4-chloro-2-trifluoroacetyl aniline hydrochloride microchannel reactor and synthesis method

Abstract

The application discloses a 4-chloro-2-trifluoroacetyl aniline hydrochloride microchannel reactor and a synthesis method, relates to the field of reactors, and comprises a reactor body, the reactor body comprises a reactor one and a reactor two, the reactor one is provided with a reaction tube one, the reactor two is provided with a reaction tube two, the reaction tube one is communicated with the reaction tube two, and the reactor body is provided with a limiting piece which limits separation of the reactor one and the reactor two. Through the above technical scheme, the reaction tube one and the reaction tube two are arranged, the microchannel is formed through the connection of the reaction tube one and the reaction tube two, in actual use, the length of the microchannel is increased through the connection of the two, so that the reactants can fully react, when cleaning is needed, the microchannel is split into the reaction tube one and the reaction tube two, and the reaction tube one and the reaction tube two are cleaned respectively, the cleaning and maintenance of components are facilitated, and the convenience of product use is improved.

Description

Technical Field

[0001] This application relates to the field of reactors, and more specifically, to a microchannel reactor for 4-chloro-2-trifluoroacetylaniline hydrochloride and a method for its synthesis. Background Technology

[0002] Microchemical technology, due to its superior heat and mass transfer capabilities, will find wide application in fields such as chemistry, chemical engineering, energy, and the environment. Its core component is a microreactor manufactured entirely or partially using microfabrication technology.

[0003] For example, Chinese invention patent CN110961060A discloses a microchannel reactor, comprising: a shell having an inlet, an outlet, a cooling fluid inlet, and a cooling fluid outlet; a microchannel reaction unit located inside the shell; the microchannel reaction unit including a microchannel reactor wall; the microchannel reactor wall comprising: a stainless steel substrate layer having a first side surface forming a reaction channel; a roughened layer processed on the first side surface; and a catalyst support layer formed on the roughened layer; the inlet and outlet being connected through the reaction channel; and a cooling channel arranged along the microchannel reaction unit inside the shell, with the cooling fluid inlet and outlet being connected through the cooling channel. In this way, the catalyst support layer adheres to the stainless steel substrate layer through the roughened layer. The roughened surface of the roughened layer effectively increases the adhesion area of ​​the catalyst support layer and simultaneously improves the adhesion between the catalyst support layer and the stainless steel substrate layer, which is beneficial for the smooth progress of the reaction.

[0004] In practical use, due to the long length and limited width of the microchannels, cleaning the inside of the microchannel reactor is inconvenient and needs to be improved. Summary of the Invention

[0005] To address the problem of inconvenient cleaning inside microchannel reactors, this application provides a microchannel reactor for 4-chloro-2-trifluoroacetylaniline hydrochloride and a synthesis method thereof.

[0006] This application provides a microchannel reactor and synthesis method for 4-chloro-2-trifluoroacetylaniline hydrochloride, employing the following technical solution:

[0007] A microchannel reactor includes a reactor body, which includes a reactor one and a reactor two. The reactor one is provided with a reaction tube one, and the reactor two is provided with a reaction tube two. The reaction tube one is connected to the reaction tube two. The reactor body is provided with a limiting member that restricts the separation of the reactor one and the reactor two.

[0008] The above technical solution sets up reaction tube one and reaction tube two, and forms a microchannel by connecting reaction tube one and reaction tube two. In actual use, the connection between the two increases the length of the microchannel, allowing the reactants to react fully. When cleaning is required, the microchannel is split into reaction tube one and reaction tube two, and reaction tube one and reaction tube two are cleaned separately, which facilitates the cleaning and maintenance of the components and improves the ease of use of the product.

[0009] Furthermore, the reactor body is provided with a sealing sleeve, which is fitted onto the outer walls of reaction tube one and reaction tube two. The outer wall of the sealing sleeve is provided with an installation hole and an installation pin. The installation hole penetrates the sealing sleeve to the inner wall of the sealing sleeve. Reaction tube one is provided with an installation groove, and the installation pin passes through the installation hole and is embedded in the installation groove.

