Fluorination reaction device for trichlorotrifluoroethane
By setting up a tetrachloroethylene feed pipe, discharge pipe and return pipeline in the fluorination reaction device of trifluorotrichloroethane, tetrachloroethylene absorbs unreacted chlorine and heat, the problem of high consumption of alkali liquid in traditional devices is solved, and cost reduction and efficiency improvement are achieved.
Patent Information
- Application Number
- CN202421738706.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-22
- Publication Date
- 2025-07-25
- Estimated Expiration
- 2034-07-22
AI Technical Summary
In the fluorination reaction device of traditional trifluorotrichloroethane, the crude trifluorotrichloroethane contains more unreacted chlorine, resulting in large consumption of alkali liquid, increasing production costs and reducing production efficiency.
The tetrachloroethylene feed pipe, discharge pipe and return pipeline are installed in the reaction device. The tetrachloroethylene raw material is used to contact high-temperature crude gas in the reaction distillation tower to absorb unreacted chlorine, and the contact area is increased through the atomization nozzle. The reflux inner tube washes the entrained catalyst back to the reaction kettle to reduce alkali washing consumption and energy consumption.
It improves the utilization rate of chlorine, reduces alkaline washing consumption and energy consumption, reduces production costs, and reduces catalyst losses and equipment corrosion risks.
Smart Images
Figure CN223144161U_ABST
Abstract
Description
Technical Field
[0001] This application belongs to the technical field of chemical production equipment and relates to a fluorination reaction device for trichlorotrifluoroethane. Background Art
[0002] The fluorination reaction of trichlorotrifluoroethane (R113A) is mainly a gas-phase catalytic reaction based on tetrachloroethylene raw material with hydrogen fluoride (HF) and chlorine (Cl2) under specific conditions.
[0003] As Figure 1 shown, the traditional fluorination reaction device for trichlorotrifluoroethane includes a reactive distillation column 1 and a fluorination reaction kettle 2. The tetrachloroethylene raw material is added into the fluorination reaction kettle 2 through the tetrachloroethylene feed pipe 11 on the fluorination reaction kettle. Hydrogen fluoride and chlorine are also introduced into the fluorination reaction kettle. After fluorination, the crude trichlorotrifluoroethane enters the subsequent water and alkali washing system for acid removal and chlorine removal treatment after passing through the reactive distillation column 1.
[0004] In this process, the crude trichlorotrifluoroethane contains a large amount of unreacted chlorine, which consumes a large amount of alkali liquor and is not conducive to reducing production costs and improving production efficiency. Utility Model Content
[0005] In order to reduce the fluorination cost of trichlorotrifluoroethane, this application provides a fluorination reaction device for trichlorotrifluoroethane.
[0006] The fluorination reaction device for trichlorotrifluoroethane provided by this application adopts the following technical solutions:
[0007] A fluorination reaction device for trichlorotrifluoroethane includes a reactive distillation column and a fluorination reaction kettle. The fluorination reaction kettle is connected with a hydrogen fluoride feed pipe and a chlorine feed pipe. An outlet pipeline is arranged between the fluorination reaction kettle and the reactive distillation column. A reflux pipeline is arranged between the reactive distillation column and the fluorination reaction kettle. A tetrachloroethylene feed pipe is also arranged on the reactive distillation column. The connection between the outlet pipeline and the reactive distillation column and the connection between the reflux pipeline and the reactive distillation column are both located below the tetrachloroethylene feed pipe.
[0008] By adopting the above technical solutions, during the reaction process, the tetrachloroethylene raw material is transported into the reactive distillation column through the tetrachloroethylene feed pipe and contacts with the high-temperature crude gas coming from the bottom of the reactive distillation column. The high-temperature crude gas can be formed by catalytic reactions such as hydrogen fluoride and chlorine. On the one hand, tetrachloroethylene absorbs the unreacted chlorine in the crude gas and returns it to the fluorination reaction kettle, improving the chlorine utilization rate, reducing the chlorine content in the crude trichlorotrifluoroethane, and reducing the consumption of alkali in the subsequent alkali washing system. On the other hand, through heat conduction between tetrachloroethylene and the crude gas, heat is absorbed, reducing the externally supplied heat required for the fluorination reaction, reducing energy consumption, and reducing the fluorination cost.
