A method and apparatus for preparing ethoxypentafluorocyclotriphosphazene

Abstract

This invention belongs to the technical field of ethoxypentafluorocyclic triphosphazene preparation, specifically a method and apparatus for preparing ethoxypentafluorocyclic triphosphazene, including a reaction vessel; a sampling structure is provided at the top of the reaction vessel; the sampling structure includes a linear slide rail; the linear slide rail is fixedly connected to the top of the reaction vessel and is vertically arranged; a mounting plate is fixedly connected to the slider of the linear slide rail; a liquid extraction pipe is fixedly connected to the bottom surface of the mounting plate; a fixed sealing seat is fitted around the outer ring of the liquid extraction pipe; a liquid outlet is provided on the top side of the liquid extraction pipe; a liquid extraction pump is fixedly connected to the side of the mounting plate away from the linear slide rail; the inlet end of the liquid extraction pump is connected to the liquid outlet of the liquid extraction pipe; the outlet end of the liquid extraction pump is connected to a collection unit through a hose; by sampling the reaction liquid at different heights in the reaction vessel for detection, the accuracy of the detection results for the etherification reaction process is improved.

Description

Technical Field

[0001] This invention belongs to the technical field of ethoxypentafluorocyclic triphosphazene preparation, specifically a method and apparatus for preparing ethoxypentafluorocyclic triphosphazene. Background Technology

[0002] With the application of lithium-ion batteries in the power and energy storage fields, the safety issues of lithium-ion batteries are becoming increasingly prominent. Under abuse conditions such as overcharging, high temperature, puncture, or crushing, the positive electrode material in the charging state has strong oxidizing properties and easily releases oxygen. The oxygen reacts with the electrolyte to release a large amount of heat and gas, which raises the battery temperature, causes more reactions, and leads to the destruction of the battery system. Ethoxypentafluorocyclotriphosphazene has excellent flame retardant properties and has almost no impact on other aspects of battery performance, making it a relatively ideal and widely used lithium-ion electrolyte additive.

[0003] The preparation of ethoxypentafluorocyclotriphosphazene mainly involves first fluorinating hexafluorocyclotriphosphazene with a fluorinating agent to form hexafluorocyclotriphosphazene, and then reacting hexafluorocyclotriphosphazene with an ethoxide to generate ethoxy(pentafluoro)cyclotriphosphazene. The entire preparation process mainly involves fluorination and etherification reactions in a reaction vessel, followed by distillation to obtain high-concentration ethoxypentafluorocyclotriphosphazene.

[0004] During the etherification reaction in the reactor, multiple samples need to be taken to determine the reaction process through chromatography, thereby judging the progress of the entire preparation process. The existing sampling method mainly takes samples through the drain port of the reactor, which makes the range of each sample relatively concentrated and difficult to comprehensively and accurately represent the reaction process in the reactor.

[0005] Therefore, the present invention provides a method and apparatus for preparing ethoxypentafluorocyclotriphosphazene. Summary of the Invention

[0006] In order to overcome the shortcomings of the prior art, at least one technical problem raised in the background art is solved.

[0007] The technical solution adopted by this invention to solve its technical problem is as follows: An apparatus for preparing ethoxypentafluorocyclotriphosphazene according to this invention includes a reaction vessel; a sampling structure is provided at the top of the reaction vessel; the sampling structure is used to extract the solution inside the reaction vessel; the sampling structure includes a linear slide rail; the linear slide rail is fixedly connected to the top of the reaction vessel and is vertically arranged; a mounting plate is fixedly connected to the slider of the linear slide rail; a liquid extraction pipe is fixedly connected to the bottom surface of the mounting plate; the liquid extraction pipe slides through the opening at the top of the reaction vessel; a fixed sealing seat is fitted around the outer ring of the liquid extraction pipe; the fixed sealing seat is fixedly connected to the opening at the top of the reaction vessel; a liquid outlet is provided on the top side of the liquid extraction pipe; a liquid extraction pump is fixedly connected to the side of the mounting plate away from the linear slide rail; the inlet end of the liquid extraction pump is connected to the liquid outlet of the liquid extraction pipe; the outlet end of the liquid extraction pump is connected to a collection unit through a flexible hose; by extracting reaction liquid at different heights in the reaction vessel for detection, the accuracy of the detection results regarding the etherification reaction process is improved.

[0008] Preferably, a valve body is fixedly connected to the bottom end of the extraction pipe; the valve body is cylindrical and has a sealed bottom end; multiple vertical grooves are formed around the side of the valve body; a slide cylinder is slidably installed inside the valve body; the height of the slide cylinder is greater than the height of the vertical grooves; multiple connecting blocks are fixedly connected to the bottom outer ring of the slide cylinder; the connecting blocks are slidably engaged with the vertical grooves; a floating ring plate is slidably installed on the outer ring of the valve body; the connecting blocks are fixedly connected to the inner ring of the floating ring plate; the reaction liquid inside the reactor passes through the vertical grooves and the inner ring of the slide cylinder in sequence, and then enters the extraction pipe to be extracted; the floating ring plate is blocked by the reaction liquid and its own gravity, causing the floating ring plate, connecting blocks, and slide cylinder to slide downwards, so that the slide cylinder blocks and seals the vertical grooves, thereby sealing the bottom end of the extraction pipe.