[0010] Through the above technical solution, in actual use, due to the low reaction temperature of some reactions, there is a change in gas pressure inside reaction tube one and reaction tube two. Therefore, leakage of reaction solution is likely to occur at the connection between reaction tube one and reaction tube two. Such situations can reduce reaction efficiency and cause material waste. Therefore, a sealing sleeve is set to improve the sealing degree at the connection between reaction tube one and reaction tube two, reduce the occurrence of liquid leakage, and make the overall use more stable.

[0011] Furthermore, the sealing tube sleeve is provided with an installation groove located on the inner wall of the sealing tube sleeve. A return spring is provided at the bottom of the installation groove, and an adjusting block is connected to the return spring. The elastic force of the return spring limits the movement of the adjusting block towards the bottom of the installation groove. The first reaction tube is provided with a clearance hole that penetrates the first reaction tube. The adjusting block passes through the clearance hole, and the end of the adjusting block away from the bottom of the installation groove is flush with the inner wall of the first reaction tube.

[0012] Through the above technical solution, in practical use, because the reactants have temperature requirements for the reaction and the reaction is accompanied by changes in gas pressure, the gas pressure in reaction tube 1 and reaction tube 2 will change to a certain extent during the reaction process. The changes in gas pressure can easily cause liquid leakage and damage at the connection between reaction tube 1 and reaction tube 2. Therefore, an adjusting block and a reset spring are set up. When the gas pressure in reaction tube 1 and reaction tube 2 changes, the adjusting block 1 is pushed to move to help balance the gas pressure in reaction tube 1 and reaction tube 2, reducing the possibility of damage at the connection between reaction tube 1 and reaction tube 2 caused by changes in gas pressure, and making the overall use more stable.

[0013] Furthermore, the reaction tube is provided with a balance channel and a reaction channel, the reaction channel passing through the reaction tube, and the balance channel connecting the reaction channel and the clearance hole; the adjusting block is provided with a connecting channel, the connecting channel being used to connect the balance channel and the mounting groove.

[0014] By using the above technical solution, a balance channel and a reaction channel are set up. In actual use, when the gas pressure in the reaction channel increases or there is a lot of reaction solution, the connecting channel connects the balance channel and the installation tank. At this time, the gas pressure inside the reaction channel decreases or some of the reaction solution enters the installation tank. In this way, the possibility of tube rupture caused by excessive gas pressure in reaction tube 1 and reaction tube 2 is reduced, making the overall use more stable.

[0015] Furthermore, the reaction tube one is also provided with a balance channel two, one end of which is connected to the balance channel one, and the other end is used to connect to the connecting channel.

[0016] Through the above technical solution, in actual use, excessive or insufficient air pressure in reaction tube 1 and reaction tube 2 can easily damage them. Therefore, a second balancing channel is set up. When the air pressure in reaction tube 1 and reaction tube 2 is too high, the second balancing channel connects to the first balancing channel to balance the air pressure. When the air pressure in reaction tube 1 and reaction tube 2 decreases, the adjusting block moves to connect the first balancing channel to balance the air pressure. In this way, the whole system can provide a certain degree of protection against different air pressures.

[0017] Furthermore, the mounting groove is provided with a return spring, and the return spring is connected to a return block. The elastic force of the return spring restricts the return block from moving towards the bottom of the mounting groove; the reaction tube is provided with a return hole, and the return block passes through the return hole.

[0018] With the above technical solution, in actual use, when the connecting channel connects the first balance channel and the installation tank, the liquid easily enters the installation tank. Therefore, a return spring and a reflux block are set. When the gas pressure in the reaction channel returns to normal, the movement of the regulating block keeps the gas pressure in the installation tank at the state it was when the connecting channel first connects the balance channel and the installation tank. As the reaction channel reacts, the reflux block moves, making it easier for the reaction solution in the installation tank to re-enter the reaction channel, reducing the loss of the reaction solution.

[0019] Furthermore, the reflux block is provided with a reflux channel, one end of which is connected to the reaction channel and the other end is used to connect to the mounting slot.

[0020] The above technical solution, by setting up a reflux channel, facilitates the re-entry of the reaction solution into the reaction channel after entering the installation tank, reducing solution loss and improving reaction efficiency.

