Reaction vessel for cationic living polymerization and nanofiber production device

Abstract

The application provides a reaction kettle and a nanofiber preparation device for cationic active polymerization, the reaction kettle comprises a reaction kettle body (11) which forms a containing space, an ultrasonic device (12) which is used for providing an ultrasonic field and is arranged at least partially in the interior of the reaction kettle body (11), a stirring paddle (13) which is arranged in the interior of the reaction kettle body (11) and can be driven to rotate, and a shearing machine (14) which is arranged at least partially in the interior of the reaction kettle body (11) and is used for shearing polymer fibers so that the polymer fibers in the interior of the reaction kettle body (11) are shortened.

Description

Technical Field

[0001] This application belongs to the technical field of cationic polymerization reaction equipment, and specifically relates to a reaction vessel and nanofiber preparation device for cationic active polymerization reaction. Background Technology

[0002] Cationic polymerization is characterized by its rapid reaction rate, enabling fast industrial production. However, it is prone to chain transfer, resulting in low molecular weight products. Therefore, it requires lower reaction temperatures, leading to significant energy consumption. Currently, only a few monomers, such as isobutylene, have relatively mature technologies for industrial-scale cationic polymerization production.

[0003] Cationic precipitation polymerization utilizes the poor solubility of the polymerized product as a driving force, can be carried out at room temperature, and can significantly reduce product costs. Furthermore, the reaction is a living polymerization, meaning the degree of polymerization can be adjusted by regulating the amount of monomer added or by subsequent monomer supplementation, effectively controlling the product's properties. Living cationic polymerization is characterized by rapid reaction and mild reaction conditions. However, for large-scale industrial production, suitable mass production equipment is required. Utility Model Content

[0004] This application aims to provide a reaction vessel for cationic living polymerization to meet the needs of mass production of nanofibers.

[0005] This application discloses a nanofiber preparation apparatus for a cationic living polymerization reaction reactor, comprising: a reactor body having a containment space; an ultrasonic device for providing an ultrasonic field, the ultrasonic device being at least partially disposed inside the reactor body; a stirring paddle disposed inside the reactor body and capable of being driven to rotate; and a shearing machine, at least partially disposed inside the reactor body, the shearing machine being used to shear polymer fibers, thereby shortening the polymer fibers inside the reactor body.

[0006] In at least one possible implementation, the ultrasonic device is rod-shaped and extends vertically into the reactor vessel from above.

[0007] In at least one possible implementation, the agitator extends vertically into the reactor vessel from above, and the agitator is located at the center of the reactor vessel.

[0008] In at least one possible implementation, the shearing machine extends into the reactor vessel from above at an angle relative to the vertical direction.

[0009] In at least one possible embodiment, the reactor for cationic living polymerization further includes a pump connected to the reactor body for pumping reactants into the reactor body.

[0010] In at least one possible implementation, the reactor vessel is provided with a solvent reflux port.

[0011] In at least one possible implementation, the reactor vessel is provided with a stop agent reflux port.

[0012] In at least one possible implementation, the shearing machine is telescopically movably disposed within the reactor vessel, extending to shear the polymer fibers when used for shearing, and retracting when not used for shearing.

[0013] In at least one possible implementation, the bottom of the reactor vessel is provided with a reactor discharge port, the bottom surface of the reactor vessel is a downwardly concave spherical or arc-shaped surface, and the reactor discharge port is provided with a valve that can be opened and closed.

[0014] The embodiments of this application also propose a nanofiber preparation apparatus, comprising: a reactor for cationic active polymerization as described in any of the above technical solutions; a solid-liquid separation tank connected to the reactor discharge port of the reactor for cationic active polymerization, receiving the reaction products of the reactor for cationic active polymerization, and separating the solid and liquid in the reaction products; a solvent collection tank connected to the separation tank discharge port of the solid-liquid separation tank, for collecting solvent filtered by a filter screen in the solid-liquid separation tank; a nanofiber collection tank connected to the separation tank discharge port of the solid-liquid separation tank, for collecting nanofibers filtered by a filter screen in the solid-liquid separation tank; and a terminator collection tank connected to the separation tank discharge port of the solid-liquid separation tank, for collecting terminator.

