Reaction device for preparing acid through continuous catalytic oxidation of methyl and fluorine substituted aromatic hydrocarbon
By designing a reaction device including a microchannel plate reactor and an inorganic vaporization permeable membrane dehydration unit, the problem that moisture affects the performance of the catalyst in the oxidation reaction is solved, and efficient continuous conversion of raw materials and stability of reaction are achieved.
Patent Information
- Application Number
- CN202420907185.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-29
- Publication Date
- 2025-02-25
- Estimated Expiration
- 2034-04-29
AI Technical Summary
In the prior art, water generated during the oxidation reaction affects the performance of the catalyst, resulting in a slower reaction speed, and the one-way conversion rate can only reach 20-30%, making it difficult to achieve continuous reaction.
A reaction device for the continuous catalytic oxidation of methyl and fluorine-containing aromatic hydrocarbons is designed, and a micro-channel plate reactor is used to combine a thermopressure regulator, a post-reaction material gas-liquid separator, a gas-phase superheater and an inorganic vaporization permeable membrane dehydration unit. , realize continuous online reaction and continuous dehydration, and remove moisture from the reaction system.
Through this device, the one-way conversion rate of raw materials can be increased to more than 60%, ensuring stable reaction speed, achieving continuous reaction, and reducing post-treatment load.
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Figure CN222518532U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to a continuous oxidation reaction device, in particular to a reaction device for preparing acid by continuous catalytic oxidation of methyl- and fluorine-substituted aromatic hydrocarbons. Background Art
[0002] When preparing the corresponding acids from methyl- and fluorine-substituted aromatic hydrocarbons such as 2-chloro-6-fluorotoluene, p-fluorotoluene, and m-fluorotoluene, conventional methods include electrolytic oxidation, chlorination hydrolysis, halogen exchange, and direct oxidation with air or oxygen.
[0003] Electrolytic oxidation is divided into direct electrolytic oxidation and indirect electrolytic oxidation. Direct electrolytic oxidation refers to the oxidation reaction of the reactants directly on the electrode to obtain the final product; indirect electrolytic oxidation refers to the electron exchange between the second substance other than the reactants and the electrode, and then the substance and the reactants exchange electrons in the reactor outside the tank to produce a redox reaction to obtain the product. The disadvantage of direct electrolytic oxidation is that organic matter is easily adsorbed by the electrode during electrolysis, affecting the electrolysis; in the indirect oxidation method, since the reaction is outside the tank, the oily organic matter will not directly contact the electrode, so it will not be adsorbed on the electrode surface to affect the electrolytic reaction. However, this process has high equipment requirements and high technical difficulty, and it is still difficult to achieve industrialization.
[0004] Oxygen (or air) oxidation method refers to the catalytic oxidation reaction of methyl- and fluorine-substituted aromatic hydrocarbons such as 2-chloro-6-fluorotoluene, p-fluorotoluene, and m-fluorotoluene in an atmosphere of oxygen or air. This method is simple in process, has no pollution to the environment, and is a green and clean process.
[0005] The invention of CN115677481A "A method for preparing p-fluorobenzoic acid from p-fluorotoluene" states: add a certain amount of acetic acid to p-fluorotoluene and add an appropriate amount of catalyst (cobalt acetate); after heating, start passing oxygen to maintain the pressure; after keeping warm, cool to room temperature; filter, wash with a small amount of ice water; and dry at high temperature to obtain white flaky p-fluorobenzoic acid.
[0006] The invention of CN106748686A "A method for preparing p-fluorobenzaldehyde by continuous oxidation of fluorotoluene" states: p-fluorotoluene compound is used as raw material, one or more metal ion complexes of cobalt, molybdenum and bromine are used as catalysts, hydrogen peroxide is used as oxidant, acetic acid is used as solvent, and p-fluorotoluene is continuously oxidized in a tubular reactor to prepare p-fluorobenzaldehyde.
[0007] The invention of CN106565445A "Method for preparing p-fluorobenzaldehyde" states: p-fluorotoluene is used as a raw material, and p-fluorobenzaldehyde is prepared by catalytic oxidation; the catalyst is arbitrarily selected from one of a manganese compound, a cobalt compound, and an iron compound, and the co-catalyst is any one of a bromide; the reaction solvent is any one of acetic acid or acetonitrile.
