A polyphenylene sulfide preparation reaction kettle and process

By combining a temperature control structure consisting of a hollow shaft and a U-shaped tube with a mixing pusher, the problem of slow temperature rise of materials in the middle of the reactor was solved, achieving rapid and uniform heating and efficient stirring, thereby improving reaction efficiency and production capacity.

CN120939873BActive Publication Date: 2025-12-05JIANGSU OURUIDA NEW MATERIAL SCI&TECH CO LTD
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Patent Information

Application Number
CN202511476179.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-10-16
Publication Date
2025-12-05
Estimated Expiration
2045-10-16

AI Technical Summary

Technical Problem

The temperature of the material in the middle of the existing reactor rises slowly, which leads to prolonged heating time, uneven reaction, and affects production capacity and product purity.

Method used

The temperature control structure, consisting of a hollow shaft and a U-shaped tube, combined with a water distribution sleeve, enables multi-directional heat transfer. Through the cooperation of the mixing pusher and the external mixer, efficient stirring is achieved, breaking the fixed circulation state of the material.

Benefits of technology

It shortens the heat transfer path, improves material reaction efficiency and mixing uniformity, reduces energy consumption, and extends the equipment's applicability and production stability.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application relates to the technical field of reaction preparation, and discloses a reaction kettle for preparing polyphenylene sulfide and a process, wherein the reaction kettle for preparing polyphenylene sulfide comprises a reactor, a water distribution sleeve fixedly connected to the top end of the reactor, and a motor fixedly connected to the top end of a hollow shaft; the inside of the reactor is temperature-controlled through the hollow shaft and a U-shaped tube; when the hollow shaft rotates, the mixed pushing piece drives the outer mixer to rotate intermittently through centrifugal force and in cooperation with upper and lower arc blocks. The internal temperature-control structure formed by the hollow shaft and the U-shaped tube, in cooperation with the water distribution sleeve, can directly deliver the temperature-control medium to each region in the inside of the reactor without being affected by the rotation of the hollow shaft, realizes multidirectional heat transfer from the inside of the material to the outside or from the outside to the inside, instead of the traditional one-way diffusion from the kettle wall, shortens the heating time, improves the material reaction efficiency, and further shortens the whole reaction period, and improves the production capacity of the equipment per unit time.
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Description

Technical Field

[0001] This invention relates to the technical field of preparation reactions, and more particularly to a reaction vessel and process for preparing polyphenylene sulfide. Background Technology

[0002] The reaction vessel for the preparation of polyphenylene sulfide (PPS) needs to withstand the high reaction temperature and pressure during the preparation process. It should be able to achieve heating and cooling through external heat source injection, and be equipped with a suitable stirring system to alleviate the problem of uneven heating of materials, so as to provide a closed reaction environment that meets the process requirements for the generation of PPS resin.

[0003] However, in existing technologies, the heat source of the reactor is supplied only through an external or internal heat medium. Heat diffuses unidirectionally from the reactor wall to the material inside. This results in rapid heat transfer to materials near the reactor wall, allowing them to absorb heat instantly and causing a rapid temperature rise. However, materials in the middle of the reactor require secondary heat transfer through the edge materials to acquire heat. This not only results in a longer transfer path but also heat loss due to the material's own thermal resistance, leading to a slower temperature rise in the middle. While a stirrer can circulate the material, allowing materials in the middle to move sequentially or randomly to the edge areas for heating, this directly increases the time required. In each cycle, only a portion of the material reaches the edge areas and comes into contact with the efficient heat source, while the rest remains in the low-temperature middle zone. Furthermore, as the reactor volume increases and the material viscosity rises, the circulation efficiency further decreases, and the extension of heating time also increases. This extended heating time directly leads to a decrease in the material's reaction efficiency, resulting in a corresponding increase in the overall reaction cycle and a reduction in the equipment's capacity per unit time. As a result, the temperature difference decreases. On the other hand, the continuous existence of temperature difference will cause significant differences in the reaction process. The material in the edge area will enter the reaction stage first because the temperature reaches the target earlier, while the material in the middle will remain in the unreacted state because the temperature has not reached the required reaction temperature. This creates an asynchronous situation where some materials have reacted and some have not, which in turn reduces the purity of the target product. Therefore, the stirring effect is improved by increasing the number of stirring blades. Increasing the number of blades will directly increase the rotational resistance of the material to the stirring shaft. The contact area between the blades and the material increases with the increase in the number of blades, but the motor needs to output more power to maintain the set speed. This will not only lead to increased energy consumption, but also significantly increase the torque on the stirring bearing. Long-term operation will easily cause shaft wear, leading to equipment overload. In addition, too many blades will cause the material mixing to fall into an overly stable rotational state. The circulation path formed by the blade rotation is relatively fixed. The material can only circulate within the preset trajectory and cannot form local turbulence. Instead, it will lead to insufficient mixing of the material and failure to fully exchange heat and components with the material in other areas. Summary of the Invention

[0004] The purpose of this invention is to provide a reaction vessel and process for preparing polyphenylene sulfide, which solves the problem of slow temperature rise of materials in the middle of the vessel.