[0009] Preferably, the bottom inner ring of the slide is trumpet-shaped; a sealing cone seat is fixedly connected to the bottom of the valve body; the sealing cone seat matches the bottom inner ring of the slide; a bracket is fixedly connected to the top inner ring of the slide; a sealing ring is sleeved on the top outer ring of the bracket; the outer ring of the sealing ring is elastic; this further improves the sealing effect on the bottom of the liquid extraction tube.

[0010] Preferably, magnets are embedded in the top of the vertical channel and the top of the connecting block; the two magnets attract each other; the top magnet attracts the bottom magnet, thereby fixing the slide, connecting block and floating ring plate to the top of the vertical channel, thus ensuring the smooth flow of the reaction liquid into the pumping pipe.

[0011] Preferably, the inner ring of the liquid extraction tube is fixedly connected with multiple air tubes; the bottom end of the air tube can contact and seal with the top surface of the slide cylinder; the top end of the liquid extraction tube is provided with an air cavity; the top end of the air tube communicates with the air cavity; an air pump is fixedly connected to the top surface of the mounting plate; the air outlet pipe of the air pump is connected to the air cavity; thereby, the residual reaction liquid in the liquid extraction tube and the hose is discharged together, thereby reducing the residual reaction liquid in the liquid extraction tube and the hose and improving the accuracy of the reaction liquid extraction again.

[0012] Preferably, the collection unit includes a housing; the housing is located on one side of the reactor; a slot is opened on one side of the housing; a waste liquid chamber is opened inside the other side of the housing; an electric three-way valve is fixedly connected to the top surface of the housing; the inlet of the electric three-way valve is connected to a flexible hose; an outlet pipe is fixedly connected through the top of the slot; the top of the outlet pipe is connected to one outlet of the electric three-way valve; a waste liquid pipe is fixedly connected through the top of the waste liquid chamber near the slot; the top of the waste liquid pipe is connected to the other outlet of the electric three-way valve; the bottom end of the waste liquid pipe extends into the bottom of the waste liquid chamber; a sample liquid tube is installed inside the slot; the bottom of the outlet pipe extends into the sample liquid tube; thus facilitating the removal of reaction liquid samples for testing by personnel, and facilitating the collection and removal of residual reaction liquid by personnel.

[0013] Preferably, the inner wall of the groove is fixedly connected with multiple spring clips; the inner wall of the spring clips slides in fit with the outer wall of the sample tube; a baffle is fitted around the outer ring of the outlet tube; multiple No. 1 springs are fixedly connected between the top surface of the baffle and the inner top surface of the groove; the bottom surface of the baffle can slide in contact with the top of the sample tube; the bottom outer ring of the outlet tube is threaded; an adjusting nut is installed on the bottom outer ring thread of the outlet tube; this facilitates the sampling of the reaction solution by the staff.

[0014] Preferably, a mesh partition is fixedly connected to the middle of the waste liquid chamber; a vent is provided at the top of the side of the waste liquid chamber away from the waste liquid pipe; the vent is separated from the waste liquid pipe by the mesh partition; the mesh partition blocks the reaction liquid entering the waste liquid chamber, thereby improving the stability of the reaction liquid in the waste liquid chamber.

[0015] Preferably, an air nozzle is installed internally via a threaded connection in the vent hole; multiple air grooves are formed around the top of the air nozzle; a fixing frame is fixedly connected to the bottom of the inner ring of the air nozzle; a sliding rod is slidably installed in the middle of the fixing frame; a limiting plate is fixedly connected to the top outer ring of the sliding rod; a second spring is fixedly connected between the limiting plate at the top of the sliding rod and the top surface inside the air nozzle; a hollow float is fixedly connected to the bottom of the sliding rod; a sealing ring is fixedly connected to the top outer ring of the hollow float; the sealing ring at the top of the hollow float can contact and seal with the bottom of the air nozzle; thereby preventing excessive reaction liquid from being stored in the waste liquid chamber and improving the safety of the collection unit.

[0016] A method for preparing ethoxypentafluorocyclic triphosphazene, the method employing the aforementioned apparatus for preparing ethoxypentafluorocyclic triphosphazene, and the method comprising the following steps:

[0017] S1: Fluorination reaction: Hexachlorocyclotriphosphazene, trifluorotoluene, and antimony pentachloride are added to a reaction vessel and stirred to react. Hydrogen fluoride gas is introduced at the same time. After the reaction is completed, nitrogen gas is introduced to remove the hydrogen fluoride gas inside the reaction vessel. Then, the mixture is distilled to obtain hexachlorocyclotriphosphazene.

[0018] S2: Etherification reaction: The obtained hexafluorocyclotriphosphazene and methyl tert-butyl ether are added back to the reaction vessel and stirred. At the same time, sodium ethoxide is slowly added to carry out the reaction.

[0019] S3: Control the linear slide rail to extend the liquid extraction tube into the appropriate position in the reactor. At this time, the valve body is in the open state, sealing the bottom end of the gas pipe. The liquid extraction pump extracts the reaction liquid in the reactor through the liquid extraction tube and delivers it to the sample liquid tube.