[0009] Preferably, a spraying device communicating with the tetrachloroethylene feed pipe is arranged in the reactive distillation column.
[0010] By adopting the above technical solution, the spraying device can increase the contact area between tetrachloroethylene and the crude gas.
[0011] Preferably, the spraying device includes an atomizing nozzle, the liquid inlet end of the atomizing nozzle is communicated with the tetrachloroethylene feed pipe, and the spraying direction of the atomizing nozzle is downward.
[0012] By adopting the above technical solution, the atomizing nozzle can disperse the tetrachloroethylene raw material into fine water droplets, form a mist-like spraying water flow, increase the coverage area and reduce the raw material consumption.
[0013] Preferably, the reflux pipeline includes a reflux outer pipe and a reflux inner pipe. The upper end of the reflux outer pipe is connected to the bottom of the reactive distillation column, the lower end of the reflux outer pipe is connected to the upper end of the reflux inner pipe, the reflux inner pipe is located in the fluorination reaction kettle, and the lower end of the reflux inner pipe extends below the lowest liquid level of the fluorination reaction kettle.
[0014] By adopting the above technical solution, the reflux outer pipe and the reflux inner pipe cooperate to fully wash the catalyst entrained by the crude gas back into the fluorination reaction kettle, reduce the loss of the catalyst, and at the same time reduce the corrosion risk to the subsequent pipelines and equipment. The lower end of the reflux inner pipe extends below the lowest liquid level of the fluorination reaction kettle, making the catalytic reaction more thorough.
[0015] Preferably, a regulating valve and a check valve are arranged on the tetrachloroethylene feed pipe, and the check valve is located between the regulating valve and the reactive distillation column.
[0016] By adopting the above technical solution, designed as a check valve, it can prevent the reflux of tetrachloroethylene, and the regulating valve can adjust the feed amount of tetrachloroethylene according to actual needs.
[0017] Preferably, a condenser is arranged in the upper half of the reactive distillation column, and the condenser is connected with a cooling water supply pipeline and a cooling water return pipeline.
[0018] By adopting the above technical solution, the condenser is mainly used to cool the gas discharged from the top of the distillation column, condense the gas-phase components therein into a liquid state for subsequent collection and treatment.
[0019] Preferably, ball valves are arranged on both the discharge pipeline and the reflux pipeline.
[0020] By adopting the above technical solution, ball valves are arranged on the discharge pipeline and the reflux pipeline, which can control the on-off between the reactive distillation column and the fluorination reaction kettle.
[0021] Preferably, the hydrogen fluoride feed pipe includes an outer feed pipe and an inner feed pipe. A ball valve and a check valve are provided on the outer feed pipe. The lower end of the outer feed pipe is connected to the upper end of the inner feed pipe. The inner feed pipe is located in the fluorination reactor, and the lower end of the inner feed pipe extends towards the bottom of the fluorination reactor. The lower end of the inner feed pipe is lower than the lower end of the inner reflux pipe.
[0022] By adopting the above technical solution, hydrogen fluoride flows through the outer feed pipe and the inner feed pipe to the bottom of the fluorination reactor, further making the reaction more complete.
[0023] In summary, the present application includes at least one of the following beneficial technical effects:
[0024] 1. The tetrachloroethylene raw material is fed into the reactive distillation column, improving the utilization rate of chlorine in the crude gas and reducing the consumption of alkali washing.
[0025] 2. By arranging atomizing nozzles in the reactive distillation column, mass transfer and heat transfer between the tetrachloroethylene raw material and the high-temperature crude gas are carried out, reducing the externally supplied heat required for the fluorination reaction and lowering the energy consumption.