[0021] A method for synthesizing 4-chloro-2-trifluoroacetylaniline hydrochloride includes the following steps: adding n-butyllithium solution dropwise to a 4-chloro-N-pivaloylaniline solution at a temperature of -40°C to -10°C to obtain a bislithium salt solution of 4-chloro-N-pivaloylaniline; then, introducing trifluoroacetyl chloride gas into the solution at a temperature of -40°C to -10°C to obtain 4-chloro-2-trifluoroacetyl-N-pivaloylaniline; the time for introducing trifluoroacetyl chloride gas is 20 min to 120 min; the reaction time after introducing trifluoroacetyl chloride gas is 0.8 h to 1.5 h; finally, hydrolyzing 4-chloro-2-trifluoroacetyl-N-pivaloylaniline under acidic conditions to obtain the product 4-chloro-2-trifluoroacetylaniline hydrate hydrochloride.

[0022] With the above technical solution, the reaction time after introducing trifluoroacetyl chloride gas is 0.8 hours to 1.5 hours. By limiting the reaction time, the situation where some raw materials are not fully reacted and the yield is reduced due to too short a reaction time is avoided. It also reduces the situation where by-products are generated due to too long a reaction time, which in turn reduces the yield, reduces efficiency, and increases production costs. In this way, production efficiency is improved.

[0023] In summary, this application includes at least one of the following beneficial technical effects:

[0024] (1) By limiting the reaction time, the situation where some raw materials are not fully reacted and the yield is reduced due to the reaction time being too short; it also reduces the situation where byproducts are generated due to the reaction time being too long, thereby reducing the yield, efficiency and increasing production costs; thus, production efficiency is improved.

[0025] (2) By setting up reaction tube one and reaction tube two, the microchannel is divided into reaction tube one and reaction tube two, and reaction tube one and reaction tube two are cleaned respectively, which facilitates the cleaning and maintenance of components and improves the ease of use of the product.

[0026] (3) By setting an adjustment block and a reset spring, when the gas pressure of reaction tube 1 and reaction tube 2 changes, the adjustment block 1 is pushed to move to help balance the gas pressure in reaction tube 1 and reaction tube 2, reducing the possibility of damage at the connection between reaction tube 1 and reaction tube 2 caused by changes in gas pressure in reaction tube 1 and reaction tube 2, making the overall use more stable. Attached Figure Description

[0027] Figure 1 This is an overall schematic diagram of an embodiment.

[0028] Figure 2 This is a cross-sectional schematic diagram of an embodiment.

[0029] Figure 3 for Figure 2An enlarged diagram of A in the diagram.

[0030] Figure 4 This is a cross-sectional schematic diagram from another perspective of the embodiment.

[0031] Figure 5 for Figure 4 Enlarged diagram of B in the diagram.

[0032] Reference numerals in the attached drawings: 1. Reactor body; 2. Reactor 1; 3. Reactor 2; 4. Limiting component; 5. Limiting protrusion ring; 6. Limiting bolt; 7. Reaction tube 1; 8. Reaction tube 2; 9. Relief groove; 10. Sealing sleeve; 11. Mounting hole; 12. Mounting pin; 13. Mounting groove; 14. Reaction channel; 15. Mounting groove; 16. Return spring; 17. Adjusting block; 18. Relief hole; 19. Connecting channel; 20. Balance channel 1; 21. Balance channel 2; 22. Return spring; 23. Reflux block; 24. Reflux hole; 25. Reflux channel. Detailed Implementation

[0033] The present application will be further described in detail below with reference to the accompanying drawings.

[0034] This application discloses a microchannel reactor and synthesis method for 4-chloro-2-trifluoroacetylaniline hydrochloride.

[0035] Example:

[0036] See Figure 1 and Figure 2 A microchannel reactor for the synthesis of 4-chloro-2-trifluoroacetylaniline hydrochloride is disclosed. The reactor body 1 includes a reactor main body 1, which comprises a first reactor 2 and a second reactor 3. The reactor main body 1 is equipped with a limiting element 4 to restrict the separation of the first reactor 2 and the second reactor 3. In practical use, the limiting element 4 can be a limiting protrusion 5 and a limiting bolt 6. Two limiting protrusions 5 are provided, one located on the outer wall of the first reactor 2 and the other on the outer wall of the second reactor 3. The limiting bolt 6 passes through both limiting protrusions 5 to fix the first reactor 2 and the second reactor 3. Alternatively, the limiting element 4 can also be a limiting protrusion 5 and a positioning pin, with the positioning pin fixing the limiting protrusion 5 to restrict the separation of the first reactor 2 and the second reactor 3.

