Low-boiling-point material gas-liquid fluorination device
By designing a gas-liquid fluorination device for low-boiling-point materials, and employing a reaction vessel, a condenser reflux device, and a fluorine gas absorber, safe and efficient fluorination of low-boiling-point materials under high temperature and normal pressure is achieved. This solves the problems of long fluorination cycles and low fluorine gas utilization, and enhances safety and environmental friendliness.
Patent Information
- Application Number
- CN202423093110.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-14
- Publication Date
- 2025-11-21
- Estimated Expiration
- 2034-12-14
AI Technical Summary
Existing technologies for low-boiling-point perfluoropolyether fluoride suffer from problems such as long fluorination cycles, incomplete fluorination, and low fluorine utilization, especially posing safety hazards when operating at high temperatures.
Design a gas-liquid fluorination device for low-boiling-point materials, employing a reaction vessel, a condenser reflux condenser, and a fluorine gas absorber. Heating is achieved using a heating jacket, and fluorine gas is absorbed by potassium hydroxide solution through the condenser reflux pipe, realizing a gas-liquid reaction at high temperature and normal pressure, increasing the condensation area and efficiency. A serpentine condenser and a back pressure valve are used to control the pressure.
It enables low-boiling-point materials to fully react under high temperature and normal pressure, improves the utilization rate of fluorine gas, and achieves a safe and efficient fluorination process. The waste liquid can be reused, the condensation efficiency is high, and the environmental performance is good.
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Figure CN223570719U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of fluorination equipment, in particular to a low-boiling-point material gas-liquid fluorination device. BACKGROUND
[0002] The perfluoropolyether oil is a colorless and transparent oily liquid at room temperature, has the characteristics of high temperature resistance, chemical corrosion resistance, oxidation resistance and radiation resistance, is mainly used as heat conducting oil, lubricating oil and vacuum pump oil, has a wide application in the fields of electronic industry, mechanical industry and aerospace industry due to the high stability and safety, and thus it is very important to mass-produce the perfluoropolyether oil.
[0003] At present, most of the perfluoropolyether oils on the market are obtained by fluorination of perfluoropolyether acyl fluoride, and the low-boiling-point perfluoropolyether acyl fluoride is in a gaseous state at high temperature and cannot be fluorinated under normal pressure, and the fluorination under high pressure is dangerous, and the fluorination temperature that is too low cannot stimulate the activity of fluorine gas, resulting in low conversion rate, long fluorination period, incomplete fluorination and low fluorine gas utilization rate of the low-boiling-point perfluoropolyether acyl fluoride relative to the high-boiling-point perfluoropolyether acyl fluoride. Therefore, a device for efficiently, safely and fluorinating low-boiling-point perfluoropolyether acyl fluoride is particularly important. CONTENT OF THE INVENTION
[0004] In order to solve the problems of long fluorination period, incomplete fluorination and low fluorine gas utilization rate of the low-boiling-point perfluoropolyether acyl fluoride, the present application provides a low-boiling-point material gas-liquid fluorination device.
[0005] The low-boiling-point material gas-liquid fluorination device provided by the present application adopts the following technical scheme:
[0006] The low-boiling-point material gas-liquid fluorination device comprises a reaction kettle, a heating jacket is wrapped around the circumferential outer side wall of the reaction kettle, a gas feeding pipe and a gas discharging pipe that are in communication with the inside of the reaction kettle are arranged on the reaction kettle, a condensation reflux device and a fluorine gas absorber are arranged on the reaction kettle, the condensation reflux device is in communication with the inside of the reaction kettle, and the fluorine gas absorber is connected with the condensation reflux device through a pipeline.
[0007] Through the above technical scheme, fluorine nitrogen gas enters the reaction kettle to react with the material in liquid state from the gas feeding pipe, the excess fluorine nitrogen gas enters the condensation reflux device to react with the liquid material condensed by the condensation reflux device again, and then enters the fluorine gas absorber through the pipeline for absorption. The low-boiling-point perfluoropolyether acyl fluoride can be fully reacted under high temperature and normal pressure, the fluorine gas utilization rate is high, and the low-boiling-point material is fluorinated safely, efficiently and environmentally.
[0008] Optionally, the condensing reflux device comprises condensing reflux pipes, the condensing reflux pipes are arranged in parallel, and two ends of each condensing reflux pipe are connected to the reaction kettle and the pipeline through multiple connecting pipes.
[0009] By using the above technical scheme, fluorine nitrogen gas reacts with the reflux material when passing through the condensing reflux pipes, the multiple condensing reflux pipes increase the condensing area, the condensing efficiency is high, and the gas-liquid reaction is beneficial.
[0010] Optionally, water inlets and water outlets are arranged on the condensing reflux pipes, and the water pipes are sequentially connected between the water inlets and the water outlets of the condensing reflux pipes.
