Process for synthesizing fluorinated phenol by microchannel continuous flow one-step method
Through the combination of the microchannel continuous flow one-step process and the Venturi structure, the problem of low mixing efficiency of raw materials in the fluorinated phenol synthesis process is solved, efficient fluorinated phenol production is achieved, and the purity and quality of the product are improved.
Patent Information
- Application Number
- CN202411677406.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-22
- Publication Date
- 2025-03-28
AI Technical Summary
The existing fluorinated phenol synthesis process is difficult to quickly improve the mixing efficiency of materials during the raw material mixing process, resulting in denaturation and low output efficiency.
The microchannel continuous flow one-step process is adopted to achieve efficient mixing and reaction between phenol and fluoronitride gas through distillation, fluoro-nitrogen mixture mixing, pressurized mixing and distillation separation steps, combined with the use of the Venturi structure and heating tank.
It improves the production efficiency of fluorinated phenol, reduces the generation of impurities, and improves the purity and quality of the product.
Smart Images
Figure CN119707640A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of chemical production, in particular to a process for synthesizing fluorinated phenol by a microchannel continuous flow one-step method. Background Art
[0002] Fluorinated phenol is an important organic compound, widely used in medicine, pesticides, dyes and other fields. Fluorinated phenol can be used as an antibacterial agent, etc. The introduction of fluorine atoms enhances the stability and biological activity of the drug and improves the affinity of the drug to specific biological targets.
[0003] In the prior art, the synthesis process of fluorinated phenol mainly includes photocatalysis, diazotization and other specific chemical synthesis methods. The photocatalysis method is to heat phenol and then introduce a fluorine-nitrogen mixed gas to react under the irradiation of a light source. After the reaction is completed, nitrogen is purged to obtain a crude fluorinated phenol, which is then separated by distillation to obtain different types of fluorinated phenol. The above method does not require solvents or catalysts, and the raw materials are completely converted, the fluorine gas utilization rate is high, and the production cost is low. The diazotization method is to obtain the fluorinated phenol by diazotizing the corresponding aminophenol with sodium nitrite and fluoroboric acid, and then co-heating with appropriate substances.
[0004] However, in the preparation process of the above process, it is inevitable to mix the raw materials. However, in the mixing process of the raw materials of fluorinated phenol, the evaporated vaporized raw materials and the corresponding gases need to be mixed and reacted. In order to ensure the sufficient mixing, neither extending the mixing time nor increasing the power of the mixing equipment can intuitively and quickly improve the mixing efficiency and effect of the materials, which leads to the easy denaturation of the materials during the mixing process, thereby affecting the synthesis output efficiency of fluorinated phenol. In view of this, we propose a microchannel continuous flow one-step synthesis process for fluorinated phenol. Summary of the invention
[0005] The object of the present invention is to provide a process for synthesizing fluorinated phenol in a microchannel continuous flow one-step method to solve the problems raised in the above background technology.
[0006] To achieve the above object, the present invention provides the following technical solution: a process for synthesizing fluorinated phenol by a microchannel continuous flow one-step method, comprising the following steps: S1. Phenol distillation: Phenol is added into a distillation container, and the distillation container is heated to melt the phenol crystals into a liquid state; S2, mixing of fluorine and nitrogen mixed gas: introducing the liquid phenol obtained in S1 into a mixing container through a conduit, and continuously heating and heat-insulating the mixing container, while blowing a mixed gas of fluorine and nitrogen into the mixing container; S3, pressurized mixing: pressurizing the mixing container to fully mix the fluorine gas and nitrogen mixed gas in the mixing container with the phenol, and finally obtaining a crude fluorinated phenol product; S4, distillation separation: the crude fluorinated phenol product obtained in S3 is introduced into a distillation container through a conduit, the distillation container is heated in batches, and filtered to obtain a fluorinated phenol product.