[0008] Since water is produced during the oxidation reaction, it affects the performance of the catalyst, causing the reaction rate to slow down. In severe cases, the reaction must be stopped and the single-pass conversion rate can only reach 20-30%. Therefore, it is necessary to stop the reaction for post-processing, and then return the unreacted raw materials to the reaction system, resulting in the inability to achieve continuous reaction.
[0009] Therefore, how to improve the single-pass conversion efficiency of raw materials is the key to the technology, and it is also a key problem to improve production efficiency, reduce production costs and post-processing load. Utility Model Content
[0010] The technical problem to be solved by the utility model is to provide a reaction device for preparing acid by continuous catalytic oxidation of methyl- and fluorine-substituted aromatic hydrocarbons.
[0011] In order to solve the above technical problems, the utility model provides a reaction device for preparing acid by continuous catalytic oxidation of methyl- and fluorine-substituted aromatic hydrocarbons, comprising a liquid oxygen storage tank, a liquid oxygen vaporizer, an oxygen buffer tank, an oxygen pressure reducing valve, an oxygen booster pump, a raw material storage tank, a feed pump, an oxygen flow meter, a raw material flow meter, a gas-liquid mixer, a raw material preheater, a microchannel plate reactor, a temperature and pressure regulator, a gas-liquid separator for materials after reaction, a gas phase superheater, an inorganic vaporization permeation membrane dehydration unit, a condenser, a permeate gas-liquid separator and a vacuum pump;
[0012] The liquid oxygen storage tank, the pipeline with a regulating valve, the liquid oxygen vaporizer, the pipeline with a valve, the oxygen buffer tank, the oxygen pressure reducing valve, the pipeline with a regulating valve and the inlet of the oxygen booster pump are connected in sequence; the outlet of the oxygen booster pump is connected to the inlet of the gas-liquid mixer after passing through the oxygen flow meter;
[0013] The raw material storage tank is connected to the inlet of the feed pump through a pipeline with a regulating valve; the outlet of the feed pump is connected to the inlet of the gas-liquid mixer after passing through the raw material flow meter;
[0014] The outlet of the gas-liquid mixer, the raw material preheater, and the inlet of the microchannel plate reactor are connected in sequence; a back pressure regulating valve is provided at the outlet of the microchannel plate reactor, and then connected to the inlet of the post-reaction material gas-liquid separator through a temperature and pressure regulator;
[0015] After the reaction, a valve is provided at the liquid phase outlet of the gas-liquid separator of the material, and then it is divided into two paths, one is a discharge port with a valve, and the other is connected to the inlet of the feed pump through a pipeline with a valve;
[0016] The gas phase outlet of the gas-liquid separator of the reacted material, the gas phase superheater, the pipeline with a valve, and the inlet of the inorganic vaporization permeation membrane dehydration unit are connected in sequence;
[0017] The water vapor outlet of the inorganic vaporization permeation membrane dehydration unit, the condenser, and the inlet of the permeate liquid gas-liquid separator are connected in sequence, and the gas outlet of the permeate liquid gas-liquid separator is connected to the vacuum pump.
[0018] The gas outlet of the inorganic vaporization permeation membrane dehydration unit is connected to the inlet of the oxygen booster pump through a pipeline with a regulating valve.
[0019] As an improvement of the reaction device for preparing acid by continuous catalytic oxidation of methyl- and fluorine-substituted aromatic hydrocarbons of the utility model: a thermometer and a pressure gauge are respectively arranged on the pipeline connecting the raw material preheater and the microchannel plate reactor.
[0020] As a further improvement of the reaction device for preparing acid by continuous catalytic oxidation of methyl- and fluorine-substituted aromatic hydrocarbons of the utility model: the liquid outlet of the permeate gas-liquid separator is connected to the permeate storage tank through a pipeline with a valve.
