performed twice a day until the detection values ​​of the two liquid density detection components reach or exceed the predetermined value, and the detection value error of the two liquid density detection components is less than 0.2kg / m³, and then the electrolytic component starts to infuse liquid into the intermediate cylinder, and the intermediate cylinder starts to discharge liquid. When the liquid level detector detects that the liquid in the electrolytic component is lower than the rated value, the valve between the intermediate cylinder and the electrolytic component is closed, and liquid is automatically added to the electrolytic component. After the crude perfluorotripropylamine in the intermediate cylinder is completely discharged, the valve between the intermediate cylinder and the electrolytic component is opened for the next electrolytic cycle. Through the above-mentioned device and process, automatic discharging can be achieved without affecting the electrolytic reaction.

[0026] 2. After the crude product of perfluorotripropylamine is produced in the present invention, secondary distillation is performed, and the light components are collected and reused to reduce the loss of raw materials.

[0027] 3. In order to flush away the tar attached to the surface of the electrode plate produced during the electrolysis process, the mother liquor of this scheme will be pressurized when entering from the liquid inlet of the partition, 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 mother liquor will rush into the liquid inlet channel at a faster speed. This impact force can flush out the tar on the surface of the anode plate and the cathode plate. Since the bottom of the liquid inlet channel is connected to the reaction chamber of the electrolytic cell, the mother liquor enters the liquid inlet channel and flows out to both sides. Therefore, the speed at which the mother liquor enters the liquid inlet channel tends to gradually decrease, which may lead to incomplete cleaning of the tar attached to the bottom of the anode plate and the cathode plate. Therefore, a cover frame is set to close the top of multiple liquid inlet channels, and the side of the liquid channel is closed by the sealing plate on the cover plate, so that the mother liquid flowing into the liquid inlet channel can maintain a relatively constant speed to flush the surface of the electrode plate. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 This is a schematic diagram of the principle structure of an automatic liquid replenishment continuous production device for perfluorotripropylamine of the present invention;

[0029] Figure 2It is a schematic diagram of the principle structure of the double distillation device in the present invention;

[0030] Figure 3 It is a schematic diagram of the three-dimensional structure of the electrolytic component in the present invention;

[0031] Figure 4 It is a schematic diagram of the split structure of the electrolytic component in the present invention;

[0032] Figure 5 It is a schematic diagram of the split structure of the electrolytic component in another direction of the present invention;

[0033] Figure 6 It is a schematic cross-sectional view of the electrolytic component in the present invention;

[0034] Figure 7 It is a schematic cross-sectional view of the electrolytic component in another direction of the present invention;

[0035] Figure 8 It is a partial cross-sectional enlarged structural schematic diagram of the cover frame position in the present invention;

[0036] Fig. 9 It is a schematic diagram of the three-dimensional structure of the partition in the present invention;

[0037] Fig.10 It is a schematic diagram of the three-dimensional structure of the electrolytic cell in the present invention;

[0038] Fig.11 It is a schematic diagram of the three-dimensional structure of the electrolytic plate set in the present invention;

[0039] Fig.12 It is a schematic cross-sectional view of the electrolytic plate set in the present invention;

[0040] Fig.13 It is a schematic diagram of the side view structure of the electrolytic plate kit of the present invention after the sealing plate is hidden;

[0041] Fig.14 It is a schematic diagram of the top view of the liquid density detection assembly in the present invention;

[0042] Fig.15 It is a schematic diagram of the three-dimensional structure of the liquid density detection component in the present invention;

[0043] Fig.16 It is a schematic cross-sectional structural diagram of the liquid density detection component in the present invention.

