Reaction device
By designing vertical and horizontal liquid inlet pipes, stirring shafts and auxiliary liquid inlet units in the reaction device, the problem of uneven material mixing during the preparation of epichlorohydrin rubber is solved, and the stability, uniformity and safety of the reaction are achieved, which is suitable for the preparation of small-scale samples.
Patent Information
- Application Number
- CN202422827854.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-19
- Publication Date
- 2025-09-19
- Estimated Expiration
- 2034-11-19
AI Technical Summary
The existing reaction device has the problem of uneven material mixing during the preparation process of epichlorohydrin rubber.
A reaction device was designed, including a kettle body and a liquid inlet pipe. The liquid inlet pipe had a vertical section and a horizontal section. Multiple discharge ports were set on the horizontal section. The stirring shaft was arranged vertically, and the stirring paddle had an adjustable position. The auxiliary liquid inlet unit ensured the sealing and safety of catalyst addition through a three-way valve and a rubber gasket. The monomer flow control unit adjusted the raw material dripping acceleration.
It achieves uniform reaction of materials in a wide viscosity range, improves the stability and uniformity of the reaction, avoids local overheating and raw material aggregation, ensures the safety and controllability of the reaction, is suitable for small-scale sample preparation, and reduces raw material loss.
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Figure CN223351645U_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of rubber preparation, and in particular to a reaction device. Background Art
[0002] As a high-performance specialty rubber, epichlorohydrin rubber (ECR) boasts excellent oil, ozone, and chemical resistance, as well as low-temperature flexibility. It enjoys widespread and critical applications in numerous fields, including the automotive, aerospace, and petrochemical industries. Experimental preparation of ECR is crucial for understanding its polymerization mechanism, optimizing synthesis process parameters, and developing new ECR materials.
[0003] In the existing reaction device, the materials are mixed unevenly during the preparation of epichlorohydrin rubber. Utility Model Content
[0004] In view of this, the purpose of this application is to provide a reaction device for solving the technical problem of uneven material mixing existing in the prior art.
[0005] To achieve at least one of the above objectives, this application provides the following technical solutions:
[0006] In the first aspect, the present application provides a reaction device, comprising a kettle body and a liquid inlet pipe; wherein the liquid inlet pipe comprises a vertical section and a horizontal section; the vertical section has a top end for material entry, and a bottom end connected to the horizontal section; a plurality of discharge ports are provided on the horizontal section, and the plurality of discharge ports are spaced apart along the length direction of the horizontal section.
[0007] In some embodiments, it also includes a stirring shaft, which is vertically arranged in the kettle body; the horizontal section is in the shape of a ring arranged around the stirring shaft.
[0008] In some embodiments, the radius of the horizontal section is r1, and the radius of the stirring shaft is r2, wherein 1.5*r2≤r1≤2*r2.
[0009] In some embodiments, the stirring shaft includes a main shaft and a plurality of stirring paddles; wherein the main shaft is arranged vertically, the stirring paddles are fixed at a first position or a second position of the main shaft, and the first position and the second position are arranged vertically at intervals.
[0010] In some embodiments, the agitator includes a ring-shaped part, a plurality of blades and a locking bolt; wherein the blades are fixed on the outside of the ring-shaped part; the ring-shaped part is sleeved on the main shaft, and a connecting screw hole is provided on the ring-shaped part; the connecting screw hole passes through the ring-shaped part radially; the locking bolt is connected to the ring-shaped part through the connecting screw hole, and the agitator is fixed on the main shaft when the locking bolt is pressed against the main shaft.
[0011] In some embodiments, a cover plate for closing the horizontal section is provided at one end of the horizontal section away from the vertical section, and a first notch is provided on the cover plate, which connects the inner cavity of the horizontal section with the inner cavity of the kettle body.
[0012] In some embodiments, it also includes a monomer flow control unit fixed on the kettle body, the monomer flow control unit includes a feed pipe and a flow regulating valve, the flow regulating valve is connected to the feed pipe, and the feed pipe is connected to the vertical section for feeding fluid into the vertical section.
[0013] In some embodiments, it also includes a pipeline interface, an auxiliary liquid inlet unit and an emptying pipeline. The pipeline interface is used to inject protective gas into the kettle body or vacuum the kettle body. The auxiliary liquid inlet unit is used to inject solvent and / or catalyst into the kettle body. The emptying pipeline is used for the gas in the kettle body to flow out.
[0014] In some embodiments, the auxiliary liquid inlet unit includes a three-way valve, a first tube and a rubber gasket; wherein one end of the three-way valve is connected to the kettle body, and the other end is connected to the first tube; the rubber gasket seals the first tube.
[0015] In some embodiments, an external thread is provided on the outer side of the end of the first tube away from the three-way valve, and a rubber gasket is provided on the end of the first tube away from the three-way valve; the auxiliary liquid inlet unit also includes a pressure cover, which includes a connecting part and a clamping part; the connecting part is an annular part with an internal thread provided on the inner side, and the connecting part is threadedly connected to the first tube; the clamping part is fixed at one end of the connecting part, and the inner diameter of the clamping part is smaller than the inner diameter of the connecting part, and the clamping part presses the rubber gasket on the end of the first tube.