[0015] By adopting the above technical solution, the size of nanofibers can be reduced by using a shearing machine, thereby increasing the surface area of ​​the nanofibers and enabling them to perform functions such as catalytic reaction, gas storage, and heat insulation. Attached Figure Description

[0016] Figure 1 A schematic diagram of a nanofiber preparation apparatus according to an embodiment of this application is shown.

[0017] Explanation of reference numerals in the attached figures

[0018] 1. Reactor 11. Reactor body 12. Ultrasonic equipment 13. Stirring paddle 14. Shearing machine 15. Pump 16. Solvent reflux port 17. Terminator reflux port 18. Reactor discharge port

[0019] 2. Solid-Liquid Separation Tank 21. Tank Body 211. First Part 212. Second Part 22. Filter Section 23. Separation Tank Inlet 24. Separation Tank Discharge Outlet 25. Power Unit 26. Sealing Device 27. Blower 28. Termination Agent Sprayer

[0020] 3 Solvent collection tank 31 Solvent collection tank inlet 32 ​​Solvent collection tank outlet

[0021] 4. Nanofiber collecting tank; 41. Nanofiber collecting tank inlet; 42. Nanofiber collecting tank outlet.

[0022] 5 Terminator Collection Tank 51 Terminator Collection Tank Inlet 52 Terminator Collection Tank Outlet 53 Terminator Sprayer Connection Port

[0023] 6. Condensation recovery equipment Detailed Implementation

[0024] To more clearly illustrate the above-mentioned objectives, features, and advantages of this application, specific embodiments of this application are described in detail in conjunction with the accompanying drawings in this section. Besides the embodiments described in this section, this application can also be implemented in other different ways. Those skilled in the art can make corresponding improvements, modifications, and substitutions without departing from the spirit of this application; therefore, this application is not limited to the specific embodiments disclosed in this section. The scope of protection of this application should be determined by the claims.

[0025] like Figure 1 As shown, embodiments of this application propose a nanofiber preparation apparatus, which includes a reaction vessel (a reaction vessel for cationic living polymerization) 1, a solid-liquid separation tank 2, a solvent collection tank 3, a nanofiber collection tank 4, a terminator collection tank 5, and a condensation recovery device 6.

[0026] The solid-liquid separation tank 2 can be located below and connected to the reaction vessel 1. The solvent collection tank 3, nanofiber collection tank 4, and terminator collection tank 5 can all be located below the solid-liquid separation tank 2, and can be connected to the solvent collection tank 3, nanofiber collection tank 4, or terminator collection tank 5 via a selector valve. The selector valve enables the discharge port 24 of the separation tank to be connected to the solvent collection tank 3, nanofiber collection tank 4, or terminator collection tank 5.

[0027] The reaction vessel 1 includes a reaction vessel body 11, an ultrasonic device 12, a stirring paddle 13, and a shearing machine 14.

[0028] The reactor vessel 11 can be used to contain solids and liquids (e.g., cationic initiators, solvents, and monomers to be polymerized). The reactor vessel 11 may be provided with a reactor inlet, a reactor outlet 18, a solvent reflux outlet 16, and a terminator reflux outlet 17. The ultrasonic device 12, the agitator 13, and the shearing machine 14 may be at least partially disposed inside the reactor vessel 11.

[0029] The reactor vessel 11 can be cylindrical, and the discharge port 18 can be located at the bottom of the reactor vessel 11. The discharge port 18 can be equipped with an openable and closable valve. The bottom surface of the reactor vessel 11 can be a concave spherical surface or an arc surface, which facilitates the discharge of the dispersed system under gravity and its entry into the container used in the next process (i.e., the solid-liquid separation tank 2). The agitator 13 is located inside the reactor vessel 11 and can be driven to rotate by a power device such as an electric motor. The agitator 13 can extend vertically into the reactor vessel 11 from the top and can be located at the center of the reactor vessel 11. The agitator 13 can stir the dispersed system to fully emulsify it, homogenize the emulsion system, and prevent local unevenness.