[0044] Markings in the figure: 1. electrolytic assembly; 11. electrolytic cell; 111. reaction chamber; 12. cover body; 121. liquid inlet chamber; 13. electrolytic plate kit; 131. fixing column; 132. reaction plate; 1321. anode plate; 1322. cathode plate; 1323. liquid inlet channel; 133. left fixing plate; 134. right fixing plate; 135. middle plate; 136. power supply column; 137. cover frame; 1371. liquid through hole; 1372. sealing plate; 14. partition; 141. liquid inlet hole; 2. automatic detection and liquid replenishment assembly; 3. water circulation assembly; 31. pump body; 32. middle cylinder; 33. circulation pipeline; 331. first pipeline; 3311. first solenoid valve; 332. second pipeline; 3321. second solenoid valve; 333. third pipeline; 334. fourth pipeline; 3341. third solenoid valve; 4. liquid density detection assembly; 41. density detector; 411. transmitter; 412. receiver; 42. liquid extraction cylinder; 421. extraction block; 43. detection body; 431. diverter; 5. double distillation device; 51. transition cylinder; 52. first distillation tower; 53. first recovery tower; 54. first tail gas treatment tower; 55. second distillation tower; 56. finished liquid integration tower; 57. second tail gas treatment tower. DETAILED DESCRIPTION

[0045] 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.

[0046] Example 1

[0047] like Figure 1-16 As shown in the figure, this embodiment provides an automatic liquid replenishment continuous production device for perfluorotripropylamine, including an electrolysis component 1, a water circulation component 3, an automatic detection liquid replenishment component 2 and a liquid density detection component 4.

[0048] like Figure 3-Figure 13As shown, the electrolytic assembly 1 includes an electrolytic cell 11, a cover body 12, a fixing column 131, and two electrolytic plate kits 13. A reaction chamber 111 is arranged in the electrolytic cell 11. The reaction chamber 111 of the electrolytic cell 11 has upper and lower openings. The cover body 12 is sealed and covered on the top of the 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 of 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 chamber 121. The reaction chamber 111 of the electrolytic cell 11 is surrounded by the inner wall of the electrolytic cell 11 and the partition 14. The bottom of the reaction chamber 111 is an arc-shaped bottom or a conical bottom. The present scheme adopts an arc-shaped bottom, and the bottom of the reaction chamber 111 is an arc-shaped bottom or a conical bottom, so that the products generated by electrolysis can be fully circulated. A first densitometer for measuring the nitrogen density in the reaction area is arranged in the middle of the circumference of the electrolytic cell 11. A nitrogen inlet and a mother liquid inlet are also arranged on the side wall of the electrolytic cell 11. Specifically, the automatic detection of liquid replenishment includes a liquid level detector and a mother liquid driving body. The liquid level detector is used to detect the liquid level in the electrolytic component 1, and the mother liquid driving body is used to drive the mother liquid to be replenished into the electrolytic cell 11 from the mother liquid inlet. The mother liquid driving body is driven by a liquid pump plus electronic control.

[0049] like Figure 11-13 As shown, 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] like Fig.13As shown, the reaction plate 132 includes an anode plate 1321, a cathode plate 1322 and an ion membrane, the ion membrane 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 and the number of the electrolytic plate set 13 and the volume of the reaction chamber 111. Figure 8 , Figure 11-Figure 12 As shown, the cover frame 137 is covered on the multiple groups of reaction plates 132, and a plurality of strip-shaped liquid holes 1371 are formed on the cover frame 137. The lower openings of the plurality of liquid holes 1371 correspond to the upper openings of the plurality of liquid inlet channels 1323. Specifically, the upper surface of the cover frame 137 is in contact with the lower surface of the partition 14. The partition 14 is provided with a plurality of liquid inlet holes 141. The positions and numbers of the liquid inlet holes 141 correspond to the liquid inlet holes 1371. The upper opening of the liquid inlet is formed with The upper opening of the liquid hole 1371 is provided with a V-shaped expansion, and the vertical cross-section of the lower opening of the liquid hole 1371 is arc-shaped, that is, an arc-shaped opening. The lower opening of the liquid hole 1371 covers the upper opening of the liquid inlet channel 1323. The cover frame 137 is made of insulating material. Sealing plates 1372 are formed on both sides of the lower surface of the cover frame 137. The sealing plates 1372 are located on both sides of the multiple liquid holes 1371. The sealing plates 1372 are used to close the sides of the multiple reaction plates 132. In the present embodiment, the cover frame 137 is made of plastic, and a liquid inlet hole 141 and a liquid passage 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. Since the bottom of the liquid inlet channel 1323 is connected to the reaction chamber 111 of the electrolytic cell 11, the mother liquid enters the liquid inlet channel 1323 and flows out to both sides, so the speed at which the mother liquid enters the liquid inlet channel 1323 tends to gradually decrease, which may lead to incomplete cleaning of tar adhesion under the anode plate 1321 and the cathode plate 1322. Therefore, the cover frame 137 is provided to close the top of multiple liquid inlet channels 1323, and the side of the liquid passage is closed by the sealing plate 1372 on the cover plate, so that the mother liquid flowing into the liquid inlet channel 1323 can maintain a relatively constant speed to flush the surface of the electrode plate.