[0016] In the above technical solution, the discharge ports are arranged at intervals on the horizontal section, so that the material flowing out of the discharge ports is relatively dispersed, ensuring that the reaction materials can react evenly within a wide viscosity range, thereby ensuring reaction stability and uniformity.
[0017] The annular horizontal section ensures that the raw materials can be distributed as evenly as possible regardless of their viscosity, avoiding the risk of raw materials gathering at the port and local overconcentration of raw materials when traditional feed pipes encounter high-viscosity materials, leading to uneven reaction and local overheating.
[0018] The stirring shaft with adjustable stirring paddle position ensures that the reaction materials can react evenly within a wide range of preparation amount and viscosity, ensuring reaction stability, uniformity and reproducibility.
[0019] The three-way valve and sealing rubber gasket of the auxiliary liquid inlet unit not only facilitate the addition of catalyst and reduce loss, but also ensure the sealing and safety of the reaction system and prevent impurities from entering and material leakage.
[0020] The monomer flow control unit is used to adjust the raw material droplet addition speed to avoid the safety hazards caused by the one-pot addition method, ensure the controllable reaction heat, and enhance the controllability and repeatability of the reaction.
[0021] The device has a reasonable structure and complete functions, and can achieve a controllable single preparation amount of 50 to 300g, solving the difficulties of insufficient preparation amount and safety of small-scale sample preparation, and avoiding the problems of complex operation of large-scale equipment and large raw material loss. BRIEF DESCRIPTION OF THE DRAWINGS
[0022] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following briefly introduces the drawings required for use in the embodiments or descriptions of the prior art. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.
[0023] Figure 1 This is a schematic diagram of the overall structure of a kettle body in a cutaway embodiment;
[0024] Figure 2 is a schematic diagram of the top view of the liquid inlet pipe in an embodiment;
[0025] Figure 3 is a schematic structural diagram of a single flow control unit in an embodiment;
[0026] Figure 4 is a schematic cross-sectional view of the connection position between the stirring paddle and the main shaft in an embodiment;
[0027] Figure 5 is a schematic structural diagram of an auxiliary liquid inlet unit in an embodiment;
[0028] Figure 6 It is a schematic diagram of the cross-sectional structure of the sealing cover and the pressing cover in an embodiment.
[0029] The reference numerals are as follows:
[0030] 1. Kettle body; 11. Kettle body; 12. Kettle cover; 2. Liquid inlet pipe; 21. Vertical section; 22. Horizontal section; 221. Discharge port; 23. Cover plate; 24. First notch; 3. Stirring shaft; 31. Main shaft; 32. Stirring paddle; 321. Ring part; 322. Paddle; 323. Locking bolt; 4. Single flow control unit; 41. Feed pipe; 42. Flow regulating valve; 43. Transparent part; 5. Pipe interface; 6. Auxiliary liquid inlet unit; 61. Three-way valve; 62. First pipe; 63. Rubber gasket; 64. Pressure cover; 65. Sealing cover; 7. Drain pipe. DETAILED DESCRIPTION
[0031] The present application will be further described in detail below through the accompanying drawings and examples, through which the features and advantages of the present application will become more clear and distinct.
[0032] Unless otherwise defined, all technical and scientific terms used in this application have the same meanings as commonly understood by technicians in the technical field to which this application belongs; the terms used in this application are only for the purpose of describing specific embodiments and are not intended to limit this application; the terms "including" and "having" in the specification of this application and the above-mentioned drawings and any variations thereof are intended to cover non-exclusive inclusions.
[0033] The phrase "embodiment" mentioned in this application means that a particular feature, structure, or characteristic described in conjunction with the embodiment may be included in at least one embodiment of the application. The appearance of this phrase in various places in the specification does not necessarily refer to the same embodiment, nor does it refer to independent or alternative embodiments that are mutually exclusive with other embodiments. It is understood, both explicitly and implicitly, by those skilled in the art that the embodiments described in this application may be combined with other embodiments.
[0034] The term "exemplary" is used herein to mean "serving as an example, embodiment, or illustration." Any embodiment described as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments. Although various aspects of the embodiments are shown in the drawings, the drawings are not necessarily drawn to scale unless otherwise indicated.
[0035] In the description of this application, the technical terms "first", "second", "third", etc. are only used to distinguish different objects and cannot be understood as indicating or implying relative importance or implicitly indicating the quantity, specific order or primary and secondary relationship of the indicated technical features.
[0036] In the description of this application, the technical term "and / or" is simply a description of the association relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A exists alone, A and B exist simultaneously, and B exists alone. In addition, the character " / " in this document generally indicates that the related objects are in an "or" relationship.