[0021] As a further improvement of the reaction device for preparing acid by continuous catalytic oxidation of methyl- and fluorine-substituted aromatic hydrocarbons of the utility model: a heat medium pipeline and a reaction pipeline are respectively arranged in the microchannel plate reactor, and the heat medium enters the heat medium pipeline in the microchannel plate reactor from the heat medium inlet and is then discharged from the heat medium outlet;
[0022] The temperature and pressure regulator is provided with a medium pipeline and a material pipeline respectively. The medium enters the medium pipeline of the temperature and pressure regulator from the medium inlet and is discharged from the medium outlet.
[0023] The gas phase superheater is provided with a steam pipeline and a material pipeline. The steam enters the steam pipeline from the steam inlet and is discharged from the steam outlet.
[0024] The condenser is provided with a refrigerant pipeline and a material pipeline. The refrigerant enters the refrigerant pipeline from the refrigerant inlet and is discharged from the refrigerant outlet.
[0025] As a further improvement of the reaction device for preparing acid by continuous catalytic oxidation of methyl- and fluorine-substituted aromatic hydrocarbons of the utility model: a raw material preheater, a pipeline with a thermometer and a pressure gauge, and an inlet of a reaction pipeline in a microchannel plate reactor are connected in sequence; a back pressure regulating valve is provided at the outlet of the reaction pipeline in the microchannel plate reactor; the outlet of the reaction pipeline in the microchannel plate reactor is connected in sequence to the inlet of a gas-liquid separator of the material after the reaction through the back pressure regulating valve and then through the material pipeline in the temperature and pressure regulator;
[0026] After the reaction, the gas phase outlet of the gas-liquid separator is connected to the material pipeline in the gas phase superheater.
[0027] Through a large number of experiments and technical improvements, the utility model finds that the key factor affecting the reaction speed is the water content in the reaction system, so how to continuously remove the water in the reaction system is the decisive factor.
[0028] The reaction device of the utility model mainly comprises a microchannel plate reactor, and a subsequent temperature and pressure regulator, a gas-liquid separator for materials after reaction, a gas phase superheater and an inorganic vaporization permeation membrane dehydration unit. The materials obtained by the reaction are azeotropically watered through the temperature and pressure regulator, the gas-liquid separator for materials after reaction separates the materials of the reactants into a liquid phase and a water phase, and the steam in the gas phase is dehydrated through the inorganic vaporization permeation membrane dehydration unit, thereby removing the water generated by the reaction from the system, thereby realizing the continuity of the reaction, ensuring the stability of the reaction speed, and the single-pass conversion rate of the raw materials can be increased to more than 60%.
[0029] The main technical points of the utility model are to couple the reaction process and the post-treatment process, and to add a temperature and pressure regulator, a gas-liquid separator for post-reaction materials, a gas phase superheater and an inorganic vaporization permeation membrane dehydration unit to the microchannel plate reactor to remove the water generated by the reaction from the system.
[0030] The reaction end point of the utility model is that the target product contains fluorine-substituted aromatic acid ≥60%; by sampling and analyzing (gas chromatography), continuous harvesting can be performed when the specified ratio (≥60%) is reached.
[0031] The technical advantages of this utility model are:
[0032] 1. The microchannel plate reaction and inorganic vaporization permeation membrane dehydration unit are coupled to realize online continuous reaction and continuous dehydration, improve the reaction rate and raw material conversion efficiency, and the single-pass conversion rate of the target product can be stabilized at 60%;
[0033] 2. Combine the azeotropic distillation unit and the inorganic vaporization permeation membrane dehydration unit to improve the dehydration efficiency. BRIEF DESCRIPTION OF THE DRAWINGS
[0034] The specific implementation of the utility model is further described in detail below with reference to the accompanying drawings.
[0035] Figure 1 The utility model is a schematic diagram of a reaction device for preparing acid by continuous catalytic oxidation of methyl- and fluorine-substituted aromatic hydrocarbons. DETAILED DESCRIPTION
[0036] The present invention is further described below in conjunction with specific embodiments, but the protection scope of the present invention is not limited thereto:
[0037] Embodiment 1, a reaction device for preparing acid by continuous catalytic oxidation of methyl- and fluorine-substituted aromatic hydrocarbons, comprising a liquid oxygen storage tank 1, a liquid oxygen vaporizer 2, an oxygen buffer tank 3, an oxygen pressure reducing valve 4, an oxygen booster pump 5, a raw material storage tank 6, a feed pump 7, an oxygen flow meter 8, a raw material flow meter 9, a gas-liquid mixer 10, a raw material preheater 11, a thermometer 12, a pressure gauge 13, a microchannel plate reactor 14, a temperature and pressure regulator 15, a post-reaction material gas-liquid separator 16, a gas phase superheater 17, an inorganic vaporization permeation membrane dehydration unit 18, a condenser 19, a permeate gas-liquid separator 20 and a vacuum pump 21.