[0051] The water circulation assembly 3 includes two pump bodies 31, an intermediate cylinder 32 and a circulation pipeline 33. The intermediate cylinder 32 is connected to the circulation pipeline 33. The two ends of the circulation pipeline 33 are respectively connected to the liquid inlet and the liquid outlet of the electrolytic assembly 1. The two pump bodies 31 are connected to the circulation pipeline 33 and are located at the two ends of the circulation pipeline 33. Specifically, the circulation pipeline 33 includes a first pipeline 331, a first solenoid valve 3311, a second pipeline 332, a second solenoid valve 3321, a third pipeline 333, a fourth pipeline 334 and a third solenoid valve 3341 The first solenoid valve 3311 is connected to the first pipeline 331, and the first pipeline 331 is respectively connected to the liquid outlet of the electrolytic cell 11 and the pump body 31. The second solenoid valve 3321 is connected to the second pipeline 332, and the first pipeline 331 is respectively connected to the inlet of the intermediate cylinder 32 and the pump body 31. The third pipeline 333 is respectively connected to the outlet of the intermediate cylinder 32 and the pump body 31. The third solenoid valve 3341 is connected to the fourth pipeline 334, and the fourth pipeline 334 is respectively connected to the liquid inlet of the electrolytic cell 11 and the pump body 31.

[0052] One liquid density detection component 4 is located between the liquid outlet of the electrolytic component 1 and one pump body 31, specifically, it is arranged on the first pipeline 331, and the other liquid density detection component 4 is located between the liquid inlet of the electrolytic component 1 and the other pump body 31, specifically, it is arranged on the fourth pipeline 334.

[0053] like Figure 14-16 As shown, the liquid density detection assembly 4 includes a density detector 41, a liquid pumping cylinder 42 and a detection body 43. The detection body 43 has a volume cavity. The detection body 43 is connected to the circulation pipeline 33 through a shunt pipe 431. The liquid pumping cylinder 42 is used to pump liquid into or out of the volume cavity from the shunt pipe 431. The density detector 41 is used to detect the density of the liquid in the volume cavity; the density detector 41 uses a gravity sensor or an ultrasonic sensor for detection. In this embodiment, the density detector 41 uses an ultrasonic sensor for measurement. The detection body 43 and the volume cavity are prismatic, the detection body 43 is made of glass, and the output end of the liquid pumping cylinder 42 is provided with a A pull-out block 421 is provided, and the pull-out block 421 is adapted to the volume cavity and is sealed and connected. The ultrasonic sensor includes a transmitter 411 and a receiver, and the transmitter 411 and the receiver are respectively fixedly arranged on two corresponding side walls of the detection body 43. The transmitting end of the transmitter 411 and the receiving end of the receiver face each other. According to the relationship between the speed of sound and the density, the formula C*C*ρ=K, C is the speed of ultrasonic wave propagation in liquid, ρ is the density of liquid, K is the compression coefficient, and the density is: The speed of sound can be calculated by measuring the time of ultrasonic wave propagation in liquid and the known distance (the distance between the transmitter 411 and the receiver 412). Then, the above formula can be used to obtain K / C*C=ρ, and the density of the liquid can be calculated.