[0007] Preferably, the distillation container, mixing container and distillation container are all provided with an exhaust gas treatment structure, and the exhaust gas treatment structure includes a cooling component and a waste gas treatment component. The cooling component uses cooling water filled in a closed pipeline and continuously cools the exhaust gas generated in the distillation container, mixing container and distillation container through a circulating pump. The waste gas treatment component uses an aeration treatment device to treat the exhaust gas. The ends of the exhaust gas pipes corresponding to the distillation container, mixing container and distillation container are located at the bottom of the aeration treatment device, thereby achieving purification of the exhaust gas generated in the production process of fluorinated phenol, avoiding the generation of a large amount of toxic gases in the industrial production process to damage the surrounding environment.
[0008] Preferably, a pressure relief structure is provided on the top of the distillation container, and a heating pool is provided on the outside of the distillation container. The interior of the heating pool is filled with heat transfer oil, and the depth of the heat transfer oil is higher than the height of the heating chamber in the distillation container, so that the distillation container adopts a constant temperature heating method when heating the phenol raw material placed therein. The boiling point of phenol is 182°C, and the maximum operating temperature of the heat transfer oil exceeds 400°C. Therefore, it can ensure the steady heating of the distillation container and prevent the heat transfer oil from evaporating on its own, thereby ensuring that the phenol in the distillation container can evaporate into a gaseous state to better participate in the subsequent mixing reaction.
[0009] Preferably, the S2 fluorine-nitrogen mixed gas is premixed using a venturi structure before being introduced into the mixing container. The venturi structure includes a large tube and a small tube. The diameter of the small tube is set to be one-fourth of the large tube. There are two groups of large tubes, and the two groups of large tubes are fixedly connected to the two ends of the small tube, respectively, to form a premixed structure with thick ends and thin middle. The fluorine gas and nitrogen gas enter the large tube through pipelines respectively. When passing through the small tube, the air flow rate changes due to the narrowing of the pipeline channel to promote the mixing effect of fluorine gas and nitrogen in the small tube. An atomizing port is fixedly connected between the conduits of the mixing container and the distillation container. A three-way pipe is used between the atomizing port, the venturi structure and the feed port of the mixing container, so that the atomized phenol can fully react with the fluorine gas, and nitrogen is used as a protective gas to ensure the safety of the reaction and finally enters the mixing container.
[0010] Preferably, when the mixed gas is blown in S2, fluorine gas and nitrogen gas are blown in separately, and the blowing inlets of fluorine gas and nitrogen gas are provided with solenoid valves to control the blowing timing and total amount of fluorine gas and nitrogen gas, and a constant temperature pool filled with heat transfer oil is provided on the outside of the mixing container, and the blowing pipes of the fluorine gas and nitrogen gas are provided with a heating section, and the heating section is arranged inside the constant temperature pool, so as to ensure that the temperature of the mixing container will not drop too quickly due to the blowing of gas and cause crystallization, and the blown reaction gas is preheated to ensure the reaction effect between phenol and fluorine gas.
[0011] Preferably, the nitrogen pipe blown in S2 is also connected to a circulation pipe, and the end of the circulation pipe away from the nitrogen pipe is connected to the connecting port between the three-way pipe and the mixing container, so that the residual gas generated during the continuous reaction between phenol and the fluorine-nitrogen mixed gas can flow back into the blowing part of the nitrogen pipe through the circulation pipe again, and a one-way valve is arranged between the nitrogen blowing pipe and the nitrogen supply equipment to avoid the reflux of waste gas caused by excessive gas pressure during the reaction, which affects the safe use of the external gas supply equipment.
[0012] Preferably, the phenol raw material used in S1 also includes a pretreatment step before distillation, wherein phenol is put into a distiller, and an appropriate amount of pure water is added, the distiller is heated, the temperature is set at 120°C, and the heating of the distiller is gradually increased in intervals of 20°C, and finally a phenol distillation product is obtained after filtration and separation, and then the phenol distillation product is put into the distillation container in S1 for production, thereby ensuring the purity of the phenol raw material itself, reducing impurities, thereby ensuring the purity of the fluorinated phenol product, and improving the product quality.