[0026] 3. The catalyst entrained by the crude gas is fully washed back into the fluorination reactor, reducing the loss of the catalyst and simultaneously reducing the corrosion risk to the subsequent pipelines and equipment. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] Figure 1 is a schematic structural diagram of a fluorination reaction device in the related art.
[0028] Figure 2 is a schematic structural diagram of the fluorination reaction device in Embodiment 1 of the present application.
[0029] Figure 3 is a schematic structural diagram of the reactive distillation column in Embodiment 2 of the present application.
[0030] Description of the reference numerals: 1, reactive distillation column; 11, tetrachloroethylene feed pipe; 12, condenser; 121, cooling water supply pipeline; 122, cooling water return pipeline; 2, fluorination reactor; 21, hydrogen fluoride feed pipe; 211, outer feed pipe; 212, inner feed pipe; 22, chlorine feed pipe; 3, discharge pipeline; 4, reflux pipeline; 41, outer reflux pipe; 42, inner reflux pipe; 5, spraying device; 51, atomizing nozzle; 6, rotary joint; 7, motor; 8, receiving plate; 81, receiving groove; 9, pressure sensor. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0031] The following is a further detailed description of the present application with reference to the attached Figure 2-3 drawings. Embodiment 1
[0032] As Figure 2As shown in the figure, the fluorination reaction device for trichlorotrifluoroethane includes a reactive distillation column 1 and a fluorination reaction kettle 2.
[0033] In this embodiment, the fluorination reaction kettle 2 is located below the reactive distillation column 1. The fluorination reaction kettle 2 is connected with a hydrogen fluoride feed pipe 21 and a chlorine feed pipe 22.
[0034] Specifically, the chlorine feed pipe 22 is connected to the bottom of the fluorination reaction kettle 2. A ball valve, a regulating valve, a ball valve, a check valve, and a switch valve - ball valve are sequentially arranged on the chlorine feed pipe 22 from the feed end to the fluorination reaction kettle 2, which is used to achieve continuous feeding, adjust the feed flow rate, and prevent the backflow of chlorine.
[0035] The hydrogen fluoride feed pipe 21 includes a feed outer pipe 211 and a feed inner pipe 212. A ball valve and a check valve are arranged on the feed outer pipe 211. Specifically, a ball valve, a switch valve - ball valve, a ball valve, a check valve, and a ball valve are sequentially arranged on the feed outer pipe 211 from the feed end to the fluorination reaction kettle 2. The lower end of the feed outer pipe 211 extends to the top of the fluorination reaction kettle 2 and is connected to the upper end of the feed inner pipe 212. The feed inner pipe 212 is located in the fluorination reaction kettle 2, and the lower end of the feed inner pipe 212 extends towards the bottom of the fluorination reaction kettle 2. Hydrogen fluoride flows to the bottom of the fluorination reaction kettle 2 through the feed outer pipe 211 and the feed inner pipe 212, which further makes the reaction more complete.
[0036] As Figure 2 shown, a discharge pipeline 3 is arranged between the fluorination reaction kettle 2 and the reactive distillation column 1, and a reflux pipeline 4 is arranged between the reactive distillation column 1 and the fluorination reaction kettle 2.
[0037] Specifically, a ball valve is arranged on the discharge pipeline 3. The reflux pipeline 4 includes a reflux outer pipe 41 and a reflux inner pipe 42. The upper end of the reflux outer pipe 41 is connected to the bottom of the reactive distillation column 1, and a ball valve is arranged near the connection between the two. The lower end of the reflux outer pipe 41 is connected to the upper end of the reflux inner pipe 42, and a ball valve is arranged near the connection between the two.
[0038] The reflux inner pipe 42 is located in the fluorination reaction kettle 2. The lower end of the reflux inner pipe 42 extends below the liquid phase of the fluorination reaction kettle 2, and the lower end of the feed inner pipe 212 is lower than the lower end of the reflux inner pipe 42, which makes the catalytic reaction more complete.