[0038] The inorganic vaporization permeation membrane dehydration unit 18 uses a conventional inorganic vaporization permeation membrane, such as that available from Jiangsu Jiutian High-Tech.
[0039] A heat medium pipeline and a reaction pipeline are respectively arranged in the microchannel plate reactor 14. The heat medium enters the heat medium pipeline from the heat medium inlet 14-1 and is discharged from the heat medium outlet 14-2, thereby providing a heat source for the reaction in the reaction pipeline.
[0040] The temperature and pressure regulator 15 is provided with a medium pipeline and a material pipeline respectively. The medium enters the medium pipeline from the medium inlet 15-1 and is discharged from the medium outlet 15-2, thereby adjusting the temperature of the reacted material; so that the water in the reacted material and the raw material can be azeotropically vaporized, thereby reducing the moisture content of the lower liquid phase part of the reacted material gas-liquid separator 16.
[0041] The gas phase superheater 17 is provided with a steam pipe and a material pipe respectively. The steam enters the steam pipe from the steam inlet 17-1 and is discharged from the steam outlet 17-2, thereby increasing the temperature of the gas phase material provided by the gas-liquid separator 16 after the reaction (thereby ensuring that the water and raw materials in the gas phase material are not condensed into liquid).
[0042] The condenser 19 is provided with a refrigerant pipeline and a material pipeline respectively. The refrigerant enters the refrigerant pipeline from the refrigerant inlet 19-1 and is discharged from the refrigerant outlet 19-2, thereby condensing the components in the material pipeline.
[0043] The liquid oxygen storage tank 1, the pipeline with the regulating valve 1-1, the liquid oxygen vaporizer 2, the pipeline with the valve 3-1, the oxygen buffer tank 3, the oxygen pressure reducing valve 4, the pipeline with the regulating valve 5-1 and the inlet of the oxygen booster pump 5 are connected in sequence; the outlet of the oxygen booster pump 5 is connected to the inlet of the gas-liquid mixer 10 after passing through the oxygen flowmeter 8;
[0044] The raw material storage tank 6 is connected to the inlet of the feed pump 7 through a pipeline with a regulating valve 6-1; the outlet of the feed pump 7 is connected to the inlet of the gas-liquid mixer 10 after passing through the raw material flow meter 9;
[0045] The outlet of the gas-liquid mixer 10, the raw material preheater 11, the pipeline with the thermometer 12 and the pressure gauge 13, and the inlet of the reaction pipeline in the microchannel plate reactor 14 are connected in sequence; the outlet of the reaction pipeline in the microchannel plate reactor 14 is provided with a back pressure regulating valve 14-3, and then connected in sequence with the inlet of the post-reaction material gas-liquid separator 16 through the material pipeline in the temperature and pressure regulator 15;
[0046] A valve 16-1 is provided at the liquid phase outlet of the gas-liquid separator 16 of the reacted material, and then it is divided into two paths, one is a discharge port with a valve 16-2, and the other is connected to the inlet of the feed pump 7 through a pipeline with a valve 16-3; the valve 16-2 is a discharge control valve for the qualified reaction material. When the content of the reacted material product reaches the specified ratio, it is discharged into the post-processing process through the discharge port with the valve 16-2 for refining and purification.
[0047] The gas phase outlet of the gas-liquid separator 16 of the reacted material, the material pipeline in the gas phase superheater 17, the pipeline with the valve 17-3, and the inlet of the inorganic vaporization permeation membrane dehydration unit 18 are connected in sequence;
[0048] The water vapor outlet of the inorganic vaporization permeation membrane dehydration unit 18, the material pipeline in the condenser 19, and the inlet of the permeate liquid gas-liquid separator 20 are connected in sequence, the gas outlet of the permeate liquid gas-liquid separator 20 is connected to the vacuum pump 21, and the liquid outlet of the permeate liquid gas-liquid separator 20 is connected to the permeate storage tank through a pipeline with a valve 20-1.