[0037] In the description of this application, the orientations or positional relationships indicated by technical terms such as "upper", "lower", "inside", "outside", "front", "back", "left", "right", "top", and "bottom" are orientations or positional relationships based on the working state of this application. They are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation. Therefore, they cannot be understood as limitations on this application.
[0038] In the description of this application, unless otherwise specified or limited, technical terms such as "mounted," "connected," "connect," and "fixed" should be understood broadly. For example, these terms may refer to fixed connections, removable connections, or integration; mechanical connections or electrical connections; direct connections or indirect connections through an intermediary; and internal connections between two components or interactions between two components. Those skilled in the art will understand the specific meanings of these terms in this application based on the specific circumstances.
[0039] In the description of this application, unless otherwise expressly specified or limited, a first feature being "above" or "below" a second feature may mean that the first and second features are in direct contact, or that the first and second features are in indirect contact through an intermediate medium. Furthermore, a first feature being "above," "above," and "above" a second feature may mean that the first feature is directly above or obliquely above the second feature, or simply means that the first feature is at a higher level than the second feature. A first feature being "below," "below," and "below" a second feature may mean that the first feature is directly below or obliquely below the second feature, or simply means that the first feature is at a lower level than the second feature.
[0040] The "parallel" and "perpendicular" mentioned in this application can not only be completely parallel or perpendicular, but also have a certain error; for example, if the angle between the two is greater than or equal to 0° and less than or equal to 5°, the two are considered to be parallel to each other; if the angle between the two is greater than or equal to 85° and less than or equal to 95°, the two are considered to be perpendicular to each other.
[0041] In the description of the present application, “a plurality of” means two or more (including two), unless otherwise clearly and specifically defined.
[0042] In the description of this application, the same reference numerals represent the same components, and for the sake of brevity, detailed descriptions of the same components in different embodiments are omitted. It should be understood that the thickness, length, and other dimensions of the various components in the embodiments of this application, as well as the overall thickness, length, and other dimensions of the integrated device shown in the drawings are merely illustrative and do not constitute any limitation on this application.
[0043] As part of the creative concept of this application, before describing the embodiments of this application, it is necessary to analyze the causes of the problem of uneven material mixing in related technologies, and obtain the technical solutions of the embodiments of this application through reasonable analysis.
[0044] In related technology, epichlorohydrin rubber is a rubber made by polymerizing polymer-grade epichlorohydrin or a mixture with a comonomer such as ethylene oxide. The raw materials for producing epichlorohydrin rubber include monomers, catalysts, and solvents. Epichlorohydrin is the primary monomer of epichlorohydrin rubber and can be used alone or in copolymers with other monomers, such as ethylene oxide. Common catalysts include coordinated anionic catalysts or catalysts based on triisobutylaluminum. Toluene is a common solvent used to dissolve the monomers and catalyst.
[0045] The polymerization reaction of epichlorohydrin rubber is to dissolve epichlorohydrin in toluene, add a catalyst, and carry out ring-opening polymerization at appropriate temperature and pressure. After the reaction is completed, a large amount of n-hexane is added to precipitate the polymer, and then it is washed with solvents such as methanol to remove impurities.
[0046] The reaction device disclosed in this application is mainly used for the preparation of epichlorohydrin rubber. Of course, it can also be used to prepare other materials that require similar preparation processes, which will not be explained in detail here.
[0047] To this end, the present application provides a reaction device, including a kettle body and a liquid inlet pipe, the liquid inlet pipe including a vertical section and a horizontal section; the vertical section has a top end for material entry, and a bottom end connected to the horizontal section, and the bottom end is located below the top end; the horizontal section is provided with multiple discharge ports, and the multiple discharge ports are spaced apart along the length direction of the horizontal section, thereby solving the technical problem of uneven material mixing in the prior art.
[0048] The technical solutions of the embodiments of the present application are described in detail below with reference to the accompanying drawings. The technical features involved in the different implementation modes of the present application described below can be combined with each other as long as there is no conflict between them.
[0049] The present application discloses a reaction device, referring to Figure 1 , Figure 1 This is a structural schematic diagram showing the liquid inlet pipe 2 in the kettle body 1 in the reaction device. The reaction device includes the kettle body 1 and the liquid inlet pipe 2. The liquid inlet pipe 2 includes a vertical section 21 and a horizontal section 22. The vertical section 21 has a top end for material entry and a bottom end connected to the horizontal section 22, and the bottom end is located below the top end; the horizontal section 22 is provided with multiple discharge ports 221, and the multiple discharge ports 221 are arranged at intervals along the length direction of the horizontal section 22.
[0050] Exemplarily, the kettle 1 comprises a kettle body 11 and a kettle cover 12. The kettle body 11 is a cylindrical double-layer structure, with both the inner and outer layers of the kettle body 11 made of high-strength, pressure-resistant, and corrosion-resistant glass. The outer layer of the kettle body 11 is encased in a frame, which covers at least one-third of the outer layer of the kettle body 11. In this embodiment, the frame is made of stainless steel and provides secure support for the kettle body 11.