[0013] Preferably, during the pressurized mixing in S3, air blowing and pressurization are used to increase the air pressure in the mixing container to ensure that the air pressure in the mixing container is between 1.5 and 2 standard atmospheres, and nitrogen is used for the air blowing and pressurization. A reflux pipe is provided at the bottom of the mixing container and is connected to a circulation pipeline, and a one-way valve is provided on the reflux pipe so that the gas in the mixing container can only flow toward the reflux pipe, and the gas in the circulation pipeline will not flow back in the reverse direction, thereby ensuring that the reaction in the mixing container is always under a slightly higher pressure, so as to promote the mixing reaction between phenol and fluorine gas and improve the production efficiency of the device.
[0014] Preferably, the distillation container, mixing container and distillation container are all connected by glass pipes, and the distillation container, mixing container and distillation container all adopt a sealing structure, and the outer side of the glass pipe is provided with a heat preservation structure, and the heat preservation structure adopts heat preservation cotton wrapped with a layer of tin foil to reduce the gas blowing into the reaction and the pre-cooling and direct crystallization of the distilled gasified phenol, so as to ensure the stability of the material transmission required for the reaction.
[0015] Preferably, the large tube, small tube and mixing container included in the venturi structure are all made of transparent glass material, and lighting equipment is used to illuminate the venturi structure during the introduction of the fluorine-nitrogen mixed gas in S2 to avoid the equipment itself from blocking the light, thereby catalyzing the reaction of phenol and the fluorine-nitrogen mixed gas to ensure the output of the fluorinated phenol product.
[0016] Compared with the prior art, the present invention provides a process for synthesizing fluorinated phenol in a microchannel continuous flow one-step method, which has the following beneficial effects: 1. The microchannel continuous flow one-step synthesis process of fluorinated phenol uses a glass pipe to connect a distillation container, a mixing container and a rectification container in series to make the preparation process of fluorinated phenol simpler. At the same time, a Venturi structure is used to atomize liquid phenol during the blowing process of the fluorine-nitrogen mixed gas. Then, the Venturi principle is used to promote the rapid and efficient mixing of the atomized phenol and the fluorine-nitrogen mixed gas in the small tube, thereby improving the production efficiency of fluorinated phenol, reducing the generation of impurities, and further improving the purity of the subsequent fluorinated phenol products.
[0017] 2. The process for synthesizing fluorinated phenol by one-step microchannel continuous flow is characterized in that a heating pool and a constant temperature pool are respectively arranged on the outside of the distillation container and the mixing container, so that the temperature rise in the distillation container and the mixing container is more stable. At the same time, the circulation pipeline and the supply pipelines of fluorine gas and nitrogen gas are all provided with heating sections immersed in the constant temperature pool to ensure that the temperature of the mixing container will not drop too quickly due to the blowing of gas and crystallization will not occur, and the blown reaction gas is preheated to ensure the reaction effect between phenol and fluorine gas.
[0018] 3. The microchannel continuous flow one-step synthesis process of fluorinated phenol reduces the gas blowing reaction and the pre-cooling and direct crystallization of the distilled gasified phenol by providing a heat preservation structure on the outside of the distillation container, the mixing container and the rectification container, thereby ensuring the stability of the material transmission required for the reaction. BRIEF DESCRIPTION OF THE DRAWINGS
[0019] Figure 1 It is a schematic diagram of the production process of the present invention. DETAILED DESCRIPTION
[0020] like Figure 1 As shown, the present invention provides a technical solution: a process for synthesizing fluorinated phenol by a microchannel continuous flow one-step method, comprising the following steps: S1. Phenol distillation: adding phenol raw material into a distillation container, and heating the distillation container to melt phenol crystals into liquid; S2, mixing of fluorine and nitrogen mixed gas: introducing the liquid phenol obtained in S1 into a mixing container through a conduit, and continuously heating and heat-insulating the mixing container, while blowing a mixed gas of fluorine and nitrogen into the mixing container; S3, pressurized mixing: pressurizing the mixing container to fully mix the fluorine gas and nitrogen mixed gas in the mixing container with the phenol, and finally obtaining a crude fluorinated phenol product; S4, distillation separation: the crude fluorinated phenol product obtained in S3 is introduced into a distillation container through a conduit, the distillation container is heated in batches, and filtered to obtain a fluorinated phenol product.