[0049] The gas outlet of the inorganic vaporization permeation membrane dehydration unit 18 is connected to the inlet of the oxygen booster pump 5 through a pipeline with a regulating valve 5-2.
[0050] When the above-mentioned device is working, the flow rate of the mixed oxygen entering the gas-liquid mixer 10 (including the oxygen provided by the liquid oxygen storage tank 1 + the circulating oxygen dehydrated by the inorganic vaporization permeable membrane dehydration unit 18) is set to be 50 to 100 times the flow volume of the reaction mixed raw materials entering the gas-liquid mixer 10 (including the raw materials with catalyst provided by the raw material storage tank 6 + the liquid phase obtained by the post-reaction material gas-liquid separator 16).
[0051] The working process is as follows:
[0052] 1. The liquid oxygen in the liquid oxygen storage tank 1 enters the liquid oxygen vaporizer 2 through a pipeline with a regulating valve 1-1 for vaporization (the vaporization temperature is 35±5°C), and the vaporized oxygen enters the oxygen buffer tank 3 through a pipeline with a valve 3-1; the oxygen in the oxygen buffer tank 3 is decompressed (decompressed to 0.25±0.05Mpa) after passing through the oxygen pressure reducing valve 4, and then enters the oxygen booster pump 5 (pressurized to 1.0±0.1MPa) through a pipeline with a regulating valve 5-1;
[0053] At the same time, the circulating oxygen dehydrated by the inorganic vaporization permeable membrane dehydration unit 18 also enters the oxygen booster pump 5 after passing through the pipeline with the regulating valve 5-2;
[0054] That is, under the action of the oxygen booster pump 5, the two mixed oxygen streams are sent into the gas-liquid mixer 10 after passing through the oxygen flow meter 8;
[0055] Note: The purpose of reducing the pressure of oxygen through the oxygen pressure reducing valve 4 is to ensure that it can subsequently enter the oxygen booster pump 5.
[0056] The regulating valve 1-1 is used to regulate the flow of liquid oxygen flowing out of the liquid oxygen storage tank 1; the regulating valve 5-1 is used to regulate the flow of oxygen after decompression. The regulating valve 5-2 is used to regulate the flow of circulating oxygen; in the utility model, firstly, it is ensured that all the circulating oxygen is utilized, and fresh oxygen is supplemented through the valve 5-1 if it is insufficient.
[0057] 2. The raw material (containing methyl and fluorine-substituted aromatic hydrocarbons) added with a quantitative catalyst in the raw material storage tank 6 enters the feed pump 7 through the pipeline with the regulating valve 6-1;
[0058] At the same time, the liquid phase obtained from the gas-liquid separator 16 of the reacted material enters the feed pump 7 through the liquid phase outlet of the gas-liquid separator 16 of the reacted material and the pipeline with the valve 16-3;
[0059] That is, under the action of the feed pump 7, the raw material and the liquid phase obtained from the gas-liquid separator 16 after the reaction are mixed and then sent to the gas-liquid mixer 10 after passing through the raw material flow meter 9;
[0060] The function of the regulating valve 16-1 is to control the flow rate discharged from the gas-liquid separator 16 of the material after reaction to prevent the liquid material in the gas-liquid separator 16 from being emptied and causing gas to be discharged from the bottom. The function of the valve 16-3 is to control the flow rate of the liquid phase (liquid material) of the gas-liquid separator 16 of the material after reaction entering the feeding pump 7.
[0061] When the content of the product in the liquid phase obtained from the gas-liquid separator 16 after the reaction is ≥ 60%, it is determined that the reaction meets the requirements;
[0062] Only when the reaction meets the requirements, the liquid phase (liquid material) of the gas-liquid separator 16 of the material after the reaction is transferred out of the system through the discharge port with valve 16-2 as the material after the reaction. Before this, the liquid phase (liquid material) of the gas-liquid separator 16 of the material after the reaction all enters the feed pump 7. The raw material provided by the raw material storage tank 6 is adjusted by the regulating valve 6-1, so as to control the amount of the mixed raw material entering the gas-liquid mixer 10.