[0051] The jacket cavity is located between the inner and outer layers of the kettle body 11, and cooling / heating liquid can be injected into the kettle to control the temperature according to experimental requirements to meet the requirements of different reaction temperatures.
[0052] The kettle cover 12 covers the upper part of the kettle body 11, so that the inner cavity of the kettle body 1 forms a cavity for raw material reaction.
[0053] In this embodiment, the liquid inlet pipe 2 is disposed on the kettle cover 12. In another embodiment, the liquid inlet pipe 2 is disposed on the kettle body 11. The liquid inlet pipe 2 is a passage for materials to enter the interior of the kettle body 11 from the outside. In this embodiment, the liquid inlet pipe 2 is used to allow polymer-grade epichlorohydrin, which is a raw material, to enter the interior of the kettle body 11.
[0054] The liquid inlet pipe 2 includes a vertical section 21 and a horizontal section 22, which are interconnected. The vertical section 21 is arranged vertically, and in this embodiment, it is arranged vertically. In another embodiment, the vertical section 21 is arranged at an angle. The top end of the vertical section 21 is fixed to the kettle cover 12, and the bottom end of the vertical section 21 is fixedly connected to the horizontal section 22. The raw material enters from the top end of the vertical section 21, flows along the vertical section 21, passes through the bottom end of the vertical section 21, and enters the horizontal section 22.
[0055] In this embodiment, the horizontal section 22 is arranged horizontally. In another embodiment, a portion of the horizontal section 22 is arranged tilted, or the entire horizontal section 22 is arranged tilted, with the tilt angle being no greater than 30°, and the highest position of the horizontal section 22 is lower than the top of the vertical section 21.
[0056] The horizontal section 22 is provided with multiple discharge ports 221, spaced apart along its length. The shape of the discharge ports 221 is determined by design requirements and may be circular, oval, square, or other shapes. The discharge ports 221 connect the interior of the horizontal section 22 with the interior of the kettle body 11, allowing the raw material within the horizontal section 22 to flow into the kettle body 11 through the discharge ports 221.
[0057] There are multiple discharge ports 221, preferably 7. The length direction of the horizontal section 22 is the direction extending from the first end of the horizontal section 22 toward the second end of the horizontal section 22 along the centerline of the horizontal section 22. The first end is the end of the horizontal section 22 connected to the vertical section 21, and the second end is the end of the horizontal section 22 away from the vertical section 21.
[0058] In this embodiment, the plurality of discharge ports 221 are arranged at equal intervals on the horizontal section 22. In another embodiment, the plurality of discharge ports 221 are arranged at intervals on the horizontal section 22, and the gaps between adjacent discharge ports 221 are different. For example, the distance between adjacent discharge ports 221 gradually decreases as they move away from the first end.
[0059] After the raw materials enter the horizontal section 22, they are discharged from the discharge port 221 of the horizontal section 22 under the action of the pressure difference and are evenly distributed throughout the inner cavity of the kettle body 1. This can avoid the situation where the raw materials in local areas are too concentrated when the viscosity of the raw materials is too high, and the raw materials cannot fully participate in the reaction, thereby affecting the reaction effect. It ensures that regardless of the viscosity of the raw materials, the raw materials can enter the inner cavity of the kettle body 1 in a manner as evenly dispersed as possible, which is conducive to the full mixing of the raw materials and improves the uniformity of the reaction.
[0060] In order to prepare the chloroether rubber, the reaction device further includes a component for the introduction of solvent, catalyst or gas, and the reaction device also includes a stirring power unit, which will be described in the following content.
[0061] In this embodiment, the stirring power unit is arranged in the center of the kettle cover 12. In another embodiment, the stirring power unit can be arranged in the inner cavity of the kettle body 11 or at the bottom of the kettle body 11 as needed.
[0062] In this embodiment, the member for the solvent, catalyst or gas to enter is arranged on the kettle cover 12. In another embodiment, the member for the solvent, catalyst or gas to enter is arranged on the kettle body 11.
[0063] A discharge port is provided at the bottom of the kettle body 11 and is opened and closed by a valve.
[0064] The above and below described in this embodiment indicate that when the reaction device is normally placed or used, it is located above or below in the vertical direction, and does not only mean directly below or directly above, but can also be expressed as obliquely below or obliquely above. White steel in this embodiment refers to stainless steel.
[0065] Furthermore, the gap between the bottom end of the vertical section 21 and the bottom wall of the kettle body 1 is any gap between 5 and 8 cm. For example, the gap between the bottom end of the vertical section 21 and the bottom wall of the kettle body 1 is 6 cm.
[0066] Reference Figure 1 As an optional solution, the stirring power unit includes a stirring shaft 3, which is vertically arranged in the kettle body 1. The horizontal section 22 is in the shape of a ring arranged around the stirring shaft 3.