[0054] like Figure 2As shown, the present application also proposes a double distillation device, which includes a transition tube 51, a first distillation tower 52, a first recovery tower 53, a first tail gas treatment tower 54, a second distillation tower 55, a finished liquid integration tower 56 and a second tail gas treatment tower 57; the transition tube 51 is connected to the intermediate tube 32, and the transition tube 51 draws the crude perfluorotripropylamine into the first distillation tower 52, and the first distillation tower 52 is distilled and then discharged into the second distillation tower 55, and high-purity perfluorotripropylamine can be obtained after distillation in the second distillation tower 55; the first recovery tower 53 and the first tail gas treatment tower 54 are connected to each other. The first recovery tower 53 and the first tail gas treatment tower 54 are connected to the first distillation tower 52. The first tail gas treatment tower 54 is used to treat the tail gas generated during the operation of the first recovery tower 53 and the first distillation tower 52. The first recovery tower 53 is used to recover light components. The finished liquid integration tower 56 is connected to the second distillation tower 55 and the second tail gas treatment tower 57. The finished liquid integration tower 56 is used to collect high-purity perfluorotripropylamine and then discharge it. The connection method and function of the second distillation tower 55 and the second tail gas treatment tower 57 are the same as those of the first distillation tower 52 and the first tail gas treatment tower 54, which will not be repeated here.

[0055] This embodiment also provides an automatic liquid replenishment continuous production process of perfluorotripropylamine, which adopts an automatic liquid replenishment continuous production device of perfluorotripropylamine for production, and includes the following steps:

[0056] S1. Replace the air in the electrolytic component 1 with nitrogen, and mix hydrogen fluoride and tripropylamine into a mother liquid and inject it into the electrolytic component 1, so that the mother liquid fills 60%-80% of the sum of the volumes of the intermediate cylinder 32 and the inner cavity of the electrolytic component 1; the mass ratio of tripropylamine to hydrogen fluoride in step S1 is 20kg:200kg, and the specific steps are as follows: After the air in the electrolytic cell 11 is replaced with nitrogen, the pump body 31 located on the liquid outlet side of the electrolytic cell 11 starts to operate, and the mother liquid is pumped into the intermediate cylinder 32, and the pump body 31 located on the liquid inlet side of the electrolytic cell 11 starts to operate, and the mother liquid is pumped from the intermediate cylinder 32 into the electrolytic cell 11, until the mother liquid fills 70% of the volume of the inner cavity of the electrolytic cell 11 and 80% of the volume of the intermediate cylinder 32.

[0057] S2, the electrolytic component 1 is passed through a low-voltage current to perform an electrolytic substitution reaction, the reaction pressure is normal pressure and the temperature is controlled at 0-5°C, and the mother liquid in the electrolytic component 1 is controlled to account for 70%-80% of the total volume of the inner cavity of the electrolytic component 1 through the input and output of the two pump bodies 31. The specific steps are: through the operation of the two pump bodies 31, the mother liquid is circulated in the electrolytic cell 11, the circulation pipeline 33 and the intermediate cylinder 32 to achieve circulating electrolysis. When the mother liquid enters the electrolytic cell 11, the mother liquid is circulated in the circulation pipeline 33 and the intermediate cylinder 32. The path is as follows: the mother liquor flows in from the liquid inlet of the partition 14, the mother liquor 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 mother liquor in the liquid hole 1371 rushes into the liquid inlet channel 1323 to flush the surface of the anode plate 1321 and the cathode plate 1322, and flushes away the tar on the surface (the anode plate 1321 and the cathode plate 1322 will produce tar attached during the electrolysis process).

[0058] S3. During the electrolysis process, the reaction pressure is adjusted to 0.01MPa-0.03MPa, and the electrolysis current is gradually increased; the electrolysis current is increased to 500A.

[0059] S4. After 7 days of electrolysis, the two liquid density detection components 4 detect the liquid density at the liquid inlet and liquid outlet of the electrolysis component 1. Starting from the 5th day of electrolysis, the two liquid density detections are performed twice a day until the detection values ​​of the two liquid density detection components 4 reach or exceed the predetermined value, and the detection value error of the two liquid density detection components 4 is less than 0.2kg / m³.

[0060] S5. After the electrolysis is completed, the crude perfluorotripropylamine in the circulation pipeline 33, the intermediate cylinder 32 and the electrolysis assembly 1 is discharged; the specific steps are as follows: the crude perfluorotripropylamine in the intermediate cylinder 32 is discharged into the transition cylinder 51.

[0061] S6. When the liquid level detector detects that the liquid in the electrolytic component 1 is lower than the rated value, the valve between the intermediate cylinder 32 and the electrolytic component 1 is closed, and liquid is automatically added to the electrolytic component 1. After the crude perfluorotripropylamine in the intermediate cylinder 32 is completely discharged, the valve between the intermediate cylinder 32 and the electrolytic component 1 is opened, and steps S1-S6 are repeated. When repeating step S1, there is no need to replace the ammonia in the electrolytic cell 11.

