Micro reactor for high-viscosity reaction system

Abstract

The utility model relates to the technical field of chemical equipment, and discloses a microreactor for a high-viscosity reaction system, which comprises a feeding end cover (2), a discharging end cover (9), a primary reactor (4), a secondary reactor (8), an interstage connector I (6), an interstage connector II (18) and a crossover line (7), the feeding end cover (2) is arranged at the inlet end of the first-stage reactor (4), the first-stage reactor (4) and the second-stage reactor (8) are connected through the overline (7), the first-stage reactor (4) and the overline (7) are connected through the interstage connector I (6), and the second-stage reactor (8) and the overline (7) are connected through the interstage connector II (18); concave sealing pieces (3) are arranged on the inner walls of the interstage connector I (6) and the interstage connector II (18), and the concave corners are chamfered; and a discharge end cover (9) is arranged at the outlet end of the secondary reactor (8). The reactor weight is reduced, and the application is flexible and convenient.

Description

Technical Field

[0001] This utility model relates to the field of chemical equipment technology, specifically a microreactor for high-viscosity reaction systems. Background Technology

[0002] Microreactors are miniaturized devices for developing continuous flow processes, suitable for pilot development, process optimization, and process validation. Common types include fixed-bed high-pressure hydrogenation microreactors, cracking microreactors, and continuous flow synthesis units. However, most of these involve low-viscosity systems, offering higher reaction efficiency and flexible operating environments. High-viscosity reaction systems, on the other hand, suffer from high fluid resistance, poor heat transfer, and high design pressures. Commonly used plug flow reactors often employ flange connections, resulting in large reactor weight and volume, making them unsuitable for microreactor applications.

[0003] In recent years, with the development of polymer materials, the development of gradually polymerized polymers and free radical polymers has been rapid. However, the main equipment used for small-scale research is batch reactor, which is far from industrial-scale equipment. This can easily lead to inaccurate parameters during the later industrial scale-up process, resulting in huge economic losses.

[0004] CN115106024A discloses a mixed-flow reactor with multiple sets of reaction tubes, each having a straight section and a bend, with adjacent sets of reaction tubes interconnected. The continuous S-bends in the reaction tubes increase the residence time of the reacted material. However, it cannot be connected in parallel, making its application inflexible.

[0005] Therefore, a new technical solution is needed to solve the above-mentioned technical problems. Utility Model Content

[0006] The technical problem to be solved by this invention is to provide a microreactor for high-viscosity reaction systems that reduces reactor weight and is easy to use.

[0007] To address the above technical problems, this utility model provides a microreactor for high-viscosity reaction systems, comprising an inlet end cap, an outlet end cap, a primary reactor, a secondary reactor, an interstage connector I, an interstage connector II, and a crossover line; the inlet end cap is located at the inlet end of the primary reactor, the primary reactor and the secondary reactor are connected by the crossover line, the primary reactor and the crossover line are connected by the interstage connector I, and the secondary reactor and the crossover line are connected by the interstage connector II; the inner walls of the interstage connector I and the interstage connector II are provided with concave sealing elements, and the concave corners are chamfered; the outlet end cap of the secondary reactor is provided at the outlet end.

[0008] By adopting the above technical solution, the primary reactor and the secondary reactor are connected in series through interstage connector I and interstage connector II, which replaces the traditional flange connection, reduces the weight of the reactor, makes installation convenient, occupies little space, and facilitates quick disassembly during the experiment.

[0009] Preferably, the seal of the interstage connector II is provided with a partition plate, which divides the concave seal into two cavities, an inlet cavity and an outlet cavity; the inlet cavity is connected to the heating coil inlet, and the outlet cavity is connected to the heating coil outlet; a heating inlet pipe is provided on the end cap of the inlet cavity, and a heating outlet pipe is provided on the end cap of the outlet cavity.

[0010] By adopting the above technical solution, the heating coil is connected through interstage connector II to exchange heat with the fluid in the secondary reactor, which simplifies the heating structure and enhances internal heat exchange.

[0011] Preferably, heating elements are installed on the outer walls of the primary reactor, secondary reactor, crossover line, interstage connector I, and interstage connector II, and an electric heating layer is installed on the inner walls of each. A spiral shearing element is installed in the primary reactor via a support frame. A heating coil is installed in the secondary reactor.