[0020] S4: After sampling, the linear slide rail raises the liquid extraction tube, so that the bottom end of the liquid extraction tube is separated from the reaction liquid in the reactor. At this time, the valve body is in the closed state, the bottom end of the gas pipe is opened, and the electric three-way valve connects the waste liquid pipe to the hose.

[0021] S5: The air pump introduces high-pressure gas into the interior of the liquid extraction tube through the air pipe; the high-pressure gas enters the waste liquid chamber through the liquid extraction tube, hose, and waste liquid tube, and at the same time, it carries the residual reaction liquid inside the liquid extraction tube and hose into the waste liquid chamber for storage.

[0022] S6: Staff members test the sample liquid inside the sample tube to determine the reaction progress inside the reactor; after the reaction is complete, ethoxypentafluorocyclotriphosphazene is obtained through filtration and distillation.

[0023] The beneficial effects of this invention are as follows:

[0024] 1. The present invention discloses a method and apparatus for preparing ethoxypentafluorocyclotriphosphazene, comprising a reaction vessel, a linear slide rail, a mounting plate, a liquid extraction pipe, a fixed sealing seat, a liquid extraction pump, and a flexible hose. During the etherification reaction inside the reaction vessel, the sliding block of the linear slide rail is controlled to descend, causing the mounting plate to descend and pushing the bottom end of the liquid extraction pipe to different heights of the reaction liquid inside the reaction vessel. At this time, the liquid extraction pump extracts the reaction liquid from the reaction vessel through the liquid extraction pipe and transports it to a collection unit for storage through the flexible hose. The operator retrieves a sample of the reaction liquid from the collection unit for testing to determine the progress of the etherification reaction in the reaction vessel. By sampling the reaction liquid at different heights in the reaction vessel for testing, the accuracy of the test results in determining the progress of the etherification reaction is improved.

[0025] 2. The method and apparatus for preparing ethoxypentafluorocyclotriphosphazene according to the present invention comprises a housing, an electric three-way valve, an outlet pipe, a waste pipe, and a sample pipe. When sampling the reaction solution, the sample pipe is installed in the slot of the housing, with the bottom end of the outlet pipe inserted into the sample pipe. The electric three-way valve connects the hose and the outlet pipe, and the extracted reaction solution enters the sample pipe for storage through the outlet pipe. After the reaction solution extraction is complete, the electric three-way valve connects the hose and the waste pipe, and compressed gas carries the residual reaction solution through the waste pipe into the waste chamber of the housing for storage. This facilitates the removal of reaction solution samples for testing and the collection of residual reaction solution. Attached Figure Description

[0026] The invention will now be further described with reference to the accompanying drawings.

[0027] Figure 1 This is a perspective view of the present invention;

[0028] Figure 2 This is a perspective view of the sampling structure and collection unit in this invention;

[0029] Figure 3 This is a cross-sectional view of the mounting plate in this invention;

[0030] Figure 4 This is a cross-sectional view of the valve body in this invention;

[0031] Figure 5 This is a cross-sectional view of the collecting unit in this invention;

[0032] Figure 6 This is a cross-sectional view of the air nozzle in this invention;

[0033] Figure 7 This is a flowchart of the preparation method in this invention;

[0034] In the diagram: 1. Reactor; 2. Linear slide rail; 3. Mounting plate; 4. Liquid extraction pipe; 5. Fixed sealing seat; 6. Liquid extraction pump; 7. Hose; 8. Valve body; 9. Vertical through groove; 10. Slide cylinder; 11. Connecting block; 12. Floating ring plate; 13. Sealing cone seat; 14. Bracket; 15. Sealing ring plate; 16. Magnet; 17. Gas pipe; 18. Gas chamber; 19. Gas pump; 20. Box body; 21. Groove opening; 22. Waste liquid chamber; 23. Electric three-way valve; 24. Liquid outlet pipe; 25. Waste liquid pipe; 26. Sample liquid pipe; 27. Spring clip; 28. Baffle; 29. ​​Spring No. 1; 30. Adjusting nut; 31. Mesh partition; 32. Vent hole; 33. Air nozzle; 34. Fixing frame; 35. Slide rod; 36. Spring No. 2; 37. Hollow float seat. Detailed Implementation

[0035] To make the technical means, creative features, objectives and effects of this invention easier to understand, the invention will be further described below in conjunction with specific embodiments.

[0036] like Figures 1 to 3 As shown in the embodiment of the present invention, an apparatus for preparing ethoxypentafluorocyclotriphosphazene includes a reaction vessel 1; a sampling structure is provided on the top of the reaction vessel 1; the sampling structure is used to extract the solution inside the reaction vessel 1; the sampling structure includes a linear slide rail 2; the linear slide rail 2 is fixedly connected to the top of the reaction vessel 1 and is vertically arranged; a mounting plate 3 is fixedly connected to the slider of the linear slide rail 2; a liquid extraction pipe 4 is fixedly connected to the bottom surface of the mounting plate 3; the liquid extraction pipe 4 slides through the opening at the top of the reaction vessel 1; a fixed sealing seat 5 is sleeved on the outer ring of the liquid extraction pipe 4; the fixed sealing seat 5 is fixedly connected to the opening at the top of the reaction vessel 1; a liquid outlet is provided on the top side of the liquid extraction pipe 4; a liquid extraction port is fixedly connected to the side of the mounting plate 3 away from the linear slide rail 2. A liquid pump 6 is included; the inlet of the liquid pump 6 is connected to the outlet of the liquid extraction pipe 4; the outlet of the liquid pump 6 is connected to a collection unit via a hose 7; during operation, when the etherification reaction is taking place inside the reactor 1, the slider of the linear slide rail 2 is controlled to descend, causing the mounting plate 3 to descend, pushing the bottom end of the liquid extraction pipe 4 to extend to different heights of the reaction liquid inside the reactor 1. At this time, the liquid pump 6 extracts the reaction liquid inside the reactor 1 through the liquid extraction pipe 4 and transports it to the collection unit for storage through the hose 7. The operator takes out a sample of the reaction liquid from the collection unit for testing to determine the progress of the etherification reaction in the reactor 1; by extracting reaction liquid at different heights in the reactor 1 for testing, the accuracy of the test results in determining the progress of the etherification reaction is improved.