[0021] In one embodiment of the present invention, the distillation container, the mixing container and the distillation container are all provided with an exhaust gas treatment structure, and the exhaust gas treatment structure includes a cooling component and a waste gas treatment component. The cooling component uses cooling water filled in a closed pipeline and continuously cools the waste gas generated in the distillation container, the mixing container and the distillation container through a circulating pump. The waste gas treatment component uses an aeration treatment device to treat the waste gas. The ends of the waste gas pipes corresponding to the distillation container, the mixing container and the distillation container are located at the bottom of the aeration treatment device, thereby achieving purification of the waste gas generated in the production process of fluorinated phenol, avoiding the generation of a large amount of toxic gases in the industrial production process to the surrounding The environment is damaged. At the same time, a pressure relief structure is arranged on the top of the distillation container, and a heating pool is arranged on the outside of the distillation container. The interior of the heating pool is filled with heat transfer oil, and the depth of the heat transfer oil is higher than the height of the heating chamber in the distillation container, so that the distillation container heats the phenol raw material placed therein by constant temperature heating. The boiling point of phenol is 182°C, and the maximum operating temperature of the heat transfer oil exceeds 400°C. Therefore, it can ensure the steady heating of the distillation container and prevent the heat transfer oil from evaporating by itself, thereby ensuring that the phenol in the distillation container can evaporate into a gaseous state to better participate in the subsequent mixing reaction.
[0022] Furthermore, the S2 fluorine-nitrogen mixed gas is premixed using a venturi structure before being introduced into the mixing container. The venturi structure includes a large tube and a small tube. The diameter of the small tube is set to be one-fourth of the large tube. There are two groups of large tubes, and the two groups of large tubes are fixedly connected to the two ends of the small tube, respectively, to form a premixed structure with thick ends and thin middle. The fluorine gas and the nitrogen gas enter the large tube through pipelines respectively. When passing through the small tube, the air flow rate changes due to the narrowing of the pipeline channel to promote the mixing effect of the fluorine gas and the nitrogen gas in the small tube. An atomizing port is fixedly connected between the conduits of the mixing container and the distillation container. A three-way pipe is used between the atomizing port, the venturi structure and the feed port of the mixing container, so that the atomized phenol can fully react with the fluorine gas, and the nitrogen gas is used as a protective gas to ensure the safety of the reaction and finally enters the mixing container.
[0023] In addition, when the mixed gas is blown in S2, the fluorine gas and the nitrogen gas are blown in separately, and the blowing inlets of the fluorine gas and the nitrogen gas are both provided with solenoid valves to control the blowing timing and the total amount of the fluorine gas and the nitrogen gas. A constant temperature pool filled with heat transfer oil is provided on the outside of the mixing container, and the blowing pipes of the fluorine gas and the nitrogen gas are both provided with a heating section, which is arranged inside the constant temperature pool, so as to ensure that the temperature of the mixing container will not drop too quickly due to the blowing of the gas and cause crystallization, and the blown reaction gas is preheated to ensure the reaction effect between phenol and fluorine gas.