[0012] By adopting the above technical solution, through the heating elements on the outer walls of the primary reactor, secondary reactor, cross-line, interstage connector I and interstage connector II, and the electric heating layer on the inner wall, heat transfer oil or electric heating combination heating can be carried out to ensure that there are no cooling dead zones in the reaction equipment and to ensure the accuracy of experimental data.

[0013] Preferably, multiple primary reactors are connected in series, and the primary reactors are connected to each other via interstage connector I. Multiple secondary reactors are connected in series, and the secondary reactors are connected to each other via interstage connector II.

[0014] By adopting the above technical solution, the primary reactor and the secondary reactor can be connected in series through interstage connector I and interstage connector II and then connected by a cross-line according to process requirements. The installation is simple, occupies little space, and is easy to disassemble during the experiment. It can be heated by a combination of heat transfer oil or electric heating to ensure that there are no dead corners in the cooling of the reaction equipment and to ensure the accuracy of experimental data.

[0015] Preferably, the feed end cover is set at the feed end of the primary reactor, the two primary reactors are connected in parallel by an insulated tee, the two secondary reactors are also connected in parallel by an insulated tee, and the two insulated tees are connected by a cross-line connection; the outlet end of the secondary reactor is set with a discharge end cover.

[0016] By adopting the above technical solution, the primary reactor and the secondary reactor can be connected in parallel through an insulated tee and then connected by a cross-line according to the process requirements. The installation is simple, occupies little space, and is easy to disassemble during the experiment. It can be heated by a combination of heat transfer oil or electric heating to ensure that there are no dead corners in the cooling of the reaction equipment and to ensure the accuracy of the experimental data.

[0017] Preferably, the material channel I of the feed end cap is 1 / 4 to 1 / 2 of the inner diameter of the primary reactor.

[0018] By adopting the above technical solution, the residence time of materials in the feed pipe is reduced, allowing them to enter the reactor quickly and achieve better mixing in the reactor.

[0019] Preferably, the material channel II of the discharge end cap has a size of 1 / 3 to 3 / 4 of the inner diameter of the primary reactor.

[0020] By adopting the above technical solution, after the reaction is completed, the material viscosity is high, and expanding the outlet pipeline will help to discharge the material smoothly.

[0021] Preferably, both the primary and secondary reactors are plug flow reactors with an inner diameter of 6-40 mm and a length of 300-600 mm.

[0022] By adopting the above technical solution and using a small reverse feed rate, the mixing effect is improved, the heat transfer effect is more uniform during the reaction process, and the number of reaction pipes can be flexibly increased or decreased to adapt to different residence times.

[0023] Compared with the prior art, this utility model has the following advantages:

[0024] 1. The primary reactor and secondary reactor of this utility model are connected by interstage connector I and interstage connector II, replacing the original flange connection, which occupies less space and reduces the weight of the reactor.

[0025] 2. The primary and secondary reactors of this utility model can be connected in series or in parallel through insulated tees, cross-line connections and two interstage connectors, which can be flexibly connected according to process requirements, and are suitable for different reaction types and different reaction stages, making them easy to apply.

[0026] 3. This utility model uses heating elements on the outer walls of the primary reactor, secondary reactor, cross-line, interstage connector I and interstage connector II, and an electric heating layer on the inner wall to heat the materials with a combination of heat transfer oil or electric heating, ensuring that there are no dead zones in the cooling of the reaction equipment and ensuring experimental safety. Attached Figure Description

[0027] Figure 1 This is a schematic diagram of the structure of this utility model.

[0028] Figure 2 This is a schematic diagram of the feed end cap structure of this utility model.

[0029] Figure 3 This is a schematic diagram of the discharge end cap structure of this utility model.

[0030] Figure 4This is a schematic diagram of the structure of the primary reactor of this utility model.

[0031] Figure 5 This is an exploded view of the secondary reactor of this utility model.

[0032] Figure 6 This is a schematic diagram of the cross-line structure of this utility model.

[0033] Figure 7 This is a schematic diagram of the interstage connector I of this utility model.

[0034] Figure 8 This is a schematic diagram of the interstage connector II structure of this utility model.