[0011] By using the above technical scheme, water is supplied to the water inlets of the condensing reflux pipes on one side, and then sequentially supplied to the water inlets of the second condensing reflux pipes through the water pipes, and finally discharged from the water outlets of the last condensing reflux pipes, thereby reducing the inconvenience of separately circulating and supplying water to the single condensing reflux pipe.
[0012] Optionally, the condensing reflux pipes are serpentine condensing pipes.
[0013] By using the above technical scheme, the serpentine design of the serpentine condensing pipes increases the condensing area, and the gaseous material sufficiently contacts the condensing pipe wall when passing through, so that the condensing effect on the material is good.
[0014] Optionally, a back pressure valve is arranged on the pipeline.
[0015] By using the above technical scheme, the back pressure valve is arranged to adjust the pressure of the pipeline, and only allows fluorine nitrogen gas to pass through, so that the reverse flow in the pipeline is prevented.
[0016] Optionally, the solution in the fluorine gas absorber is potassium hydroxide solution.
[0017] By using the above technical scheme, the potassium hydroxide solution is used for fluorine gas absorption, and the waste liquid obtained after treatment can be reused.
[0018] Optionally, an inner pipe is connected to one end of the gas feeding pipe, and one end of the inner pipe extends into the reaction kettle and is located at a downward side position.
[0019] By using the above technical scheme, the inner pipe feeds the gas to the liquid in the reaction kettle for gas-liquid reaction, thereby reducing the problem of low reaction efficiency caused by insufficient contact.
[0020] Optionally, a temperature measuring pipe is arranged in the reaction kettle.
[0021] By using the above technical scheme, the temperature in the reaction kettle is monitored in real time through the temperature measuring pipe.
[0022] In summary, the present application includes at least one of the following beneficial technical effects:
[0023] 1. Fluorine gas from the gas feed pipe enters into reaction with the material in liquid state, and the excess fluorine gas enters into the condenser for condensation and reaction with the condensed liquid material, and then enters into the fluorine gas absorber through the pipeline for absorption. The low-boiling-point perfluoropolyether acyl can be fully reacted at high temperature and normal pressure, and the fluorine gas utilization rate is high, and the fluorine gas is safe, efficient, and environmentally friendly for fluorination of low-boiling-point material.
[0024] 2. The three-pipe parallel condensation of the condenser return pipe has high condensation efficiency and good condensation effect.
[0025] 3. The potassium hydroxide solution is used for fluorine gas absorption, and the waste liquid can be reused after treatment. BRIEF DESCRIPTION OF DRAWINGS
[0026] Figure 1 is a schematic diagram of the connecting structure of the present application.
[0027] Those skilled in the art will appreciate that the elements in the drawings are shown for simplicity and clarity and are not necessarily drawn to scale. For example, the dimensions and positions of some of the elements in the drawings can be exaggerated relative to other elements to help improve the understanding of the present embodiments.
[0028] Reference signs: 1, heating jacket; 2, temperature measuring tube; 3, gas feed pipe; 4, gas discharge pipe; 5, three-port connecting pipe; 6, water inlet; 7, condenser return pipe; 8, water outlet; 9, back pressure valve; 10, fluorine gas absorber. DETAILED DESCRIPTION
[0029] The present application will be further described in detail below with reference to the accompanying drawings.
[0030] The embodiments of the present application disclose a low-boiling-point material gas-liquid fluorination device, referring to Figure 1 , comprising a reaction kettle, liquid material is placed in the reaction kettle, a heating jacket 1 is wrapped around the outer wall of the reaction kettle, the heating range of the heating jacket 1 is 0-300℃, a temperature measuring tube 2 for real-time temperature monitoring is arranged in the reaction kettle, a gas feed pipe 3 and a gas discharge pipe 4 are arranged on the reaction kettle and communicate with the inside of the reaction kettle, the gas feed pipe 3 is connected with an inner pipe at one end in the reaction kettle, the inner pipe extends downward to the lower side of the liquid level of the liquid material in the reaction kettle, a condenser and a fluorine gas absorber 10 are arranged on the reaction kettle, the condenser communicates with the inside of the reaction kettle, and the fluorine gas absorber 10 is connected with the condenser through a pipeline.
[0031] In the production operation, first, the liquid material is put into the reaction kettle, the heating jacket 1 is heated to 150-300 DEG C, the fluorine nitrogen gas enters the reaction kettle from the gas feeding pipe 3 and reacts with the liquid material, the excess fluorine nitrogen gas enters the condensation reflux device and reacts with the condensed liquid material again, then enters the fluorine gas absorber 10 through the pipeline, the low-boiling full fluoropolyether acyl can be fully reacted at high temperature and normal pressure, the fluorine utilization rate is high, and the fluorination of the low-boiling material is safe, efficient and environmentally friendly.