[0030] An ultrasonic device 12 is used to provide an ultrasonic field, thereby fully emulsifying the dispersion system and reducing the size of the emulsion droplets. The ultrasonic device 12 can be rod-shaped and can extend vertically into the reaction vessel 11 from above. A shearing machine 14 is used to cut solid polymer fibers, reducing their size and increasing the surface area of ​​the nanofibers, enabling them to perform functions such as catalytic reaction, gas storage, and heat insulation. Optionally, the shearing machine 14 can be telescopically mounted in the reaction vessel 11. When shearing is needed, the shearing machine 14 can be extended to shear the polymer fibers; when shearing is not needed, the shearing machine 14 can be retracted, thus avoiding interference between the agitator 13 and the shearing machine 14. The shearing machine 14 can extend into the reaction vessel 11 from above at an angle relative to the vertical direction.

[0031] A pump 15 may be installed at the feed inlet of the reactor. The pump 15 is connected to the reactor tank 11 and is used to pump reactants (such as cationic initiators and solvents) into the reactor tank 11. Optionally, the pump 15 may be a peristaltic pump.

[0032] The solid-liquid separation tank 2 may include a solid-liquid separation tank body 21, a filter section 22, a rotating mechanism, a power unit 25, a sealing device 26, a blower 27, and a terminator nozzle 28.

[0033] The solid-liquid separator tank body 21 has a cavity that can be used to contain a suspension (i.e., a mixture of solids and liquids). The solid-liquid separator tank body 21 is provided with a separator tank inlet 23 and a separator tank outlet 24. The separator tank inlet 23 can be located at the upper part of the solid-liquid separator tank body 21, and the separator tank outlet 24 can be located at the bottom of the solid-liquid separator tank body 21. The solid-liquid separator tank body 21 may include a first part 211 and a second part 212, with the second part 212 located below the first part 211. The suspension entering the solid-liquid separator tank body 21 can flow from the first part 211 to the second part 212 under the action of gravity.

[0034] The filter section 22 is disposed inside the solid-liquid separation tank body 21, and the filter section 22 may be disposed between the first part 211 and the second part 212. The liquid in the suspension can pass through the filter section 22, but the solid in the suspension cannot pass through the filter section 22.

[0035] The filter section 22 may include a filter screen and a filter screen clamp. The filter screen clamp can detachably hold the filter screen, allowing for easy replacement. The filter screen may be sheet-like or plate-like. The shape of the filter screen and the cross-sectional shape of the solid-liquid separation tank body 21 may be the same (including similar sizes), for example, both the shape of the filter screen and the cross-section of the solid-liquid separation tank body 21 may be circular. The rotating mechanism may include a shaft, bearings, etc. The axis of the shaft may be perpendicular to the axis of the solid-liquid separation tank body 21; for example, the shaft may be horizontally positioned. The shaft or its axis may pass through the center of the circular filter screen. A power unit 25 may be connected to the rotating mechanism, and the power unit 25 is used to drive the filter section 22 to rotate via the rotating mechanism. The power unit 25 may include a motor.

[0036] The sealing device 26 can be installed between the rotating mechanism and the solid-liquid separation tank body 21 to seal the gap between the rotating mechanism and the solid-liquid separation tank body 21, preventing the leakage of harmful gases and liquids inside the solid-liquid separation tank body 21.

[0037] The filter section 22 can be rotatably connected to the solid-liquid separation tank body 21 via a rotating mechanism. By rotating the filter section 22, the solid-liquid separation tank 2 can be switched between the filtration state and the discharge state.

[0038] In the filtration state, the filter screen can extend horizontally, and the periphery of the filter screen can fit tightly with the inner wall of the solid-liquid separation tank 21. The solids in the suspension cannot pass through the gap between the filter screen and the inner wall of the solid-liquid separation tank 21, nor can they pass through the filter screen, so that the liquid flows through the filter screen to the second part 212, while the solids remain in the first part 211.

[0039] In the discharge state, the filter screen flips or extends in a direction inclined relative to the horizontal. For example, the filter screen can be rotated at a certain angle relative to the filtration state (e.g., it can be rotated 90 degrees to extend the filter screen vertically, or flipped (i.e., rotated 180 degrees) to allow the solids on the filter screen to fall off). The periphery of the filter screen is separated from the inner wall of the solid-liquid separation tank 21, and the first part 211 and the second part 212 are connected, allowing both solids and liquids to reach the second part 212 from the first part 211.