[0037] See Figure 2 and Figure 3Reactor 1 (2) is equipped with reaction tube 1 (7), and reactor 2 (3) is equipped with reaction tube 2 (8). Reaction tube 1 (7) is used to connect reaction tube 2 (8). Reactor 1 (2) is also equipped with a relief groove (9) located at one end of reactor 1 (2) near reactor 2 (3). Reactor body 1 is equipped with a sealing sleeve (10), which is fitted onto the outer walls of reaction tube 1 (7) and reaction tube 2 (8). When the sealing sleeve (10) is fitted onto the outer walls of reaction tube 1 (7) and reaction tube 2 (8), the sealing sleeve (10) is embedded in the relief groove (9).

[0038] The outer wall of the sealing sleeve 10 is provided with a mounting hole 11 and a mounting pin 12. The mounting hole 11 penetrates the sealing sleeve 10 to the inner wall of the sealing sleeve 10. The reaction tube 7 is provided with a mounting groove 13. The mounting pin 12 passes through the mounting hole 11 and is embedded in the mounting groove 13. In other embodiments, the sealing sleeve 10 may also be provided with mounting bolts. The sealing sleeve 10 is fixed by the mounting bolts passing through the mounting hole 11 and being embedded in the mounting groove 13.

[0039] Reaction tube 7 is provided with a reaction channel 14, which runs through reaction tube 7 and connects to reaction tube 8. Sealing sleeve 10 is provided with a mounting groove 15 located on the inner wall of sealing sleeve 10. A return spring 16 is located at the bottom of the mounting groove 15, and an adjusting block 17 is connected to the return spring 16. The adjusting block 17 is located at the end of the return spring 16 furthest from the bottom of the mounting groove 15, and the spring force of the return spring 16 limits the movement of the adjusting block 17 towards the bottom of the mounting groove 15. Reaction tube 7 is provided with a clearance hole 18, which passes through reaction tube 7 to reaction channel 14, and the adjusting block 17 passes through the clearance hole 18. When the return spring 16 is in its normal state, the end of the adjusting block 17 furthest from the bottom of the mounting groove 15 is flush with the inner wall of reaction tube 7.

[0040] The adjusting block 17 is provided with a connecting channel 19, one end of which connects to the relief groove 9, and the other end is located on the side wall of the adjusting block 17. The reaction tube 7 is provided with a first balancing channel 20 and a second balancing channel 21. One end of the first balancing channel 20 connects to the reaction channel 14, and the other end is located on the wall of the relief hole 18 for connecting to the connecting channel 19. One end of the second balancing channel 21 connects to the first balancing channel 20, and the other end connects to the connecting channel 19. In actual use, when the air pressure in the reaction channel 14 changes, the change in air pressure causes the adjusting block 17 to move closer to or further away from the bottom of the mounting groove 15. When the air pressure in the reaction channel 14 increases, the adjusting block 17 moves closer to the bottom of the mounting groove 15, at which time the second balancing channel 21 connects to the connecting channel 19. When the air pressure in the reaction channel 14 decreases, the adjusting block 17 moves further away from the bottom of the mounting groove 15, at which time the first balancing channel 20 connects to the connecting channel 19.

[0041] See Figure 4 and Figure 5In practical use, reaction tube 7 and reaction tube 8 are placed horizontally, with their lengths aligned horizontally. The mounting groove 15 is located above the axis of reaction tube 7. The mounting groove 15 is equipped with a return spring 22, positioned near the axis of reaction tube 7. A return block 23 is connected to the end of the return spring 22 furthest from the bottom of the groove. The spring force restricts the return block 23 from moving closer to the bottom of the groove. Reaction tube 7 has a return hole 24, which extends from reaction tube 7 to the reaction channel 14. The return block 23 passes through the return hole 24. When the return spring 22 is in its normal position, the end of the return block 23 furthest from the bottom of the mounting groove 15 does not protrude from the surface of the reaction channel 14. The return block 23 has a return channel 25, one end of which connects to the reaction channel 14, and the other end connects to the mounting groove 15.