[0039] As Figure 2 shown, a perchloroethylene feed pipe 11 is further arranged on the reactive distillation column 1. The connection between the discharge pipeline 3 and the reactive distillation column 1 and the connection between the reflux pipeline 4 and the reactive distillation column 1 are both located below the perchloroethylene feed pipe 11.
[0040] Specifically, for the part of the tetrachloroethylene feed pipe 11 located outside the reactive distillation column 1, a ball valve, a regulating valve, a ball valve, and a check valve are sequentially arranged from the feed end to the reactive distillation column 1 to prevent the backflow of tetrachloroethylene. The regulating valve can adjust the feed rate of tetrachloroethylene according to actual needs.
[0041] Preferably, a spraying device 5 communicating with the tetrachloroethylene feed pipe 11 is arranged inside the reactive distillation column 1. In this embodiment, the spraying device 5 includes an atomizing nozzle 51. The liquid inlet end of the atomizing nozzle 51 is communicated with the tetrachloroethylene feed pipe 11, and the spraying direction of the atomizing nozzle 51 is downward. The atomizing nozzle 51 can disperse the tetrachloroethylene raw material into fine water droplets, forming a mist-like spraying water flow, increasing the coverage area, and reducing the raw material consumption.
[0042] Preferably, a condenser 12 is arranged in the upper half of the reactive distillation column 1 for cooling the gas discharged from the top of the distillation column and condensing the gas-phase components therein into a liquid state. The condenser 12 is connected with a cooling water supply pipeline 121 and a cooling water return pipeline 122.
[0043] A pipeline capable of connecting to subsequent processes is arranged at the top of the reactive distillation column 1.
[0044] The working principle of this embodiment is as follows: The tetrachloroethylene raw material is transported into the reactive distillation column 1 through the tetrachloroethylene feed pipe 11 and forms fine water droplets in the form of a mist through the atomizing nozzle 51, and contacts with the high-temperature crude product gas coming from the bottom of the reactive distillation column 1. Tetrachloroethylene absorbs the unreacted chlorine in the crude product gas and returns it to the fluorination reaction kettle 2. At the same time, it absorbs heat through heat conduction, reduces the externally supplied heat required for the fluorination reaction, reduces the energy consumption, and reduces the fluorination cost. Embodiment 2
[0045] As Figure 3 shown, this embodiment is substantially the same as Embodiment 1, except that in this embodiment, the inner end of the tetrachloroethylene feed pipe 11 extends into the reactive distillation column 1 and is connected to the liquid inlet end of the atomizing nozzle 51 through a rotary joint 6. The motor 7 is used as a driving source to drive the atomizing nozzle 51 to rotate through the rotary joint 6, and the connection between the motor 7 and the rotary joint 6 can be realized through a gear set.
[0046] During fluorination, the motor 7 stops and the atomizing nozzle 51 atomizes normally. When the fluorination ends, the motor 7 drives the atomizing nozzle 51 to rotate, so that the liquid droplets, dirt, etc. at the outlet of the atomizing nozzle 51 are thrown away under the action of centrifugal force, reducing the risk of blockage of the atomizing nozzle 51.
[0047] A material receiving plate 8 is further arranged below the atomizing nozzle 51. The material receiving plate 8 is slidably arranged horizontally in the reactive distillation column 1 and can slide from outside the reactive distillation column 1 into the reactive distillation column 1. A pressure sensor 9 is arranged at the inner end of the material receiving plate 8. The pressure sensor 9 is connected to a controller, and the controller is connected to a motor 7. A material receiving groove 81 is formed on the upper surface of the material receiving plate 8.