[0040] The bottom surface of the solid-liquid separation tank 21 can be a concave spherical or arc-shaped surface, which facilitates the discharge of the dispersion system from the discharge port 24 of the separation tank under the action of gravity, and then into the container used in the next process.

[0041] The terminator nozzle 28 can be installed in the first part 211 of the solid-liquid separation tank body 21. The terminator nozzle 28 is used to spray a terminator onto the first part 211 to terminate the polymerization reaction. For example, the terminator can be an alcohol, amine, carboxylic acid, etc. Optionally, the terminator can be ethanol.

[0042] The blower 27 can be connected to the solid-liquid separation tank body 21. The blower 27 is used to blow air into the filter section 22 to accelerate filtration.

[0043] The nanofiber preparation apparatus may also include a chiller and a hot water heater. A reaction vessel jacket is fitted around the outside of the reaction vessel tank 11, and the chiller and / or hot water heater can be connected to the reaction vessel jacket to control the temperature inside the reaction vessel tank 11. A solid-liquid separation tank jacket is fitted around the outside of the solid-liquid separation tank 21, and a hot water heater can be connected to the solid-liquid separation tank jacket to control the temperature inside the solid-liquid separation tank 21, so as to dry the solid polymer fibers.

[0044] The solvent collection tank 3 includes a solvent collection tank inlet 31 and a solvent collection tank outlet 32. The solvent collection tank inlet 31 can be connected to the separator discharge port 24, and the solvent collection tank outlet 32 ​​can be connected to the solvent return port 16 via an electric pump, so that the solvent collected in the solvent collection tank 3 can be returned to the reactor for reuse to reduce costs.

[0045] The nanofiber collection tank 4 includes a nanofiber collection tank inlet 41 and a nanofiber collection tank outlet 42. The nanofiber collection tank inlet 41 can be connected to the separation tank outlet 24.

[0046] The terminator collection tank 5 includes a terminator collection tank inlet 51, a terminator collection tank outlet 52, and a terminator nozzle connection port 53. The terminator collection tank inlet 51 can be connected to the separator discharge port 24, and the terminator collection tank outlet 52 can be connected to the terminator return port 17 via an electric pump. The terminator nozzle connection port 53 can be connected to one end of the condensation recovery device 6, and the other end of the condensation recovery device 6 can be connected to the terminator nozzle 28, thereby allowing the terminator collected in the terminator collection tank 5 to be recycled, reducing costs.

[0047] The following is combined Figure 1 This paper describes the process of preparing hollow nanofibers using the nanofiber preparation apparatus adapted to this application.

[0048] A cationic initiator and a solvent are introduced into the reactor tank 11 through the reactor inlet. For example, the solvent can be an alkane. Optionally, the solvent can be cyclohexane, n-hexane, n-heptane, etc., preferably n-heptane. An ultrasonic field is applied by an ultrasonic device 12, and stirring is performed using a stirring paddle 13 to fully emulsify the dispersion system, resulting in an emulsion. The monomer to be polymerized is added through the reactor inlet to initiate the polymerization reaction, thereby obtaining polymer fibers. The fiber suspension then enters the solid-liquid separation tank 21 through the separation tank inlet 23. The solid-liquid separation tank 21 remains in a filtering state, and the suspension of solid polymer fibers and solvent (e.g., an alkane) falls into the filter section 22, where a blower 27 accelerates the filtration process. After filtration, the liquid solvent passes through the filter section 22 and is located in the second section 212, while the solid polymer fibers are blocked by the filter section 22 and located in the first section 211. The liquid solvent flows through the discharge port 24 of the separator to the solvent collection tank 3. The solvent in the solvent collection tank 3 can also be pumped to the solvent return port 16 and enter the reactor body 11. Then, the terminator nozzle 28 is opened to spray the terminator (e.g., ethanol) to terminate the polymerization reaction. Then, the power unit 25 drives the filter section 22 to rotate, switching the solid-liquid separator 2 to the discharge state, so that the solid polymer fibers and terminator located in the first section 211 fall into the second section 212 and enter the terminator collection tank 5 through the discharge port 24 of the separator. The solid polymer fibers and terminator are pumped back to the reactor body 11 through the discharge port 52 of the terminator collection tank. The ultrasonic device 12 and the stirring paddle 13 provide ultrasonic and stirring effects, respectively, and the shearing machine 14 shears and breaks down the fibers. The filter section 22 switches to filtration mode, and the crushed solid polymer fibers and terminating agent can enter the solid-liquid separation tank 21 through the separator inlet 23. The blower 27 blows air to accelerate filtration. After filtration, the terminating agent passes through the filter section 22 and is located in the second part 212, while the solid polymer fibers are blocked by the filter section 22 and are located in the first part 211. The terminating agent flows through the separator discharge port 24 to the terminating agent collection tank 5. Then, the hot water heater heats the solid-liquid separation tank 2 to dry the solid polymer fibers. The power unit 25 drives the filter section 22 to rotate, causing the solid-liquid separation tank 2 to switch to discharge mode. The solid polymer fibers located in the first part 211 enter the nanofiber collection tank 4 through the separator discharge port 24, and can then be discharged through the nanofiber collection tank outlet 42.