[0032] Referring to Figure 1 , the condensation reflux device comprises three condensation reflux pipes 7 arranged vertically and parallel to each other, the condensation reflux pipe 7 is a serpentine condensation pipe, three connecting pipes 5 are arranged at the upper and lower ends of the condensation reflux pipe 7, the two ends of each condensation reflux pipe 7 are connected with the three connecting pipes 5 on both sides, the downward end of the downward connecting pipe 5 on one side is connected with the reaction kettle and communicates with the inside of the reaction kettle, the upward end of the upward connecting pipe 5 on one side communicates with the pipeline, the fluorine gas that is not fully reacted in the reaction kettle is countercurrently reacted with the reflux material when passing through the condensation reflux pipe 7, the multiple condensation reflux pipes 7 increase the condensation area and the condensation efficiency is high, which is beneficial to the gas-liquid reaction.
[0033] Referring to Figure 1 , the condensation reflux pipe 7 is provided with a water inlet 6 and a water outlet 8, the condensation reflux pipes 7 are connected by water pipes between each other and at the water inlet 6 and the water outlet 8, the water inlet 6 of the condensation reflux pipe 7 on one side is supplied with water, which is then transported to the water inlet 6 of the second condensation reflux pipe 7, and then the water is supplied in sequence and discharged from the water outlet 8 of the last condensation reflux pipe 7, thereby reducing the inconvenience of the single condensation reflux pipe 7 alone.
[0034] Referring to Figure 1 , the pipeline is provided with a back pressure valve 9, the back pressure valve 9 is arranged to adjust the pressure of the pipeline and only allows fluorine nitrogen gas to pass through, which can prevent the reverse flow in the pipeline.
[0035] Referring to Figure 1 , the solution in the fluorine gas absorber 10 is potassium hydroxide solution, the fluorine gas is absorbed by the potassium hydroxide solution, and the waste liquid obtained after treatment can be reused.
[0036] The implementation principle of the low-boiling material gas-liquid fluorination device is as follows: in the production operation, first, the liquid material is put into the reaction kettle, the heating jacket 1 is heated to 150-300 DEG C, the fluorine nitrogen gas enters the reaction kettle from the gas feeding pipe 3 and reacts with the liquid material, the excess fluorine nitrogen gas enters the condensation reflux pipe 7 and reacts with the condensed liquid material again, then enters the fluorine gas absorber 10 through the pipeline, and is absorbed by the potassium hydroxide solution in the fluorine gas absorber 10.
[0037] The above are all preferred embodiments of the present application, and do not limit the protection scope of the present application, so that: all equivalent changes made according to the structure, shape, principle of the present application should be covered within the protection scope of the present application.
Claims
1. A low-boiling-point material gas-liquid fluorination device, comprising a reaction kettle, the circumferential outer wall of the reaction kettle is wrapped with a heating jacket (1), a gas feeding pipe (3) and a gas discharging pipe (4) are arranged on the reaction kettle and communicate with the inside of the reaction kettle, characterized in that: The reaction kettle is provided with a condensing reflux device and a fluorine gas absorber (10), the condensing reflux device is communicated with the inside of the reaction kettle, and the fluorine gas absorber (10) is connected with the condensing reflux device through a pipeline.
2. A low-boiling material gas-liquid fluorination apparatus according to claim 1, characterized by: The condensing reflux device comprises condensing reflux pipes (7), the condensing reflux pipes (7) are provided with a plurality of pipes and are distributed in parallel with each other, and the two ends of each condensing reflux pipe (7) are communicated with the reaction kettle and the pipeline through a plurality of connecting pipes.
3. A low-boiling material gas-liquid fluorination apparatus according to claim 2, characterized by: Water inlets (6) and water outlets (8) are arranged on the condensing reflux pipes (7), and the water inlets (6) and the water outlets (8) of the condensing reflux pipes (7) are sequentially connected through water pipes.
4. A low-boiling material gas-liquid fluorination apparatus according to claim 2, characterized by: The condensing reflux pipes (7) are serpentine condensing pipes.
5. A low-boiling material gas-liquid fluorination apparatus according to claim 1, characterized by: A back pressure valve (9) is arranged on the pipeline.
6. A low-boiling material gas-liquid fluorination apparatus according to claim 1, characterized by: The solution in the fluorine gas absorber (10) is potassium hydroxide solution.
7. A low-boiling material gas-liquid fluorination apparatus according to claim 1, characterized by: One end of the gas feeding pipe (3) is connected with an inner pipe, one end of the inner pipe extends into the reaction kettle and is located at a downward position.
8. A low-boiling material gas-liquid fluorination apparatus according to claim 1, characterized by: A temperature measuring pipe (2) is arranged in the reaction kettle.