[0037] like Figures 2 to 4As shown, a valve body 8 is fixedly connected to the bottom end of the extraction pipe 4; the valve body 8 is cylindrical, and its bottom end is a sealed structure; multiple vertical grooves 9 are circumferentially formed on the side of the valve body 8; a sliding cylinder 10 is slidably installed inside the valve body 8; the height of the sliding cylinder 10 is greater than the height of the vertical grooves 9; multiple connecting blocks 11 are fixedly connected to the outer ring of the bottom of the sliding cylinder 10; the connecting blocks 11 are slidably engaged with the vertical grooves 9; a floating ring plate 12 is slidably installed on the outer ring of the valve body 8; the connecting blocks 11 are fixedly connected to the inner ring of the floating ring plate 12; during operation, when the bottom end of the extraction pipe 4 enters the reaction liquid inside the reactor 1, it drives the valve body 8 to extend into the reaction liquid inside the reactor 1, and the floating ring plate 12 is resisted by the reaction liquid. The action of the block and buoyancy causes the floating ring plate 12 to move upward along the valve body 8, which in turn causes the connecting block 11 to slide upward along the vertical groove 9, and the sliding cylinder 10 to slide upward. This allows the inside of the extraction pipe 4 to connect sequentially with the inner ring of the sliding cylinder 10, the vertical groove 9, and the outside of the valve body 8. When the extraction pump 6 is pumping liquid, the reaction liquid inside the reactor 1 passes sequentially through the vertical groove 9 and the inner ring of the sliding cylinder 10, and enters the extraction pipe 4 to be extracted. When the extraction pipe 4 rises to a height above the reaction liquid, the floating ring plate 12 is blocked by the reaction liquid and its own gravity, causing the floating ring plate 12, the connecting block 11, and the sliding cylinder 10 to slide downward. This causes the sliding cylinder 10 to block and seal the vertical groove 9, thereby sealing and blocking the bottom end of the extraction pipe 4.

[0038] like Figure 4 As shown, the bottom inner ring of the slide cylinder 10 is trumpet-shaped; a sealing cone seat 13 is fixedly connected to the bottom of the valve body 8; the sealing cone seat 13 matches the bottom inner ring of the slide cylinder 10; a bracket 14 is fixedly connected to the top inner ring of the slide cylinder 10; a sealing ring 15 is sleeved on the top outer ring of the bracket 14; the outer ring of the sealing ring 15 is elastic; during operation, when the pump 6 pumps liquid, the reaction liquid inside the reactor 1 passes through the vertical channel 9 and the inner ring of the slide cylinder 10 in sequence, and the reaction liquid pushes the outer ring of the sealing ring 15 upward, causing the reaction liquid to enter the pumping pipe 4; when the pumping pipe 4 rises to a height that disengages from the reaction liquid, the sealing ring 15 returns to its original position, sealing the top of the slide cylinder 10, thereby improving the sealing and blocking effect at the bottom of the pumping pipe 4; by matching the sealing cone seat 13 with the bottom inner ring of the slide cylinder 10, the sealing effect at the bottom of the pumping pipe 4 is further improved.

[0039] like Figure 4As shown, magnets 16 are embedded in the top of both the vertical channel 9 and the top of the connecting block 11; the two magnets 16 attract each other; during operation, the floating ring plate 12 is blocked by the reaction liquid and subjected to buoyancy, causing the floating ring plate 12 to move upward along the valve body 8, so that the top magnet 16 and the bottom magnet 16 attract each other, thereby fixing the slide cylinder 10, the connecting block 11 and the floating ring plate 12 to the top of the vertical channel 9, thus ensuring the smooth flow of the reaction liquid into the pumping pipe 4; when the pumping pipe 4 rises to a height away from the reaction liquid, the floating ring plate 12 is blocked by the reaction liquid and subjected to its own gravity, causing the floating ring plate 12, the connecting block 11 and the slide cylinder 10 to slide downward, so that the top magnet 16 and the bottom magnet 16 separate, thereby causing the slide cylinder 10 to block and seal the vertical channel 9.