[0062] Preferably, in step S51, the crude perfluorotripropylamine is discharged from the transition tube 51 into the first distillation tower 52 for distillation, and after the distillation is completed, it is discharged into the second distillation tower 55 for distillation, and high-purity perfluorotripropylamine is obtained after double distillation.

[0063] Specifically, in step S51, the first recovery tower 53 is used to recover and process the waste liquid after distillation in the first distillation tower 52, the finished liquid integration tower 56 is used to collect high-purity perfluorotripropylamine, and the waste liquid in the second distillation tower 55 is directly discharged and recycled.

[0064] Finally, 62 kg of high-purity perfluorotripropylamine was obtained, 3.6 kg of light components and 7.3 kg of heavy components were recovered, and the purity of perfluorotripropylamine analyzed by GC-MS was 99.6%.

[0065] Example 2

[0066] The difference between this embodiment and embodiment 1 is that 25 kg of tripropylamine and 230 kg of anhydrous hydrogen fluoride are prepared into a mother liquor, the electrolysis current in step S3 is increased to 600 A, and the electrolysis time is 6 days, 53 L of crude perfluorotripropylamine can be obtained, and the crude product is distilled in a distillation device to obtain 78.3 kg of high-purity perfluorotripropylamine, 3.7 kg of light components and 9.0 kg of heavy components are recovered, and the purity of perfluorotripropylamine analyzed by GC-MS is 99.5%.

[0067] Example 3

[0068] The difference between this embodiment and embodiment 1 is that 28 kg of tripropylamine and 240 kg of anhydrous hydrogen fluoride are prepared into a mother liquor, the electrolysis current in step S3 is increased to 500 A, the electrolysis time is 9 days, 59 L of crude perfluorotripropylamine can be obtained, and the crude product is distilled in a distillation device to obtain 87.7 kg of high-purity perfluorotripropylamine, 5.0 kg of light components and 9.1 kg of heavy components are recovered, and the purity of perfluorotripropylamine analyzed by GC-MS is 99.7%.

[0069] 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. An automatic liquid replenishment continuous production device for perfluorotripropylamine, characterized in that: It includes an electrolytic component, a water circulation component, an automatic detection and liquid replenishment component and a liquid density detection component; the electrolytic component has a liquid inlet, a liquid outlet and a mother liquid inlet; the automatic detection and liquid replenishment includes a liquid level detector and a mother liquid driver, the liquid level detector is used to detect the liquid level in the electrolytic component, and the mother liquid driver is used to drive the mother liquid to be replenished into the electrolytic component; The water circulation assembly comprises two pump bodies, an intermediate cylinder and a circulation pipeline, wherein the intermediate cylinder is connected to the circulation pipeline, and the two ends of the circulation pipeline are respectively connected to the liquid inlet and the liquid outlet of the electrolytic assembly, and the two pump bodies are connected to the circulation pipeline and are located at the two ends of the circulation pipeline; one of the liquid density detection assemblies is located between the liquid outlet of the electrolytic assembly and one of the pump bodies, and the other of the liquid density detection assemblies is located between the liquid inlet of the electrolytic assembly and the other pump body; The liquid density detection assembly includes a density detector, a liquid pumping cylinder and a detection body, wherein the detection body has a volume cavity, the detection body is connected to the circulation pipeline through a shunt pipe, the liquid pumping cylinder is used to pump liquid from the shunt pipe into or out of the volume cavity, and the density detector is used to detect the density of the liquid in the volume cavity; The liquid passes through the electrolysis component, the circulation pipeline, the intermediate cylinder, the circulation pipeline and the electrolysis component in sequence for circulation electrolysis and the liquid fills the shunt tube.

2. The automatic liquid replenishment continuous production device of perfluorotripropylamine according to claim 1, characterized in that: The density detector uses a gravity sensor or an ultrasonic sensor for detection.