[0067] For example, the stirring shaft 3 is provided on the kettle cover 12, the stirring shaft 3 is located in the inner cavity of the kettle body 1, and the stirring shaft 3 is partially located in the material in the kettle body 1. The rotation axis of the stirring shaft 3 is the axis of the stirring shaft 3 and is arranged in the vertical direction. The stirring power unit stirs the material in the kettle body 1 by rotating the stirring shaft 3.
[0068] In this embodiment, the stirring power unit further includes a motor, which is fixed on the kettle body 1 and connected to the stirring shaft 3 for driving the stirring shaft 3 to rotate.
[0069] Reference Figure 2In this embodiment, the horizontal section 22 is configured to be annular, where the annular shape is a circular ring, and there is a gap between the first end and the second end of the horizontal section 22 .
[0070] In another embodiment, the horizontal section 22 is configured to be spiral, square, U-shaped, elliptical or other shapes.
[0071] In this embodiment, the vertical center axis of the annular horizontal segment 22 coincides with the rotation axis of the agitator shaft 3. In another embodiment, a gap may exist between the vertical center axis of the annular horizontal segment 22 and the rotation axis of the agitator shaft 3, or the agitator shaft 3 may intersect with the agitator shaft 3. However, it is necessary to ensure that a gap always exists between the agitator shaft 3 and the horizontal segment 22 during rotation.
[0072] The horizontal section 22 is arranged around the stirring shaft 3. When the raw materials flow into the inner cavity of the kettle body 1 from the discharge port 221, the raw materials flowing out from different discharge ports 221 are relatively dispersed and can be stirred relatively evenly by the stirring shaft 3, further reducing the situation where the local raw materials are too concentrated, improving the stirring efficiency of the stirring shaft 3, and facilitating the full reaction of the raw materials and improving the reaction effect.
[0073] Reference Figure 1 As an optional solution, the radius of the horizontal section 22 is r1, and the radius of the stirring shaft 3 is r2, wherein 1.5*r2≤r1≤2*r2.
[0074] For example, the radius of the stirring shaft 3 is the horizontal distance between the farthest end of the stirring shaft 3 and the rotation axis of the stirring shaft 3 when the stirring shaft 3 rotates, and the radius of the horizontal section 22 is the radius of the ring formed by the horizontal section 22. Figure 1 , the radius r1 of the horizontal section 22 and the radius r2 of the stirring shaft 3 are marked.
[0075] In this embodiment, 1.8*r2=r1. In another embodiment, 1.5*r2=r1, 1.6*r2=r1, 1.7*r2=r1, 1.9*r2=r1, 2*r2=r1, 1.53*r2=r1, or 1.87*r2=r1.
[0076] By the above-mentioned size limitation, when the raw materials flow from the horizontal section 22 into the inner cavity of the kettle body 1, the stirring effect of the stirring shaft 3 on the raw materials is relatively high, the dispersion effect of the raw materials is good, and the reaction efficiency is relatively high.
[0077] Reference Figure 1 As an optional solution, the stirring shaft 3 includes a main shaft 31 and a plurality of stirring paddles 32. The main shaft 31 is arranged vertically, and the stirring paddles 32 are fixed at a first position or a second position of the main shaft 31, and the first position and the second position are arranged vertically at intervals.
[0078] For example, the main shaft 31 and the plurality of stirring paddles 32 are made of stainless steel. The bottom of the main shaft 31 is positioned 3 cm above the bottom of the kettle. A motor is connected to the main shaft 31, driving the main shaft 31 to rotate about its axis. The stirring paddles 32 are fixed to the main shaft 31 and can be fixed in at least two positions on the main shaft 31.
[0079] In this embodiment, the stirring paddles 32 can be fixed at multiple positions on the main shaft 31 , and the multiple positions are arranged at intervals along the vertical direction. Figure 1 FIG. 3 shows a situation where the stirring paddle 32 is fixed at the first position of the main shaft 31 .
[0080] This embodiment discloses a connection method for fixing the stirring paddle 32 on the main shaft 31. The stirring paddle 32 can also be fixed using other existing fixing connection methods as needed, as long as a component can be fixed at at least two positions on a shaft.
[0081] The position of the stirring paddle 32 on the main shaft 31 can be adjusted up and down according to actual needs to meet the stirring requirements of different preparation amounts and ensure uniform stirring.
[0082] Three stirring paddles 32 are provided, and the three stirring paddles 32 are arranged at intervals along the length direction of the main shaft 31 .
[0083] Reference Figure 3 As an optional solution, the stirring paddle 32 includes a ring member 321, a plurality of blades 322, and a locking bolt 323. The blades 322 are fixed to the outside of the ring member 321; the ring member 321 is sleeved on the main shaft 31 and is provided with a connecting screw hole; the connecting screw hole radially penetrates the ring member 321.
[0084] The locking bolt 323 is connected to the annular member 321 through a connecting screw hole. When the locking bolt 323 presses against the main shaft 31 , the stirring paddle 32 is fixed on the main shaft 31 .