[0040] like Figures 2 to 4 As shown, multiple air pipes 17 are fixedly connected to the inner ring of the liquid extraction pipe 4; the bottom end of the air pipe 17 can contact and seal with the top surface of the slide cylinder 10; an air chamber 18 is opened at the top end of the liquid extraction pipe 4; the top end of the air pipe 17 is connected to the air chamber 18; an air pump 19 is fixedly connected to the top surface of the mounting plate 3; the air outlet pipe of the air pump 19 is connected to the air chamber 18; during operation, after the slide cylinder 10 blocks and seals the vertical through groove 9, the reaction liquid will remain in the liquid extraction pipe 4; at this time, the air pump 19 pumps compressed gas into the air chamber 18, and then guides it to the bottom of the liquid extraction pipe 4 through multiple air pipes 17. Since the bottom end of the liquid extraction pipe 4 is blocked and sealed, the compressed gas is discharged upward along the liquid extraction pipe 4, and then enters the collection unit through the hose 7, thereby discharging the reaction liquid remaining in the liquid extraction pipe 4 and the hose 7, thereby reducing the residue of reaction liquid in the liquid extraction pipe 4 and the hose 7, and improving the accuracy of the reaction liquid extraction.

[0041] like Figure 1 , Figure 2 and Figure 5As shown, the collection unit includes a housing 20; the housing 20 is located on one side of the reactor 1; a slot 21 is opened on one side of the housing 20; a waste liquid chamber 22 is opened inside the other side of the housing 20; an electric three-way valve 23 is fixedly connected to the top surface of the housing 20; the inlet of the electric three-way valve 23 is connected to a hose 7; an outlet pipe 24 is fixedly connected through the top of the slot 21; the top end of the outlet pipe 24 is connected to one outlet of the electric three-way valve 23; a waste liquid pipe 25 is fixedly connected through the top of the waste liquid chamber 22 near the slot 21; the top end of the waste liquid pipe 25 is connected to the other outlet of the electric three-way valve 23; the bottom end of the waste liquid pipe 25 extends into the bottom of the waste liquid chamber 22; the slot 21 is located on one side of the reactor 1; a slot 21 is located on one side of the reactor 1; a slot 21 is located on one side of the reactor 20 ... The sample tube 26 is installed inside the unit 1. The bottom of the outlet tube 24 extends into the sample tube 26. During operation, when the reaction solution is sampled, the sample tube 26 is installed into the slot 21 of the housing 20, so that the bottom end of the outlet tube 24 is inserted into the sample tube 26. The electric three-way valve 23 is controlled to connect the hose 7 and the outlet tube 24. The extracted reaction solution enters the sample tube 26 through the outlet tube 24 for storage. After the reaction solution is extracted, the electric three-way valve 23 connects the hose 7 and the waste liquid tube 25. The compressed gas carries the residual reaction solution through the waste liquid tube 25 and discharges it into the waste liquid chamber 22 of the housing 20 for storage. This makes it convenient for staff to take out the reaction solution sample for testing and to collect the residual reaction solution.

[0042] like Figure 2 and Figure 5 As shown, multiple spring clips 27 are fixedly connected to the inner wall of the slot 21; the inner wall of the spring clips 27 slides in fit with the outer wall of the sample tube 26; a baffle 28 is fitted around the outer ring of the outlet tube 24; multiple No. 1 springs 29 are fixedly connected between the top surface of the baffle 28 and the inner top surface of the slot 21; the bottom surface of the baffle 28 can slide in contact with the top of the sample tube 26; the bottom outer ring of the outlet tube 24 is threaded; an adjusting screw is installed on the bottom outer ring of the outlet tube 24. The position of the baffle 28 is controlled by adjusting the adjusting nut 30, which facilitates the installation of sample tubes 26 of different specifications. When installing the sample tube 26, the opening of the sample tube 26 is inserted into the slot 21 at an angle so that the opening of the sample tube 26 contacts the bottom surface of the baffle 28. Then, the sample tube 26 is clamped in the spring clip 27. At this time, the elastic force generated by the compression of the first spring 29 pushes the baffle 28 downward, fixing the sample tube 26 vertically, which facilitates the sampling of the reaction liquid by the staff.

[0043] like Figure 5As shown, a perforated partition 31 is fixedly connected to the middle of the waste liquid chamber 22; a vent 32 is provided on the top of the side of the waste liquid chamber 22 away from the waste liquid pipe 25; the vent 32 and the waste liquid pipe 25 are separated by the perforated partition 31; during operation, compressed gas carrying residual reaction liquid is discharged into the waste liquid chamber 22 of the housing 20 through the waste liquid pipe 25, and then the compressed gas passes through the holes of the perforated partition 31 and is discharged from the vent 32, reducing the pressure in the waste liquid chamber 22; at the same time, the perforated partition 31 blocks the reaction liquid from entering the waste liquid chamber 22, improving the stability of the reaction liquid in the waste liquid chamber 22.