[0024] In an embodiment of the present invention, the nitrogen pipe blown into S2 is also connected to a circulation pipe, and one end of the circulation pipe away from the nitrogen pipe is connected to the connection port between the three-way pipe and the mixing container, so that the residual gas generated during the continuous reaction between phenol and the fluorine-nitrogen mixed gas is refluxed into the blowing part of the nitrogen pipe through the circulation pipe again, and a one-way valve is arranged between the nitrogen blowing pipe and the nitrogen supply equipment to avoid the reflux of waste gas caused by excessive gas pressure during the reaction, which affects the safe use of the external gas supply equipment. At the same time, the phenol raw material used in S1 also includes a pretreatment step before distillation, in which phenol is put into a distiller, and an appropriate amount of pure water is added, and the distiller is heated. The temperature is set at 120°C, and the heating of the distiller is gradually increased in intervals of 20°C. Finally, after filtration and separation, a phenol distillation product is obtained, and then the phenol distillation product is put into the distillation container in S1 for production, thereby ensuring the purity of the phenol raw material itself, reducing impurities, thereby ensuring the purity of the fluorinated phenol product, and improving the product quality.
[0025] In the present invention, during the pressurized mixing in S3, the air pressure in the mixing container is increased by blowing and pressurizing, ensuring that the air pressure in the mixing container is between 1.5 and 2 standard atmospheres, and nitrogen is used for blowing and pressurizing. A reflux pipe is provided at the bottom of the mixing container and is connected to a circulation pipeline, and a one-way valve is provided on the reflux pipe, so that the gas in the mixing container can only flow toward the reflux pipe, and the gas in the circulation pipeline will not flow back in reverse, thereby ensuring that the reaction in the mixing container is always under a slightly higher pressure, so as to promote the mixing reaction between phenol and fluorine gas and improve the production efficiency of the device.
[0026] It is worth noting that the distillation container, mixing container and distillation container are all connected by glass pipes, and the distillation container, mixing container and distillation container are all sealed. The outside of the glass pipe is provided with an insulation structure, and the insulation structure uses insulation cotton wrapped with a layer of tin foil to reduce the gas blowing into the reaction and the pre-cooling and direct crystallization of the distilled gasified phenol, so as to ensure the stability of the material transmission required for the reaction. Furthermore, the large tube, small tube and mixing container included in the venturi structure are all made of transparent glass material, and lighting equipment is used to illuminate the venturi structure during the introduction of the fluorine-nitrogen mixed gas in S2 to avoid the equipment itself from blocking the light, thereby catalyzing the reaction of phenol and the fluorine-nitrogen mixed gas to ensure the output of fluorinated phenol products.
[0027] The above generally describes the present invention in detail, but it is obvious to a person skilled in the art that some modifications or improvements can be made to the present invention. Therefore, modifications or improvements that do not depart from the spirit of the present invention are within the scope of protection of the present invention.
Claims
1. A process for synthesizing fluorinated phenol by a microchannel continuous flow one-step method, characterized in that: The following steps are involved: S1. Phenol distillation: adding phenol raw material into a distillation container, and heating the distillation container to melt phenol crystals into liquid; S2, mixing of fluorine and nitrogen mixed gas: introducing the liquid phenol obtained in S1 into a mixing container through a conduit, and continuously heating and heat-insulating the mixing container, while blowing a mixed gas of fluorine and nitrogen into the mixing container; S3, pressurized mixing: pressurizing the mixing container to fully mix the fluorine gas and nitrogen mixed gas in the mixing container with the phenol, and finally obtaining a crude fluorinated phenol product; S4, distillation separation: the crude fluorinated phenol product obtained in S3 is introduced into a distillation container through a conduit, the distillation container is heated in batches, and filtered to obtain a fluorinated phenol product.
2. The process for synthesizing fluorinated phenol by a microchannel continuous flow one-step method according to claim 1, characterized in that: The distillation container, mixing container and distillation container are all provided with an exhaust gas treatment structure, and the exhaust gas treatment structure includes a cooling component and a waste gas treatment component. The cooling component uses cooling water filled in a closed pipeline and continuously cools the waste gas generated in the distillation container, mixing container and distillation container through a circulating pump. The waste gas treatment component uses an aeration treatment device to treat the waste gas, and the ends of the waste gas pipes corresponding to the distillation container, mixing container and distillation container are located at the bottom of the aeration treatment equipment.