3. The automatic liquid replenishment continuous production device of perfluorotripropylamine according to claim 2, characterized in that: The detection body and the volume cavity are prismatic, the detection body is made of glass, a pull-out block is provided at the output end of the liquid pumping cylinder, the pull-out block is adapted to and sealed with the volume cavity, the ultrasonic sensor comprises a transmitter and a receiver, the transmitter and the receiver are respectively fixedly arranged on two corresponding side walls of the detection body, and the transmitting end of the transmitter and the receiving end of the receiver are facing each other.

4. The automatic liquid replenishment continuous production device of perfluorotripropylamine according to claim 1, characterized in that: The electrolytic assembly includes an electrolytic cell, a cover body and a plurality of electrolytic plate kits, wherein the cover body is sealed over the electrolytic cell, wherein a reaction chamber is provided in the electrolytic cell, wherein a liquid inlet chamber is provided in the cover body, and adjacent reaction chambers and between 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 on the left and right sides.

5. The automatic liquid replenishment continuous production device of perfluorotripropylamine according to claim 4, characterized in that: The electrolytic plate set comprises a plurality of groups of reaction plates and a cover frame which are sequentially arranged on the left and right sides, wherein the reaction plates comprise an anode plate and a cathode plate, and a liquid inlet channel is provided between the anode plate and the cathode plate, and the cover frame is provided above the plurality of groups of reaction plates, and a plurality of strip-shaped liquid holes are formed on the cover frame, and the lower openings of the plurality of liquid holes respectively correspond to the upper openings of the plurality of liquid inlet channels; The upper openings of the plurality of liquid holes respectively correspond to the lower openings of the plurality of liquid inlets. A sealing plate is formed on the lower surface of the cover frame. The sealing plate is located on both sides of the plurality of liquid holes and is used to seal the sides of the plurality of reaction plates.

6. The automatic liquid replenishment continuous production device of perfluorotripropylamine according to claim 5, 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.

7. An automatic liquid replenishment continuous production process of perfluorotripropylamine, characterized in that: The production is carried out using an automatic liquid replenishment continuous production device for perfluorotripropylamine as described in any one of claims 1 to 6, comprising the following steps: S1. Replace the air in the electrolytic component with nitrogen, mix hydrogen fluoride and tripropylamine into a mother liquid and inject it into the electrolytic component, so that the mother liquid fills 60%-80% of the total volume of the intermediate cylinder and the inner cavity of the electrolytic component; S2. The electrolytic component is passed through a low-voltage current to perform an electrolytic replacement reaction. The reaction pressure is normal pressure and the temperature is controlled at 0-5°C. The mother liquid in the electrolytic component is controlled to account for 70%-80% of the total volume of the inner cavity of the electrolytic component through the input and output of two pump bodies; S3. During the electrolysis process, the reaction pressure is adjusted to 0.01MPa-0.03MPa, and the electrolysis current is gradually increased; S4. After 5-10 days of electrolysis, two liquid density detection components detect the liquid density at the liquid inlet and liquid outlet of the electrolysis component. Starting from the 5th day of electrolysis, the two liquid density detection components are tested twice a day until the detection values ​​of the two liquid density detection components reach or exceed the predetermined value, and the detection value error of the two liquid density detection components is less than 0.2kg / m³; S5. After the electrolysis is completed, the crude perfluorotripropylamine in the circulation pipeline, the intermediate cylinder and the electrolysis assembly is discharged; S6. When the liquid level detector detects that the liquid in the electrolytic component is lower than the rated value, the valve between the intermediate cylinder and the electrolytic component is closed, and liquid is automatically added to the electrolytic component. After the crude perfluorotripropylamine in the intermediate cylinder is completely discharged, the valve between the intermediate cylinder and the electrolytic component is opened for the next liquid replenishment electrolysis.

8. The automatic liquid replenishment continuous production process of perfluorotripropylamine according to claim 7, characterized in that: The mass ratio of tripropylamine to hydrogen fluoride in step S1 is 20-30kg:200-240kg.

9. The automatic liquid replenishment continuous production process of perfluorotripropylamine according to claim 7, characterized in that: In step S3, the electrolysis current is gradually increased to 500A-600A.

10. The automatic liquid replenishment continuous production process of perfluorotripropylamine according to claim 7, characterized in that: In steps S5 and S6, the crude perfluorotripropylamine is discharged into a double distillation device for distillation.

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