[0044] like Figures 5 to 6 As shown, an air nozzle 33 is threadedly installed inside the vent 32; multiple air grooves are formed around the top of the air nozzle 33; a fixing bracket 34 is fixedly connected to the bottom of the inner ring of the air nozzle 33; a sliding rod 35 is slidably installed in the middle of the fixing bracket 34; a limiting plate is fixedly connected to the top outer ring of the sliding rod 35; a second spring 36 is fixedly connected between the limiting plate at the top of the sliding rod 35 and the top surface inside the air nozzle 33; a hollow float 37 is fixedly connected to the bottom of the sliding rod 35; a sealing ring is fixedly connected to the top outer ring of the hollow float 37; the sealing ring at the top of the hollow float 37 can contact and seal with the bottom of the air nozzle 33; during operation, when compressed gas passes through the vent 32... At this time, the second spring 36 pushes the slide bar 35 downward, causing the hollow float 37 to separate from the bottom of the air nozzle 33. This allows compressed gas to pass through the gap between the hollow float 37 and the air nozzle 33, and the inner ring of the air nozzle 33 is discharged from the waste liquid chamber 22. When the reaction liquid stored inside the waste liquid chamber 22 rises to the bottom of the hollow float 37, it lifts the hollow float 37 upward, pushing the slide bar 35 upward. This causes the second spring 36 to compress, and the hollow float 37 seals the inner ring of the air nozzle 33. At the same time, the drain port at the bottom of the waste liquid chamber 22 discharges the reaction liquid for recycling. This avoids storing too much reaction liquid in the waste liquid chamber 22 and improves the safety of the collection unit.

[0045] like Figure 7 As shown, a method for preparing ethoxypentafluorocyclotriphosphazene is described above. This method utilizes the aforementioned apparatus for preparing ethoxypentafluorocyclotriphosphazene and includes the following steps:

[0046] S1: Fluorination reaction: Hexachlorocyclotriphosphazene, trifluorotoluene, and antimony pentachloride are added to reactor 1 and stirred for reaction. Hydrogen fluoride gas is introduced at the same time. After the reaction is completed, nitrogen gas is introduced to remove the hydrogen fluoride gas inside reactor 1. Then, hexachlorocyclotriphosphazene is obtained by distillation.

[0047] S2: Etherification reaction: The obtained hexafluorocyclotriphosphazene and methyl tert-butyl ether are added back to reactor 1 and stirred. At the same time, sodium ethoxide is slowly added to carry out the reaction.

[0048] S3: Control the linear slide rail 2 to extend the liquid extraction pipe 4 into the appropriate position in the reaction vessel 1. At this time, the valve body 8 is in the open state, sealing the bottom end of the gas pipe 17. The liquid extraction pump 6 extracts the reaction liquid in the reaction vessel 1 through the liquid extraction pipe 4 and delivers it to the sample liquid pipe 26.

[0049] S4: After sampling, the linear slide rail 2 raises the liquid extraction tube 4, so that the bottom end of the liquid extraction tube 4 is separated from the reaction liquid in the reactor 1. At this time, the valve body 8 is in the closed state, and the bottom end of the gas pipe 17 is opened. At the same time, the electric three-way valve 23 connects the waste liquid pipe 25 to the hose 7.

[0050] S5: The air pump 19 introduces high-pressure gas into the interior of the liquid extraction pipe 4 through the air pipe 17; the high-pressure gas enters the waste liquid chamber 22 through the liquid extraction pipe 4, the hose 7, and the waste liquid pipe 25, and at the same time, it carries the reaction liquid remaining in the liquid extraction pipe 4 and the hose 7 into the waste liquid chamber 22 for storage.

[0051] S6: The staff tests the sample liquid inside the sample tube 26 to determine the reaction progress inside the reactor 1; after the reaction is completed, ethoxypentafluorocyclotriphosphazene is obtained by filtration and distillation.

[0052] Working principle: Fluorination reaction: Hexachlorocyclotriphosphazene, trifluorotoluene, and antimony pentachloride are added to reactor 1 and stirred for reaction. Hydrogen fluoride gas is introduced at the same time. After the reaction is completed, nitrogen gas is introduced to remove the hydrogen fluoride gas inside reactor 1. Then, distillation is performed to obtain hexafluorocyclotriphosphazene; Etherification reaction: The obtained hexafluorocyclotriphosphazene and methyl tert-butyl ether are added back to reactor 1 and stirred. At the same time, sodium ethoxide is slowly added to carry out the reaction.

[0053] The opening of the sample tube 26 is inserted into the slot 21 at an angle, so that the opening of the sample tube 26 contacts the bottom surface of the baffle 28. Then the sample tube 26 is clamped in the spring clip 27. At this time, the elastic force generated by the compression of the first spring 29 pushes the baffle 28 to move downward, fixing the sample tube 26 vertically. The electric three-way valve 23 is controlled to connect the hose 7 and the outlet tube 24.

[0054] The sliding height of the slider of the linear slide rail 2 is controlled, which drives the mounting plate 3 to descend, pushing the bottom end of the liquid extraction pipe 4 to extend into different heights of the reaction liquid inside the reactor 1; the valve body 8 is driven into the reaction liquid inside the reactor 1, and the floating ring plate 12 is blocked by the reaction liquid and buoyant, causing the floating ring plate 12 to move upward along the valve body 8, driving the connecting block 11 to slide upward along the vertical channel 9, and driving the slide cylinder 10 to slide upward, so that the top magnet 16 and the bottom magnet 16 attract each other, fixing the slide cylinder 10, the connecting block 11 and the floating ring plate 12 at the top of the vertical channel 9; the liquid extraction pump 6 extracts the reaction liquid inside the reactor 1 through the liquid extraction pipe 4, and the extracted reaction liquid enters the sample liquid pipe 26 through the liquid outlet pipe 24 for storage;

[0055] After the reaction liquid is extracted, the linear slide rail 2 drives the extraction pipe 4 to rise to a higher height and detach from the reaction liquid. The floating ring plate 12 is blocked by the reaction liquid and its own gravity, causing the floating ring plate 12, the connecting block 11 and the slide cylinder 10 to slide downward, so that the top magnet 16 and the bottom magnet 16 are separated. The slide cylinder 10 blocks and seals the vertical through groove 9, and the bottom of the extraction pipe 4 is sealed and blocked.