[0035] Figure 9 This is a schematic diagram of the connection between the first and second stage reactors in Embodiment 1 of this utility model.

[0036] In the diagram, 1. Feed pipe, 2. Feed end cap, 3. Seal, 4. Primary reactor, 5. Heating element, 6. Interstage connector I, 7. Crossover line, 8. Secondary reactor, 9. Discharge end cap, 10. Discharge pipe, 11. Heating coil, 12. Heating inlet pipe, 13. Heating outlet pipe, 14. Heat exchange inlet, 15. Heat exchange outlet, 16. Material channel I, 17. Material channel II, 18. Interstage connector II, 19. Shell, 20. Shearing element, 21. Copper sealing ring I, 22. Copper sealing ring II, 23. Inlet end cap, 24. Outlet end cap, 25. Electric heating layer. Detailed Implementation

[0037] like Figure 1 As shown, a microreactor for a high-viscosity reaction system includes an inlet end cap 2, an outlet end cap 9, a seal 3, a primary reactor 4, a secondary reactor 8, an interstage connector I 6, an interstage connector II 18, and a crossover line 7. The inlet pipe 1 is installed on the inlet end cap 2, which is located at the inlet end of the primary reactor 4. The primary reactor 4 and the secondary reactor 8 are connected via the crossover line 7. The primary reactor 4 and the crossover line 7, as well as the secondary reactor 8 and the crossover line 7, are connected via the interstage connector I 6. An outlet end cap 9 is installed at the outlet end of the secondary reactor 8, and an outlet pipe 10 is installed on the outlet end cap 9.

[0038] like Figure 2 As shown, the feed end cap 2 is a high-strength threaded connector with a built-in copper sealing ring I21; it can be welded to the feed pipe as needed. The cross-line 7 is a 90° or 180° connecting pipe with built-in shearing internals, ensuring temperature uniformity of the material at the connection point between the primary and secondary reactors. The material channel I16 of the feed end cap 2 is 1 / 4 to 1 / 2 the inner diameter of the primary reactor 4. This reduces the residence time of the material in the feed pipe, allowing it to enter the reactor quickly and achieve better mixing within the reactor.

[0039] like Figure 3 As shown, the discharge end cap 9 is a high-strength threaded connector with a built-in copper sealing ring II22; the sealing surface is chamfered to ensure no dead corners for material in the case of a large discharge port. The material channel II17 of the discharge end cap 9 is 1 / 3-3 / 4 of the inner diameter of the primary reactor 4. After the reaction is complete, the material viscosity is high, so expanding the outlet pipeline helps to facilitate smooth discharge.

[0040] like Figure 4 As shown, the outer wall of the primary reactor 4 is equipped with a heating element 5, and the inner wall is equipped with an electric heating layer 25. The primary reactor 4 has threaded ends, and the ports are chamfered and ground to ensure sealing with the feed end cap 2 or the interstage connector I 6, meeting high-pressure requirements. The heating element 5 is a jacket, and it has a heat exchange inlet 14 and a heat exchange outlet 15.

[0041] A spiral shearing element 20 is installed in the primary reactor 4 via a support. Multiple primary reactors 4 are connected in series, and each primary reactor 4 is connected to the other via an interstage connector I6.

[0042] like Figure 5 As shown, the secondary reactor 8 has a structure with threads at both ends and an internal heating coil 11. The heating coil 11 is connected to the interstage connector II 18 after being bent. The heating coil has a size of 4-8 mm and an overall length of 400-600 mm. The heating medium enters from the heating inlet pipe 12 of the interstage connector II 18, and after heat exchange, it flows out through the opposing outlet pipe 13. This enhances internal heat exchange and ensures the temperature stability and material uniformity under endothermic or exothermic conditions of the material reaction.

[0043] A heating coil 11 is installed in the inner cavity of the secondary reactor 8, and a heating element 5 is also installed on the outer wall. An electric heating layer 25 is also installed on the inner wall. The heating coil 11 is located between the electric heating layer (25) and the shearing internals of the secondary reactor 8. Multiple secondary reactors 8 are connected in series, and each secondary reactor 8 is connected to the other via an interstage connector II 18. High-viscosity systems have high-molecular-weight materials with high melting points and are prone to local solidification, which brings uncertainty to the reaction results and the safety of the experimental process. Through the heating element 5 on the outer wall of the primary reactor 4, secondary reactor 8, cross-line 7, interstage connector I 6, and interstage connector II 18, and the electric heating layer 25 on the inner wall, the material can be heated by a combination of heat transfer oil or electric heating to ensure that there are no dead corners in the cooling of the reaction equipment and to ensure the accuracy of the experimental data.