[0049] In one possible implementation, 5 liters of n-heptane and 15 milliliters of boron trifluoride diethyl ether are added to reactor vessel 11. After the ultrasonic device 12 is turned on for 3 minutes, 150 milliliters of divinylbenzene (DVB) and 50 milliliters of indene are added, and the agitator 13 is rotated at a speed of 150 rpm. After the polymerization reaction has proceeded for 2 minutes, the suspension is poured into solid-liquid separation tank 2 to filter out the solvent, which is then allowed to flow into solvent collection tank 3. The discharge port 24 of the separation tank is closed, and the terminator nozzle 28 is opened to thoroughly rinse the solid polymer fibers, and 5 liters of ethanol are added. The suspension is then poured into terminator collection tank 5, and an electric pump is used to pump the suspension back into reactor vessel 11 through terminator return port 17. The ultrasonic device 12, agitator 13, and shearing machine 14 are then turned on, with the agitator 13 rotating at a speed of 500 rpm and the shearing machine 14 rotating at a speed of 3000 rpm for 10 minutes. After the reaction is complete, the suspension is introduced into a solid-liquid separation tank 2, and the filtered ethanol is collected in a terminator collection tank 5. The filtered solid is dried by heating and then falls into a nanofiber collection tank 4 through a rotating filter section 22. Through the above steps, 20 grams of solid hollow nanofibers with diameters between 50 and 70 nanometers can be obtained in a single reaction.

[0050] As described above, this application also provides a nanofiber preparation apparatus, which may include:

[0051] Reactor used for cationic living polymerization reactions;

[0052] Solid-liquid separation tank 2 is connected to the reactor discharge port 18 of the reactor used for cationic active polymerization reaction, receives the reaction products of the reactor used for cationic active polymerization reaction, and separates the solid and liquid in the reaction products;

[0053] Solvent collection tank 3 is connected to the separation tank discharge port 24 of the solid-liquid separation tank 2 and is used to collect the solvent after it has been filtered by the filter screen in the solid-liquid separation tank 2.

[0054] A nanofiber collection tank 4, connected to the discharge port 24 of the solid-liquid separation tank 2, is used to collect nanofibers filtered through the filter screen in the solid-liquid separation tank 2; and

[0055] Terminator collection tank 5, which is connected to the separation tank discharge port 24 of the solid-liquid separation tank 2, is used to collect terminator.

[0056] The nanofiber preparation apparatus proposed in this application can be used for mass production of hollow nanofibers. By collecting the solvent and the terminator separately and recycling the solvent and the terminator, the production cost can be reduced.

[0057] It should be understood that at least some aspects or features of the above-described implementation methods, embodiments, or examples can be appropriately combined.