[0056] At this time, the electric three-way valve 23 connects the hose 7 and the waste liquid pipe 25. The air pump 19 pumps compressed gas into the air chamber 18, and then guides it through multiple air pipes 17 to the bottom of the liquid extraction pipe 4. Since the bottom end of the liquid extraction pipe 4 is blocked and sealed, the compressed gas is discharged upward along the liquid extraction pipe 4. The compressed gas carries the residual reaction liquid and is discharged into the waste liquid chamber 22 of the box 20 through the waste liquid pipe 25. The compressed gas passes through the holes of the mesh partition 31. When the compressed gas passes through the vent 32, the second spring 36 pushes the slide rod 35. Moving downwards pushes the hollow float 37 to separate from the bottom of the air nozzle 33, allowing compressed gas to pass through the gap between the hollow float 37 and the air nozzle 33, and the inner ring of the air nozzle 33 is discharged from the waste liquid chamber 22; when the reaction liquid stored inside the waste liquid chamber 22 rises to the bottom of the hollow float 37, it lifts the hollow float 37 to move upwards, pushing the slide bar 35 to move upwards, causing the second spring 36 to compress, and the hollow float 37 seals the inner ring of the air nozzle 33. At the same time, the drain port at the bottom of the waste liquid chamber 22 discharges the reaction liquid for recycling.

[0057] The staff tested the sample liquid inside the sample tube 26 to determine the reaction progress inside the reactor 1; after the reaction was completed, ethoxypentafluorocyclotriphosphazene was obtained by filtration and distillation.

[0058] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. An apparatus for preparing ethoxypentafluorocyclotriphosphazene, characterized in that: Includes a reaction vessel (1); a sampling structure is provided on the top of the reaction vessel (1); the sampling structure is used to extract the solution inside the reaction vessel (1); The sampling structure includes a linear slide rail (2); the top of the reactor (1) is fixedly connected to the linear slide rail (2), and the linear slide rail (2) is vertically arranged; a mounting plate (3) is fixedly connected to the slider of the linear slide rail (2); a liquid extraction pipe (4) is fixedly connected to the bottom surface of the mounting plate (3); the liquid extraction pipe (4) slides through the opening at the top of the reactor (1); a fixed sealing seat (5) is fitted around the outer ring of the liquid extraction pipe (4); the fixed sealing seat (5) is fixedly connected to the opening at the top of the reactor (1); an outlet is provided on the top side of the liquid extraction pipe (4); a liquid extraction pump (6) is fixedly connected to the side of the mounting plate (3) away from the linear slide rail (2); the inlet end of the liquid extraction pump (6) is connected to the outlet of the liquid extraction pipe (4); the outlet end of the liquid extraction pump (6) is connected to a collection unit through a hose (7).

2. The apparatus for preparing ethoxypentafluorocyclotriphosphazene according to claim 1, characterized in that: The bottom end of the suction tube (4) is fixedly connected to a valve body (8); the valve body (8) is cylindrical and the bottom end of the valve body (8) is a sealed structure; multiple vertical through grooves (9) are opened around the side of the valve body (8); a slide cylinder (10) is slidably installed inside the valve body (8); the height of the slide cylinder (10) is greater than the height of the vertical through groove (9); multiple connecting blocks (11) are fixedly connected around the bottom outer ring of the slide cylinder (10); the connecting blocks (11) are slidably engaged with the vertical through groove (9); a floating ring plate (12) is slidably installed on the outer ring of the valve body (8); the connecting blocks (11) are fixedly connected to the inner ring of the floating ring plate (12).

3. The apparatus for preparing ethoxypentafluorocyclotriphosphazene according to claim 2, characterized in that: The bottom inner ring of the slide cylinder (10) is trumpet-shaped; a sealing cone seat (13) is fixedly connected to the bottom of the valve body (8); the sealing cone seat (13) matches the bottom inner ring of the slide cylinder (10); a bracket (14) is fixedly connected to the top inner ring of the slide cylinder (10); a sealing ring plate (15) is sleeved on the top outer ring of the bracket (14); the outer ring of the sealing ring plate (15) is elastic.

4. The apparatus for preparing ethoxypentafluorocyclotriphosphazene according to claim 2, characterized in that: The top of the vertical through groove (9) and the top of the connecting block (11) are both inlaid with magnets (16); the two magnets (16) attract each other.

5. The apparatus for preparing ethoxypentafluorocyclotriphosphazene according to claim 2, characterized in that: The inner ring of the liquid extraction tube (4) is fixedly connected with multiple air tubes (17); the bottom end of the air tube (17) can contact and seal with the top surface of the slide cylinder (10); the top end of the liquid extraction tube (4) is provided with an air chamber (18); the top end of the air tube (17) is connected to the air chamber (18); the top surface of the mounting plate (3) is fixedly connected with an air pump (19); the air outlet pipe of the air pump (19) is connected to the air chamber (18).