[0042] A method for synthesizing 4-chloro-2-trifluoroacetylaniline hydrochloride involves adding a solution of n-butyllithium dropwise to a solution of 4-chloro-N-pivaloylaniline at a temperature of -40°C to -10°C to obtain a bislithium salt solution of 4-chloro-N-pivaloylaniline. Then, trifluoroacetyl chloride gas is introduced into the solution at a temperature of -40°C to -10°C to obtain 4-chloro-2-trifluoroacetyl-N-pivaloylaniline. The time for introducing trifluoroacetyl chloride gas is 20 min to 120 min, and the reaction time after introducing trifluoroacetyl chloride gas is 0.8 h to 1.5 h. Finally, 4-chloro-2-trifluoroacetyl-N-pivaloylaniline is hydrolyzed under acidic conditions to obtain the product 4-chloro-2-trifluoroacetylaniline hydrate hydrochloride.

[0043] The working principle of this embodiment is as follows:

[0044] In practical use, when the gas pressure in reaction channel 14 increases, the regulating block 17 moves towards the bottom of the mounting tank 15, and the second balancing channel 21 connects to the connecting channel 19. When the gas pressure in reaction channel 14 decreases, the regulating block 17 moves away from the bottom of the mounting tank 15, and the first balancing channel 20 connects to the connecting channel 19. When the gas pressure in reaction channel 14 is lower than the gas pressure at the mounting tank 15, and there is accumulated reaction solvent in the mounting tank 15, the reflux block 23 moves, causing the reflux channel 25 to connect the mounting tank 15 and the reaction channel 14.

[0045] The above are all preferred embodiments of this application, and are not intended to limit the scope of protection of this application. Therefore, all equivalent changes made in accordance with the structure, shape and principle of this application should be covered within the scope of protection of this application.

Claims

1. A 4-chloro-2-trifluoroacetylaniline hydrochloride microchannel reactor characterized by: The utility model provides a double reactor, including reactor body (1), reactor body (1) includes reactor one (2) with reactor two (3), the reactor one (2) is equipped with reaction tube one (7), the reactor two (3) is equipped with reaction tube two (8), reaction tube one (7) communicates reaction tube two (8), reactor body (1) is equipped with stop piece (4), and stop piece (4) limits reactor one (2) and reactor two (3) separation; Reaction tube one (7) and reaction tube two (8) outer wall are sleeved with sealing sleeve (10), and the installation groove (15) is arranged on the inner wall of sealing sleeve (10) in the position of reaction tube one (7) and reaction tube two (8), the reset spring (16) is arranged on the groove bottom of installation groove (15), the adjusting block (17) is connected to the reset spring (16), and the elastic force of reset spring (16) limits the adjusting block (17) to move towards the direction close to the groove bottom of installation groove (15); Reaction tube one (7) and reaction tube two (8) side wall are respectively equipped with let -alone hole (18), let -alone hole (18) penetrates reaction tube one (7) and reaction tube two (8), adjusting block (17) passes through let -alone hole (18), and the end of adjusting block (17) away from the groove bottom of installation groove (15) is flush with the inner wall of reaction tube one (7) and reaction tube two (8) respectively; Reaction tube one (7) and reaction tube two (8) are respectively equipped with balance channel one (20) and reaction channel (14), and the reaction channel (14) is axially through reaction tube one (7) and reaction tube two (8);Balance channel one (20) is connected with reaction channel (14) and let -alone hole (18);Adjusting block (17) is equipped with communication channel (19), and the communication channel (19) is used for connecting balance channel one (20) and installation groove (15);Reaction tube one (7) and reaction tube two (8) are respectively equipped with balance channel two (21), and one end of balance channel two (21) is connected with balance channel one (20), and the other end is used for connecting communication channel (19); The installation groove (15) is further provided with a return spring (22), the return spring (22) is connected with a backflow block (23), and the elastic force of the return spring (22) limits the movement of the backflow block (23) towards the groove bottom of the installation groove (15).

2. The 4-chloro-2-trifluoroacetylaniline hydrochloride microchannel reactor of claim 1, wherein: The outer wall of the sealing sleeve (10) is provided with mounting holes (11) and mounting pins (12) at the positions of the reaction tube one (7) and the reaction tube two (8) respectively, the mounting holes (11) penetrate the sealing sleeve (10) to the inner wall of the sealing sleeve (10), the reaction tube one (7) and the reaction tube two (8) are respectively provided with mounting grooves (13), the mounting pins (12) pass through the mounting holes (11) and are embedded in the mounting grooves (13).

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