[0058] It is understood that, in this application, when the number of parts or components is not specifically limited, the number can be one or more, where multiple refers to two or more. For cases where the number of parts or components shown in the drawings and / or described in the specification is, for example, two, three, four, etc., this specific number is generally exemplary and not restrictive, and can be understood as multiple, i.e., two or more; however, this does not mean that this application excludes the case of one.

[0059] In this application, unless otherwise expressly stated or limited, terms such as "installation," "assembly," "connection," "linking," "joining," "linking," "abutment," "communication," "connection," "conduction," "fixing," and "fastening" should be interpreted broadly, for example, they can be direct or indirect. For instance, regarding connection, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium; it can be the internal communication of two components or the interaction between two components, unless otherwise expressly stated or limited. For instance, regarding communication / conduction, it can be direct communication / conduction or indirect communication / conduction through an intermediate medium. Those skilled in the art can understand the specific meaning of the above terms in this application according to the specific circumstances.

[0060] In this application, unless otherwise expressly stated or limited, a component being disposed / installed / located / enclosed / placed within, inside, or incorporated in another component can be either of the following two situations: a portion or a majority of the one component is located within the other component; or the one component is completely enclosed within the other component.

[0061] Although the present application has been described in detail using the above embodiments, it will be apparent to those skilled in the art that the present application is not limited to the embodiments described herein. The present application can be modified and implemented as alternative embodiments without departing from the spirit and scope of the present application as defined by the claims. Therefore, the description in this specification is for illustrative purposes only and does not have any limiting meaning for the present application.

Claims

1. A reaction vessel for cationic living polymerization, characterized in that, include: A reaction vessel tank, wherein the reaction vessel tank forms a receiving space; An ultrasonic device for providing an ultrasonic field, the ultrasonic device being at least partially disposed inside the reactor vessel; A stirring paddle is disposed inside the reactor vessel and is capable of being driven to rotate. A shearing machine, at least partially disposed inside the reactor vessel, is used to cut polymer fibers, thereby shortening the polymer fibers inside the reactor vessel.

2. The reactor for cationic living polymerization according to claim 1, characterized in that, The ultrasonic device is rod-shaped and extends vertically into the reactor vessel from above.

3. The reactor for cationic living polymerization according to claim 1, characterized in that, The stirring paddle extends vertically into the reactor vessel from above, and is located at the center of the reactor vessel.

4. The reactor for cationic living polymerization according to claim 1, characterized in that, The shearing machine extends into the reactor vessel from above at an angle relative to the vertical direction.

5. The reactor for cationic living polymerization according to claim 1, characterized in that, The reactor for cationic living polymerization also includes a pump connected to the reactor body, which is used to pump reactants into the reactor body.

6. The reactor for cationic living polymerization according to claim 1, characterized in that, The reactor vessel is equipped with a solvent reflux port.

7. The reactor for cationic living polymerization according to claim 1, characterized in that, The reactor vessel is equipped with a stop agent reflux port.

8. The reactor for cationic living polymerization according to claim 1, characterized in that, The shearing machine is telescopically and movably mounted on the reactor vessel. When the shearing machine is used for shearing, it can extend to shear the polymer fibers. When the shearing machine is not used for shearing, it can retract.

9. The reaction vessel for cationic living polymerization according to claim 1, characterized in that, The bottom of the reactor vessel is provided with a reactor discharge port, and the bottom surface of the reactor vessel is a concave spherical surface or a circular arc surface. The discharge port of the reactor is equipped with a valve that can be opened and closed.

10. A nanofiber preparation apparatus, characterized in that, include: The reaction vessel for cationic living polymerization according to any one of claims 1 to 9; A solid-liquid separation tank is connected to the discharge port of the reactor used for cationic active polymerization, receives the reaction products of the reactor used for cationic active polymerization, and separates the solid and liquid in the reaction products; A solvent collection tank, which is connected to the discharge port of the solid-liquid separation tank, is used to collect the solvent after it has been filtered by the filter screen in the solid-liquid separation tank; A nanofiber collection tank, connected to the discharge port of the solid-liquid separation tank, is used to collect nanofibers filtered through the filter screen in the solid-liquid separation tank; and A terminator collection tank, which is connected to the discharge port of the solid-liquid separation tank, is used to collect the terminator.

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