[0063] 3. The raw materials and oxygen mixed in the gas-liquid mixer 10 are sequentially passed through the preheater 11 (heated to 80±5°C), the pipeline with the thermometer 12 and the pressure gauge 13, and finally enter the reaction pipeline of the microchannel plate reactor 14 for reaction (the reaction temperature is 100±5°C, the pressure is 1.0±0.1Mpa, which is adjusted by the back pressure valve 14-3);
[0064] The reacted material obtained in the reaction pipeline of the microchannel plate reactor 14 enters the material pipeline in the temperature and pressure regulator 15 through the pipeline with the back pressure regulating valve 14-3 to adjust the temperature and pressure (control the temperature to 80±5°C and the pressure to 0.25±0.05MPa), and then enters the reacted material gas-liquid separator 16 through the pipeline. The liquid phase obtained by the reacted material gas-liquid separator 16 mainly comprises the reaction product and the unreacted raw material, the catalyst and a small amount of water, and the gas phase obtained by the reacted material gas-liquid separator 16 mainly comprises oxygen, water vapor and part of the raw material vapor;
[0065] 4. After the reaction, the gas phase separated by the gas-liquid separator 16 is sent to the material pipeline in the gas phase superheater 17 through a pipeline for heating (heated to 100±5°C to ensure that the water and raw materials in the gas phase material are not condensed into liquid). Under the suction of the vacuum pump 21, the heated gas phase is sent to the inorganic vaporization permeable membrane dehydration unit 18 for dehydration. The water vapor and non-condensable gas on the permeation side of the inorganic vaporization permeable membrane dehydration unit 18 enter the material pipeline in the condenser 19 for condensation, and then enter the permeate gas-liquid separator 20 for separation. The permeate generated by the permeate gas-liquid separator 20 is in the lower layer, and the permeate is discharged into the permeate storage tank through a pipeline with a valve 20-1.
[0066] The upper gas phase (including oxygen, water vapor and vapor containing methyl and fluorine-substituted aromatic hydrocarbons) separated by the permeate gas-liquid separator 20 is discharged into the tail gas main pipe after passing through the vacuum pump 21, and is treated to meet the emission standards;
[0067] The interception side of the inorganic vaporization permeable membrane dehydration unit 18 is the dehydrated circulating oxygen (mainly oxygen and part of the raw materials), which enters the oxygen booster pump 5 through the pipeline with the regulating valve 5-2, thereby realizing the recycling of oxygen;
[0068] After the reaction, the liquid phase separated by the gas-liquid separator 16 enters the feed pump 7.
[0069] Finally, it should be noted that the above examples are only some specific embodiments of the present invention. Obviously, the present invention is not limited to the above examples, and there are many variations. All variations that can be directly derived or associated with the content disclosed by a person skilled in the art should be considered as the protection scope of the present invention.