[0048] During fluorination, the material receiving plate 8 is located outside the reactive distillation column 1. When fluorination stops, the material receiving plate 8 is pushed to move into the reactive distillation column 1. When the pressure sensor 9 at the inner end of the material receiving plate 8 contacts the inner wall of the reactive distillation column 1, a signal is sent to the controller, and the controller sends an operation instruction to the motor 7 to rotate the atomizing nozzle 51, so as to throw off the liquid droplets and dirt at the outlet of the atomizing nozzle 51, which fall into the material receiving groove 81 of the material receiving plate 8. When the atomizing nozzle 51 is cleaned, the material receiving plate 8 is pulled out. When the pressure sensor 9 does not detect pressure, the controller sends a shutdown instruction to the motor 7.
[0049] The above are all the preferred embodiments of the present application, and the protection scope of the present application is not limited accordingly. Therefore, all equivalent changes made according to the structure, shape and principle of the present application should be covered within the protection scope of the present application.
Claims
1. A fluorination reaction device for trichlorotrifluoroethane, characterized in that, It includes a reactive distillation column (1) and a fluorination reactor (2). The fluorination reactor (2) is connected with a hydrogen fluoride feed pipe (21) and a chlorine feed pipe (22). An outlet pipeline (3) is arranged between the fluorination reactor (2) and the reactive distillation column (1). A reflux pipeline (4) is arranged between the reactive distillation column (1) and the fluorination reactor (2). A tetrachloroethylene feed pipe (11) is also arranged on the reactive distillation column (1). The connection between the outlet pipeline (3) and the reactive distillation column (1) and the connection between the reflux pipeline (4) and the reactive distillation column (1) are both located below the tetrachloroethylene feed pipe (11).
2. The fluorination reaction device for trifluorotrichloroethane according to claim 1, characterized in that, A spraying device (5) communicated with the tetrachloroethylene feed pipe (11) is arranged in the reactive distillation column (1).
3. The fluorination reaction device for trichlorotrifluoroethane according to claim 2, wherein, The spraying device (5) includes an atomizing nozzle (51). The liquid inlet end of the atomizing nozzle (51) is communicated with the tetrachloroethylene feed pipe (11), and the spraying direction of the atomizing nozzle (51) is downward.
4. The fluorination reaction device for trifluorotrichloroethane according to claim 1 or 2 or 3, characterized in that, The reflux pipeline (4) includes a reflux outer pipe (41) and a reflux inner pipe (42). The upper end of the reflux outer pipe (41) is connected with the bottom of the reactive distillation column (1). The lower end of the reflux outer pipe (41) is connected with the upper end of the reflux inner pipe (42). The reflux inner pipe (42) is located in the fluorination reactor (2), and the lower end of the reflux inner pipe (42) extends below the lowest liquid level of the fluorination reactor (2).
5. The fluorination reaction device for trifluorotrichloroethane according to claim 1 or 2 or 3, characterized in that, A regulating valve and a check valve are arranged on the tetrachloroethylene feed pipe (11), and the check valve is located between the regulating valve and the reactive distillation column (1).
6. The fluorination reaction device for trifluorotrichloroethane according to claim 1 or 2 or 3, characterized in that, A condenser (12) is arranged in the upper half of the reactive distillation column (1). The condenser (12) is connected with a cooling water supply pipeline (121) and a cooling water return pipeline (122).
7. The fluorination reaction device for trichlorotrifluoroethane according to claim 1 or 2 or 3, characterized in that, Ball valves are arranged on both the outlet pipeline (3) and the reflux pipeline (4).
8. The fluorination reaction apparatus for trifluorotrichloroethane according to claim 4, wherein The hydrogen fluoride feed pipe (21) includes a feed outer pipe (211) and a feed inner pipe (212). A ball valve and a check valve are arranged on the feed outer pipe (211). The lower end of the feed outer pipe (211) is connected with the upper end of the feed inner pipe (212). The feed inner pipe (212) is located in the fluorination reactor (2), and the lower end of the feed inner pipe (212) extends towards the bottom of the fluorination reactor (2), and the lower end of the feed inner pipe (212) is lower than the lower end of the reflux inner pipe (42).