[0085] Exemplarily, three blades 322 are provided, and the three blades 322 are fixed on the ring member 321 at equal intervals. In this embodiment, the blades 322 and the ring member 321 are integrally formed. In another embodiment, the blades 322 and the ring member 321 can be connected by welding, interference fit or other connection methods.
[0086] The inner diameter of the annular member 321 is equal to the diameter of the main shaft 31, and the annular member 321 is sleeved on the main shaft 31. In this embodiment, three connecting screw holes are provided, and the three connecting holes are provided on the annular member 321 at equal intervals.
[0087] After the ring member 321 is moved to the first position or the second position, the locking bolt 323 is rotated so that the locking bolt 323 presses against the main shaft 31, thereby securing the stirring paddle 32 to the main shaft 31. To adjust the position of the ring member 321, the locking bolt 323 is loosened, and the stirring paddle 32 is slid along the surface of the main shaft 31 to the set position, and then the locking bolt 323 is used to secure the stirring paddle 32 to the main shaft 31.
[0088] The height of the stirring paddle 32 can be adjusted according to actual needs to improve the flexibility of the device, optimize the stirring effect, and improve the material mixing efficiency.
[0089] Reference Figure 2 As an optional solution, a cover plate 23 for closing the horizontal section 22 is provided at one end of the horizontal section 22 away from the vertical section 21 , and a first notch 24 is provided on the cover plate 23 , which connects the inner cavity of the horizontal section 22 with the inner cavity of the kettle body 1 .
[0090] Illustratively, the cover plate 23 is fixed to the second end of the horizontal section 22, and the cover plate 23 closes the pipe opening of the horizontal section 22. In this embodiment, the first notch 24 is a hole provided in the cover plate 23. The shape of the hole is determined as needed, such as circular, square, or trapezoidal. In this embodiment, the hole in the cover plate 23 is a circular hole, and the diameter of the first notch 24 is equal to half the inner diameter of the horizontal section 22.
[0091] In another embodiment, the first notch 24 is a notch provided on the edge of the cover plate 23 , and the shape of the notch is determined according to design requirements. In another embodiment, the first notch 24 includes a plurality of notches provided on the edge of the cover plate 23 .
[0092] The nozzle at the second end can cause excessive material to flow out of the outlet, easily leading to material accumulation. However, if the nozzle at the second end is completely closed, material will accumulate near the second end of the horizontal section 22. This embodiment uses a cover plate 23 having a first notch 24 fixed to the second end of the horizontal section 22 to regulate the flow of material within the horizontal section 22 and facilitate the complete outflow of material.
[0093] Reference Figure 1 as well as Figure 4 As an optional solution, the reaction device also includes a monomer flow control unit 4 fixed on the kettle body 1, the monomer flow control unit 4 includes a feed pipe 41 and a flow regulating valve 42, the flow regulating valve 42 is connected to the feed pipe 41, and the feed pipe 41 is connected to the vertical section 21 for feeding fluid into the vertical section 21.
[0094] For example, the lower end of the feed pipe 41 is connected to the top of the vertical section 21, and the feed pipe 41 is fixed to the kettle cover 12. The kettle cover 12 is provided with a circular hole at a position corresponding to the feed pipe 41. The raw materials in the feed pipe 41 directly enter the vertical section 21.
[0095] The feed pipe 41 has multiple sections, including a connecting section, an intermediate section, and an external section in this embodiment. These sections are arranged sequentially. The connecting section is fixedly connected to the kettle cover 12 and directly communicates with the vertical section 21. The external section connects the feed pipe 41 to an external device that supplies raw materials. The intermediate section is located between the connecting section and the external section.
[0096] One end of the flow control valve 42 is connected to the external section, and the other end is connected to the middle section. In this embodiment, the flow control valve 42 is a manual knob-type regulating valve. When in use, turning the knob clockwise decreases the monomer flow rate, while turning the knob counterclockwise increases the monomer flow rate.
[0097] Reference Figure 4 As an optional solution, a transparent member 43 is provided on the feed pipe 41 , and the transparent member 43 is provided between the flow regulating valve 42 and the kettle body 1 .
[0098] Exemplarily, the transparent member 43 is pressure-resistant glass, a square hole is provided on the feed pipe 41 , and the transparent member 43 is embedded and fixed in the square hole. The flow of the material in the feed pipe 41 can be observed through the transparent member 43 .
[0099] Furthermore, the area of the transparent member 43 accounts for 1 / 6 of the area of the middle section of the feeding pipe 41 .
[0100] The provision of the transparent member 43 allows for intuitive observation of the flow rate of the raw materials, and facilitates intuitive observation of the flow rate of the raw materials when adjusting the flow rate of the raw materials, which helps to improve the controllability and repeatability of the reaction.
[0101] Reference Figure 1 As an optional solution, it also includes a pipeline interface 5, an auxiliary liquid inlet unit 6 and an emptying pipeline 7. The pipeline interface 5 is used to inject protective gas into the kettle body 1 or vacuum the kettle body 1. The auxiliary liquid inlet unit 6 is used to inject solvent and / or catalyst into the kettle body 1. The emptying pipeline 7 is used for the gas in the kettle body 1 to flow out.