Claims
1. A reaction device for preparing acid by continuous catalytic oxidation of methyl- and fluorine-substituted aromatic hydrocarbons, characterized in that: It comprises a liquid oxygen storage tank (1), a liquid oxygen vaporizer (2), an oxygen buffer tank (3), an oxygen pressure reducing valve (4), an oxygen booster pump (5), a raw material storage tank (6), a feed pump (7), an oxygen flow meter (8), a raw material flow meter (9), a gas-liquid mixer (10), a raw material preheater (11), a microchannel plate reactor (14), a temperature and pressure regulator (15), a post-reaction material gas-liquid separator (16), a gas phase superheater (17), an inorganic vaporization permeation membrane dehydration unit (18), a condenser (19), a permeate gas-liquid separator (20) and a vacuum pump (21); The liquid oxygen storage tank (1), the pipeline with a regulating valve, the liquid oxygen vaporizer (2), the pipeline with a valve, the oxygen buffer tank (3), the oxygen pressure reducing valve (4), the pipeline with a regulating valve and the inlet of the oxygen booster pump (5) are connected in sequence; the outlet of the oxygen booster pump (5) is connected to the inlet of the gas-liquid mixer (10) after passing through the oxygen flow meter (8); The raw material storage tank (6) is connected to the inlet of the feed pump (7) through a pipeline with a regulating valve; the outlet of the feed pump (7) is connected to the inlet of the gas-liquid mixer (10) after passing through the raw material flow meter (9); The outlet of the gas-liquid mixer (10), the raw material preheater (11), and the inlet of the microchannel plate reactor (14) are connected in sequence; a back pressure regulating valve (14-3) is provided at the outlet of the microchannel plate reactor (14), and then connected to the inlet of the post-reaction material gas-liquid separator (16) through a temperature and pressure regulator (15); A valve is provided at the liquid phase outlet of the gas-liquid separator (16) of the reacted material, and then the liquid phase is divided into two paths, one of which is a discharge port with a valve, and the other is connected to the inlet of the feed pump (7) through a pipeline with a valve; The gas phase outlet of the gas-liquid separator (16) of the reacted material, the gas phase superheater (17), the pipeline with a valve, and the inlet of the inorganic vaporization permeation membrane dehydration unit (18) are connected in sequence; The water vapor outlet of the inorganic vaporization permeable membrane dehydration unit (18), the condenser (19), and the inlet of the permeate liquid gas-liquid separator (20) are connected in sequence, and the gas outlet of the permeate liquid gas-liquid separator (20) is connected to the vacuum pump (21); The gas outlet of the inorganic vaporization permeation membrane dehydration unit (18) is connected to the inlet of the oxygen booster pump (5) through a pipeline with a regulating valve.
2. The reaction device for preparing acid by continuous catalytic oxidation of methyl- and fluorine-substituted aromatic hydrocarbons according to claim 1, characterized in that: A thermometer (12) and a pressure gauge (13) are respectively provided on the pipeline connecting the raw material preheater (11) and the microchannel plate reactor (14).
3. The reaction device for preparing acid by continuous catalytic oxidation of methyl- and fluorine-substituted aromatic hydrocarbons according to claim 2, characterized in that: The liquid outlet of the permeate gas-liquid separator (20) is connected to the permeate storage tank via a pipeline with a valve.
4. The reaction device for preparing acid by continuous catalytic oxidation of methyl- and fluorine-substituted aromatic hydrocarbons according to claim 3, characterized in that: A heat medium pipeline and a reaction pipeline are respectively arranged in the microchannel plate reactor (14). The heat medium enters the heat medium pipeline in the microchannel plate reactor (14) from the heat medium inlet (14-1) and is then discharged from the heat medium outlet (14-2). A medium pipeline and a material pipeline are respectively provided in the temperature and pressure regulator (15); the medium enters the medium pipeline of the temperature and pressure regulator (15) from the medium inlet (15-1) and is then discharged from the medium outlet (15-2); A steam pipeline and a material pipeline are respectively arranged in the gas phase superheater (17); steam enters the steam pipeline from the steam inlet (17-1) and is discharged from the steam outlet (17-2); A refrigerant pipeline and a material pipeline are respectively arranged in the condenser (19); the refrigerant enters the refrigerant pipeline from the refrigerant inlet (19-1) and is then discharged from the refrigerant outlet (19-2).
5. The reaction device for preparing acid by continuous catalytic oxidation of methyl- and fluorine-substituted aromatic hydrocarbons according to claim 4, characterized in that: A raw material preheater (11), a pipeline with a thermometer (12) and a pressure gauge (13), and an inlet of a reaction pipeline in a microchannel plate reactor (14) are connected in sequence; a back pressure regulating valve (14-3) is provided at the outlet of the reaction pipeline in the microchannel plate reactor (14); the outlet of the reaction pipeline in the microchannel plate reactor (14) is connected in sequence to an inlet of a post-reaction material gas-liquid separator (16) through the back pressure regulating valve (14-3) and then through a material pipeline in a temperature and pressure regulator (15); The gas phase outlet of the gas-liquid separator (16) of the reacted material is connected to the material pipeline in the gas phase superheater (17).
Citation Information
Patent Citations
Preparation method of p-fluorobenzaldehyde
CN106565445A
Method for preparing p-fluorobenzaldehyde through continuous oxidation of fluorotoluene
CN106748686A