[0044] like Figure 6 As shown, a heating element 5 is also provided on the outer wall of the cross-line 7, and an electric heating layer 25 is also provided on the inner wall. Both ends of the cross-line 7 have a threaded structure. The cross-line 7 has a built-in helical shearing element 20.

[0045] like Figure 7 , 8As shown, both interstage connectors II18 and I6 have a concave sealing element 3 on the inner wall of the housing 19, a heating element 5 on the outer wall of the housing 19, and an electric heating layer 25 on the inner wall of the housing 19. The sealing element 3 is made of copper. The corners of the concave sealing element 3 are chamfered, and the two ends of the housing 19 are provided with threads for connection. The middle hole is consistent with the inner diameter of the first and second stage reactors to avoid material accumulation in dead corners, which would affect the accuracy of the test. Unlike interstage connector I6, interstage connector II18 has a partition plate in the sealing element 3. The partition plate divides the concave sealing element 3 into two chambers: an inlet chamber and an outlet chamber. The inlet chamber is connected to the inlet of the heating coil 11, and the outlet chamber is connected to the outlet of the heating coil 11. A heating inlet pipe 12 is provided on the end cap 23 of the inlet chamber, and a heating outlet pipe 13 is provided on the end cap 24 of the outlet chamber. This application uses the interstage connector II18 to connect the heating coil 11 to exchange heat with the fluid inside the secondary reactor 8, which simplifies the heating structure while enhancing internal heat exchange.

[0046] The primary reactor 4 and the secondary reactor 8 are plug flow reactors with an inner diameter of 6-40 mm and a length of 300-600 mm. They can be categorized into three types based on their internal components: high-shear, low-shear, and high-efficiency heat exchange types, and can be flexibly combined according to process requirements. Using plug flow reactors with this inner diameter allows for a small micro-reverse feed rate (in the hundreds of grams), resulting in better mixing; the heat transfer is also more uniform during the reaction. To accommodate different residence times, the length of the plug flow reactor is set at 300-600 mm, allowing for flexible increases or decreases in the number of reactors.

[0047] The reactor is connected in series with a primary reactor 4 and a secondary reactor 8 via an interstage connector I6. This design makes the reactor easy to install, occupies little space, and allows for quick disassembly during the experiment, thereby improving reaction efficiency. It can be heated by heat transfer oil, electricity, or a combination of both, ensuring that there are no dead zones in the reaction equipment and guaranteeing the accuracy of experimental data.

[0048] As another form of this utility model, the microreactor for high-viscosity reaction systems also includes an insulated tee, not shown in the figure. The three ends of the insulated tee are threaded, and an insulation layer, such as glass wool wrapped around the tee, is provided. The feed end cap 2 is located at the feed end of the primary reactor 4. Two primary reactors 4 are connected in parallel via the insulated tee, and two secondary reactors 8 are also connected in parallel via the insulated tee. These two insulated tees are connected by a crossover wire 7. A discharge end cap 9 is provided at the outlet end of the secondary reactor 8. By using the primary reactor 4 and secondary reactor 8 connected in parallel via the insulated tee and then by the crossover wire 7, the reactor is easy to install, occupies little space, and is easy to disassemble quickly during experiments, improving reaction efficiency. It can be heated by heat transfer oil, electricity, or a combination of both, ensuring no cooling dead zones in the reaction equipment and guaranteeing the accuracy of experimental data.