[0102] Specifically, the pipeline interface 5 is used to inject protective gas into the kettle body 1 or to evacuate the kettle body 1. The protective gas in this embodiment is nitrogen. In this embodiment, the auxiliary liquid inlet unit 6 is only provided with one interface on the kettle body 1 for injecting solvent and catalyst into the kettle body 1.
[0103] In another embodiment, the auxiliary liquid inlet unit 6 is provided with only two interfaces on the kettle body 1 , and the two interfaces are used for injecting the solvent and the catalyst respectively in a one-to-one correspondence.
[0104] The exhaust pipe 7 is connected to the kettle body 1. When it is necessary to inject protective gas into the kettle body 1, the pipe interface 5 and the exhaust pipe 7 are opened at the same time. After nitrogen enters the kettle body 1 from the pipe interface 5, the air in the kettle body 1 is discharged from the exhaust pipe 7.
[0105] It should be noted that the pipeline interface 5, the auxiliary liquid inlet unit 6 and the emptying pipeline 7 are all provided with separate valves to control their opening and closing.
[0106] Reference Figure 5 As an optional solution, the auxiliary liquid inlet unit 6 includes a three-way valve 61, a first pipe 62 and a rubber gasket 63. One end of the three-way valve 61 is connected to the kettle body 1, and the other end is connected to the first pipe 62; the rubber gasket 63 closes the first pipe 62.
[0107] Specifically, the three-way valve 61 in this embodiment represents a component with three interfaces, which are interconnected. Each interface is provided with a valve to control opening and closing. One interface is connected to the kettle cover 12, one interface is connected to the solvent tank, and the other interface is used for catalyst injection.
[0108] The first tube 62 is connected to one of the ports of the three-way valve 61. The rubber gasket 63 seals the first tube 62. In this embodiment, the rubber gasket 63 is pressed against the end of the first tube 62 away from the three-way valve 61. In another embodiment, the rubber gasket 63 can be bonded and fixed in the first tube 62. Figure 5 It is marked with diagonal squares.
[0109] The rubber gasket 63 can withstand about 30 needle punctures and ensure the isolation effect from the external air. The rubber gasket can be replaced in time according to the wear and tear.
[0110] During use, the catalyst is removed through the Luer lock injector, and the needle penetrates the rubber gasket 63 to complete the catalyst injection.
[0111] Before use, evacuate the kettle body 1 to a slight negative pressure, inject 40-60% solvent into the kettle body 1, use a Luer lock injector to extract the catalyst, insert the needle into the sealing gasket, inject the catalyst into the kettle body 1, remove the needle, and inject the remaining solvent into the kettle body 1.
[0112] The three-way valves 61 of the auxiliary liquid inlet unit 6 are all controlled by valves to open and close, as a safeguard against external interference. This ensures that the system is completely free of external water and oxygen. When adding materials, first open the valves at the solvent and reactor ends and add some solvent. Then, close the solvent valve and insert a syringe containing the catalyst into the side rubber gasket 63. Open the side valve and inject the catalyst. Then, close the side valve and remove the syringe. Open the solvent valve and add the remaining solvent. Finally, close all valves. This sequence of operations reduces catalyst loss within the pipeline and ensures tightness throughout the entire process.
[0113] This process can avoid the introduction of external water and oxygen during catalyst injection, ensuring safety and reducing losses. The residual catalyst in the tube is flushed clean by injecting the solvent in sections, reducing operational errors.
[0114] Reference Figure 6 As an optional solution, an external thread is provided on the outer side of one end of the first tube 62 away from the three-way valve 61 , and a rubber gasket 63 is provided on the end of the first tube 62 away from the three-way valve 61 .
[0115] The auxiliary liquid inlet unit 6 further includes a pressure cover 64 , which includes a connecting portion and a pressing portion.
[0116] The connecting part is a ring with an internal thread on the inside, and the connecting part is threadedly connected to the first tube 62; the clamping part is fixed at one end of the connecting part, and the inner diameter of the clamping part is smaller than the inner diameter of the connecting part. The clamping part presses the rubber gasket 63 against the end of the first tube 62.
[0117] Specifically, an outer side of one end of the first tube 62 away from the three-way valve 61 is provided with an external thread, and the connecting portion is a ring with an internal thread provided on the inner side, and the connecting portion is threadedly connected to the first tube 62 .
[0118] The rubber gasket 63 is provided at one end of the first tube 62 away from the three-way valve 61 . When the connecting portion is threadedly connected to the first tube 62 , the pressing portion presses the rubber gasket 63 against the end of the first tube 62 .
[0119] After the rubber gasket 63 is inserted multiple times, it needs to be replaced. The pressure cap 64 is used to fix the rubber gasket 63 on the first tube 62 to facilitate replacement of the rubber gasket 63.
[0120] Reference Figure 6 As an optional solution, the auxiliary liquid inlet unit 6 further includes a sealing cover 65, which is buckled onto the pressing portion.