3. The process for synthesizing fluorinated phenol by a microchannel continuous flow one-step method according to claim 1, characterized in that: A pressure relief structure is arranged on the top of the distillation container, and a heating pool is arranged outside the distillation container. The interior of the heating pool is filled with heat transfer oil, and the depth of the heat transfer oil is higher than the height of the heating chamber in the distillation container.
4. The process for synthesizing fluorinated phenol by a microchannel continuous flow one-step method according to claim 1, characterized in that: The S2 fluorine-nitrogen mixed gas is premixed using a venturi structure before being introduced into the mixing container. The venturi structure includes a large tube and a small tube. The diameter of the small tube is set to be one-fourth of the large tube. There are two groups of large tubes, and the two groups of large tubes are fixedly connected to the two ends of the small tube, respectively, to form a premixed structure with thick ends and a thin middle. The fluorine gas and nitrogen gas enter the large tube through pipelines respectively. An atomizing port is fixedly connected between the conduits of the mixing container and the distillation container. A three-way pipe is used between the atomizing port, the venturi structure and the feed port of the mixing container.
5. The process for synthesizing fluorinated phenol by a microchannel continuous flow one-step method according to claim 1, characterized in that: When the mixed gas is blown into S2, the fluorine gas and the nitrogen gas are blown in separately, and the blowing inlets of the fluorine gas and the nitrogen gas are both provided with solenoid valves to control the blowing timing and the total amount of the fluorine gas and the nitrogen gas. A constant temperature pool filled with heat transfer oil is provided on the outside of the mixing container, and the blowing pipes of the fluorine gas and the nitrogen gas are both provided with a heating section, and the heating section is arranged inside the constant temperature pool.
6. The process for synthesizing fluorinated phenol by a microchannel continuous flow one-step method according to claim 4, characterized in that: The nitrogen pipe blown into the S2 is also connected to a circulation pipe, and one end of the circulation pipe away from the nitrogen pipe is connected to the connecting port between the three-way pipe and the mixing container. A one-way valve is provided between the nitrogen blowing pipe and the nitrogen supply device.
7. The process for synthesizing fluorinated phenol by a one-step microchannel continuous flow method according to claim 1, characterized in that: The phenol raw material used in S1 also includes a pretreatment step before distillation, in which phenol is put into a distiller, and a proper amount of pure water is added, and the distiller is heated. The temperature is set at 120°C, and the temperature of the distiller is increased stepwise in intervals of 20°C. Finally, a phenol distillation product is obtained after filtration and separation, and then the phenol distillation product is put into the distillation container in S1 for production.
8. The process for synthesizing fluorinated phenol by a one-step microchannel continuous flow method according to claim 6, characterized in that: When the pressurized mixing is performed in S3, the air pressure in the mixing container is increased by blowing pressurization to ensure that the air pressure in the mixing container is between 1.5 and 2 standard atmospheres, and nitrogen is used for the blowing pressurization. A reflux pipe is provided at the bottom of the mixing container and is connected to the circulation pipe, and a one-way valve is provided on the reflux pipe.
9. The process for synthesizing fluorinated phenol by a microchannel continuous flow one-step method according to claim 1, characterized in that: The distillation container, the mixing container and the rectification container are all connected by glass pipes, and the distillation container, the mixing container and the rectification container are all sealed. The outer side of the glass pipe is provided with a heat preservation structure, and the heat preservation structure adopts heat preservation cotton wrapped with a layer of tin foil.
10. The process for synthesizing fluorinated phenol by a microchannel continuous flow one-step method according to claim 4, characterized in that: The large tube, small tube and mixing container included in the Venturi structure are all made of transparent glass material, and lighting equipment is used to illuminate the Venturi structure during the introduction of the fluorine-nitrogen mixed gas in S2.