[0049] Research institutions and enterprises have an increasing demand for continuous flow microreactors suitable for high-viscosity systems. The continuous flow microreactor for polymerization and solution polymerization proposed in this application is economical, compact, and efficient, and is particularly suitable for reaction systems with a viscosity greater than 100,000 cp, thus providing support for the research of novel polymers. Example

[0050] like Figure 9 As shown, the reactants or intermediate products are pumped to the feed end cap 2 by a metering pump and then enter the primary reactor 4. During the forward propulsion process, efficient heat exchange and rapid reaction occur. To save space, the two primary reactors 4 are arranged in one layer, passing through the cross-line 7 before entering the second primary reactor 4. After a certain residence time, the material viscosity gradually increases, and the heat transfer coefficient decreases. A secondary reactor 8 is used at the rear of the reaction to enhance heat transfer, accelerate the later stages of polymer synthesis, and improve the conversion rate. After the reaction, the material is extruded into strips through the material channel II 17 of the large-aperture discharge end cap 9 and enters subsequent purification or granulation processes. In this embodiment, the inner diameter of the primary reactor 4 is 10 mm, the inner diameter of the secondary reactor 8 is 30 mm, the length of each stage is 50 cm, and the spacing between each layer is 30 cm. High-strength interstage connectors I 6 are used for rapid pipe connection, replacing traditional flange connections, providing a highly efficient reactor device for the development of micro-reactors for high-viscosity fluids.

[0051] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A microreactor for use with highly viscous reaction systems, characterized by: It includes a feed end cap (2), a discharge end cap (9), a primary reactor (4), a secondary reactor (8), an interstage connector I (6), an interstage connector II (18), and a crossover line (7); the feed end cap (2) is located at the inlet end of the primary reactor (4), the primary reactor (4) and the secondary reactor (8) are connected by the crossover line (7), the primary reactor (4) and the crossover line (7) are connected by the interstage connector I (6), and the secondary reactor (8) and the crossover line (7) are connected by the interstage connector II (18); the inner walls of the interstage connector I (6) and the interstage connector II (18) are provided with concave sealing elements (3), and the concave corners are chamfered; the discharge end cap (9) is located at the outlet end of the secondary reactor (8).

2. A microreactor for highly viscous reaction systems according to claim 1, characterized in that: The sealing element (3) of the inter-stage connector II (18) is provided with a partition plate, which divides the concave sealing element (3) into two cavities, an inlet cavity and an outlet cavity. The inlet cavity is connected to the inlet of the heating coil (11), and the outlet cavity is connected to the outlet of the heating coil (11). A heating inlet pipe (12) is provided on the end cap (23) of the inlet cavity, and a heating outlet pipe (13) is provided on the end cap (24) of the outlet cavity.

3. A microreactor for highly viscous reaction systems according to claim 2, characterized in that: Heating elements (5) are provided on the outer walls of the primary reactor (4), secondary reactor (8), cross line (7), interstage connector I (6) and interstage connector II (18), and electric heating layers (25) are provided on the inner walls.

4. A microreactor for highly viscous reaction systems according to claim 3, characterized in that: The spiral shearing element (20) is installed in the primary reactor (4) by means of a support.

5. A microreactor for highly viscous reaction systems according to claim 4, characterized in that: Heating coils (11) are installed inside the secondary reactor (8).

6. A microreactor for highly viscous reaction systems according to claim 5, characterized in that: The primary reactors (4) are connected in series, and the primary reactors (4) are connected to each other through interstage connector I (6).

7. A microreactor for highly viscous reaction systems according to claim 6, characterized in that: The secondary reactors (8) are connected in series, and the secondary reactors (8) are connected to each other through interstage connectors II (18).

8. A microreactor for highly viscous reaction systems according to claim 5, characterized in that: The feed end cap (2) is set at the feed end of the first-stage reactor (4). The two first-stage reactors (4) are connected in parallel through a heat-insulating tee. The two second-stage reactors (8) are also connected in parallel through a heat-insulating tee. The two heat-insulating tee are connected through a cross-line (7). The outlet end cap (9) is set at the outlet end of the second-stage reactor (8).

9. A microreactor for highly viscous reaction systems according to claim 7 or 8, characterized in that: Both the primary reactor (4) and the secondary reactor (8) are plug flow reactors with an inner diameter of 6-40 mm and a length of 300-600 mm.

10. A microreactor for highly viscous reaction systems according to claim 1, characterized in that: The material channel I (16) of the feed end cap (2) is 1 / 4 to 1 / 2 of the inner diameter of the primary reactor (4); the material channel II (17) of the discharge end cap (9) is 1 / 3 to 3 / 4 of the inner diameter of the primary reactor (4).

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