[0121] The outer side of the pressure cap 64 is provided with an external thread, and the sealing cap 65 is a metal cap with an internal thread. The sealing cap 65 is threadedly connected to the pressure cap 64, thereby sealing the rubber gasket 63 and isolating it from the external air.
[0122] The sealing cover 65 can prevent the rubber gasket 63 from being exposed to the air for a long time, thereby extending the service life.
[0123] When in use, the cover 65 is opened and the catalyst is injected through a syringe. After use, the cover 65 is tightened to isolate the external environment. If the sealing performance of the rubber gasket 63 is insufficient, the pressure cap 64 can be removed and the rubber gasket 63 can be replaced.
[0124] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the above embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the above embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not deviate from the essence of the corresponding technical solutions within the scope of the technical solutions of the embodiments of this application, and they should all be included in the scope of the claims and description of this application. In particular, as long as there is no structural conflict, the various technical features mentioned in the various embodiments can be combined in any manner.
[0125] The present application is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.
Claims
1. A reaction device, characterized in that: It comprises a kettle body (1) and a liquid inlet pipe (2); wherein, The liquid inlet pipe (2) comprises a vertical section (21) and a horizontal section (22); The vertical section (21) has a top end for material to enter, and a bottom end communicating with the horizontal section (22); The horizontal section (22) is provided with a plurality of discharge ports (221), and the plurality of discharge ports (221) are spaced apart along the length direction of the horizontal section (22).
2. The reaction device according to claim 1, characterized in that It also includes a stirring shaft (3), which is vertically arranged in the kettle body (1); The horizontal section (22) is in the shape of a ring arranged around the stirring shaft (3).
3. The reaction device according to claim 2, characterized in that The radius of the horizontal section (22) is r1, and the radius of the stirring shaft (3) is r2, wherein 1.5*r2≤r1≤2*r2.
4. The reaction device according to claim 2, characterized in that The stirring shaft (3) includes a main shaft (31) and a plurality of stirring paddles (32); wherein, The main shaft (31) is arranged vertically, and the stirring paddle (32) is fixed at a first position or a second position of the main shaft (31), and the first position and the second position are arranged vertically at intervals.
5. The reaction device according to claim 4, characterized in that The stirring paddle (32) includes a ring member (321), a plurality of blades (322) and a locking bolt (323); wherein, The blade (322) is fixed on the outside of the annular member (321); The annular member (321) is sleeved on the main shaft (31); a connecting screw hole is provided on the annular member (321), and the connecting screw hole penetrates the annular member (321) in a radial direction; The locking bolt (323) is connected to the annular member (321) via a connecting screw hole, and the stirring paddle (32) is fixed on the main shaft (31) when the locking bolt (323) is pressed against the main shaft (31).
6. The reaction device according to claim 1, characterized in that A cover plate (23) for closing the horizontal section (22) is provided at one end of the horizontal section (22) away from the vertical section (21); A first notch (24) is provided on the cover plate (23), and the first notch (24) communicates the inner cavity of the horizontal section (22) with the inner cavity of the kettle body (1).
7. The reaction device according to claim 1, characterized in that It also includes a monomer flow control unit (4) fixed on the kettle body (1), and the monomer flow control unit (4) includes a feed pipe (41) and a flow regulating valve (42); wherein, The flow regulating valve (42) is in communication with the feed pipe (41); The feed pipe (41) is in communication with the vertical section (21) for feeding fluid into the vertical section (21).
8. The reaction device according to any one of claims 1 to 7, characterized in that: It also includes a pipeline interface (5), an auxiliary liquid inlet unit (6) and an emptying pipeline (7); wherein, The pipeline interface (5) is used to inject protective gas into the kettle body (1) or to evacuate the kettle body (1), the auxiliary liquid inlet unit (6) is used to inject solvent and / or catalyst into the kettle body (1), and the exhaust pipeline (7) is used to allow the gas in the kettle body (1) to flow out.
9. The reaction device according to claim 8, characterized in that The auxiliary liquid inlet unit (6) comprises a three-way valve (61), a first tube (62) and a rubber gasket (63); wherein, One end of the three-way valve (61) is in communication with the kettle (1), and the other end is in communication with the first pipe (62); The rubber gasket (63) closes the first tube (62).
10. The reaction device according to claim 9, characterized in that An external thread is provided on the outer side of one end of the first tube (62) away from the three-way valve (61), and the rubber gasket (63) is provided on the end of the first tube (62) away from the three-way valve (61); The auxiliary liquid inlet unit (6) further includes a pressure cover (64), and the pressure cover (64) includes a connecting portion and a pressing portion; The connecting portion is a ring-shaped member with an internal thread on the inner side, and the connecting portion is threadedly connected to the first tube (62); The pressing portion is fixed to one end of the connecting portion, the inner diameter of the pressing portion is smaller than the inner diameter of the connecting portion, and the pressing portion presses the rubber gasket (63) onto the end of the first tube (62).