6. The apparatus for preparing ethoxypentafluorocyclotriphosphazene according to claim 5, characterized in that: The collection unit includes a housing (20); a housing (20) is provided on one side of the reactor (1); a slot (21) is opened on one side of the housing (20); a waste liquid chamber (22) is opened inside the other side of the housing (20); an electric three-way valve (23) is fixedly connected to the top surface of the housing (20); the inlet of the electric three-way valve (23) is connected to a hose (7); an outlet pipe (24) is fixedly connected through the top of the slot (21); the outlet pipe (24) The top of the waste liquid chamber (22) is connected to one outlet of the electric three-way valve (23); a waste liquid pipe (25) is fixedly connected to the top of the side of the waste liquid chamber (22) near the opening (21); the top of the waste liquid pipe (25) is connected to the other outlet of the electric three-way valve (23); the bottom of the waste liquid pipe (25) extends into the bottom of the waste liquid chamber (22); a sample liquid pipe (26) is installed inside the opening (21); the bottom of the outlet pipe (24) extends into the inside of the sample liquid pipe (26).

7. The apparatus for preparing ethoxypentafluorocyclotriphosphazene according to claim 6, characterized in that: Multiple spring clips (27) are fixedly connected to the inner wall of the slot (21); the inner wall of the spring clips (27) slides in fit with the outer wall of the sample tube (26); a baffle (28) is fitted around the outer ring of the outlet tube (24); multiple No. 1 springs (29) are fixedly connected between the top surface of the baffle (28) and the inner top surface of the slot (21); the bottom surface of the baffle (28) can slide in contact with the top of the sample tube (26); the bottom outer ring of the outlet tube (24) is threaded; an adjusting nut (30) is installed on the bottom outer ring of the outlet tube (24).

8. The apparatus for preparing ethoxypentafluorocyclotriphosphazene according to claim 6, characterized in that: A mesh partition (31) is fixedly connected to the middle of the waste liquid chamber (22); a vent hole (32) is opened on the top of the side of the waste liquid chamber (22) away from the waste liquid pipe (25); the vent hole (32) and the waste liquid pipe (25) are separated by the mesh partition (31).

9. The apparatus for preparing ethoxypentafluorocyclotriphosphazene according to claim 8, characterized in that: An air nozzle (33) is installed inside the vent hole (32) with internal threads; multiple air grooves are provided around the top of the air nozzle (33); a fixing frame (34) is fixedly connected to the bottom of the inner ring of the air nozzle (33); a slide rod (35) is slidably installed in the middle of the fixing frame (34); a limiting plate is fixedly connected to the top outer ring of the slide rod (35); a second spring (36) is fixedly connected between the limiting plate at the top of the slide rod (35) and the top surface inside the air nozzle (33); a hollow float (37) is fixedly connected to the bottom of the slide rod (35); a sealing ring is fixedly connected to the top outer ring of the hollow float (37); the sealing ring at the top of the hollow float (37) can contact and seal with the bottom of the air nozzle (33).

10. A method for preparing ethoxypentafluorocyclotriphosphazene, characterized in that: The preparation method uses the apparatus for preparing ethoxypentafluorocyclotriphosphazene as described in claim 6, and the preparation method includes the following steps: S1: Fluorination reaction: Hexachlorocyclotriphosphazene, trifluorotoluene and antimony pentachloride are added to the reaction vessel (1) and stirred for reaction. At the same time, hydrogen fluoride gas is introduced. After the reaction is completed, nitrogen gas is introduced to remove the hydrogen fluoride gas inside the reaction vessel (1) and then distilled to obtain hexachlorocyclotriphosphazene. S2: Etherification reaction: The obtained hexafluorocyclotriphosphazene and methyl tert-butyl ether are added back to the reaction vessel (1) and stirred. At the same time, sodium ethoxide is slowly added to carry out the reaction. S3: Control the linear slide rail (2) to extend the liquid extraction pipe (4) into the appropriate position in the reactor (1). At this time, the valve body (8) is in the open state, sealing the bottom end of the gas pipe (17). The liquid extraction pump (6) extracts the reaction liquid in the reactor (1) through the liquid extraction pipe (4) and delivers it to the sample liquid pipe (26). S4: After sampling, the linear slide rail (2) raises the liquid extraction tube (4) so ​​that the bottom end of the liquid extraction tube (4) is separated from the reaction liquid in the reactor (1). At this time, the valve body (8) is closed and the bottom end of the gas pipe (17) is opened. At the same time, the electric three-way valve (23) connects the waste liquid pipe (25) with the hose (7). S5: The air pump (19) introduces high-pressure gas into the interior of the liquid extraction pipe (4) through the air pipe (17); the high-pressure gas enters the waste liquid chamber (22) through the liquid extraction pipe (4), the hose (7), and the waste liquid pipe (25), and at the same time, it carries the reaction liquid remaining in the liquid extraction pipe (4) and the hose (7) into the waste liquid chamber (22) for storage. S6: The staff will test the sample liquid inside the sample tube (26) to determine the reaction progress inside the reactor (1); after the reaction is completed, ethoxypentafluorocyclotriphosphazene is obtained by filtration and distillation.

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