[0005] This invention proposes a reaction vessel for preparing polyphenylene sulfide (PPS), comprising a reactor, a water-distributing sleeve fixedly connected to the top of the reactor, a hollow shaft rotatably connected inside the reactor, a motor fixedly connected to the top of the hollow shaft, multiple U-shaped tubes vertically and equidistantly arranged and all fixedly connected to the outside of the hollow shaft, two collars fixedly connected inside the reactor, two mixing pushers connected to the hollow shaft, an external mixer rotatably connected between the two collars, two pressure-bearing components respectively connected to the corresponding mixing pushers, and an upper arc block and a lower arc block fixedly connected to the collars. The output end of the motor is fixedly connected to the hollow shaft. A vertical row of U-shaped tubes forms a module, with two modules symmetrical about the central axis of the hollow shaft. The multiple U-shaped tubes are interconnected with the interior of the hollow shaft, and the top of the hollow shaft is interconnected with the interior of the water-distributing sleeve. The temperature inside the reactor is controlled by the hollow shaft and the U-shaped tubes. When the hollow shaft rotates, the mixing pushers, through centrifugal force and in conjunction with the upper and lower arc blocks, intermittently drive the external mixer to rotate.

[0006] Furthermore, the interior of the water distribution sleeve is divided into a lower storage area and an upper storage area. The lower storage area is not interconnected with the upper storage area. The water distribution sleeve is equipped with an inlet pipe and an outlet pipe. The inlet pipe is interconnected with the lower storage area, and the outlet pipe is interconnected with the upper storage area.

[0007] Furthermore, the top of the hollow shaft is provided with an inlet and an outlet. The inlet is located inside the lower storage area, and the outlet is located inside the upper storage area. Multiple water distribution pipes are provided outside the hollow shaft. The number of water distribution pipes is twice that of the U-shaped pipes. Both ends of the multiple U-shaped pipes are connected to two water distribution pipes to form a loop.

[0008] Furthermore, a partition vertical plate is fixedly connected inside the hollow shaft, dividing the interior of the hollow shaft into an inlet area and an outlet area. The bottom ends of the inlet area and the outlet area are interconnected, the inlet is interconnected with the top end of the inlet area, and the outlet is interconnected with the top end of the outlet area. Multiple cross-sectional arc plates are provided on the outside of the partition vertical plate, the number of which is equal to the number of U-shaped tubes. The cross-sectional arc plates are used for guiding flow. Multiple support rods are provided on the outside of the hollow shaft, and the mixing pusher is connected to the outside of the support rods.

[0009] Furthermore, both of the aforementioned mixing pushers and pressure-bearing components are symmetrical about the central axis of the hollow shaft. The mixing pushers and the U-shaped tube are staggered in position. The pressure-bearing component is divided into an upper pressure-bearing component and a lower pressure-bearing component. The upper pressure-bearing component is connected to the top of the corresponding mixing pusher, and the lower pressure-bearing component is connected to the bottom of the corresponding mixing pusher.

[0010] Furthermore, the hybrid pusher includes a sleeve rod slidably connected between two support rods, a vertical push plate fixedly connected to one side of the sleeve rod, and a spring connected between the sleeve rod and the support rod.

[0011] Furthermore, the pressure-bearing component includes a straight rod fixedly connected to the sleeve rod at one end, and a rotating wheel rotatably connected to the other end of the straight rod. The rotating wheel is tangent to the side of the vertical push plate away from the sleeve rod. The top surface of the upper straight rod is at the same height as the top surface of the upper arc block, and the bottom surface of the lower straight rod is at the same height as the bottom surface of the lower arc block.

[0012] Furthermore, an arc-shaped protrusion is fixedly connected to the external mixer. The side of the arc-shaped protrusion near the hollow shaft is tangent to the end of the pressure-bearing component away from the hollow shaft, and the vertical push plate only contacts the arc-shaped protrusion.

[0013] Furthermore, the two collars are divided into an upper collar and a lower collar. The upper arc block is fixedly connected to the upper collar, and the lower arc block is fixedly connected to the lower collar. The upper arc block and the lower arc block have the same shape, and their positions are symmetrical about the central axis of the collar.

[0014] Another aspect of the present invention provides: a reaction process for preparing polyphenylene sulfide, employing a reaction vessel for preparing polyphenylene sulfide, comprising the following steps:

[0015] Step 1: Pre-treat the raw materials by feeding them into the reactor through the inlet, along with solvent. After feeding, close the inlet to seal the reactor and prevent subsequent material leakage or impurities from entering.

[0016] Step 2: By introducing a high-temperature heat source into the outer tube and hollow shaft of the reactor, the temperature inside the reactor is gradually raised to the preset value, while controlling the internal pressure of the reactor.

[0017] Step 3: Start the motor to drive the hollow shaft to rotate, agitate the material, and ensure that the material reacts fully to alleviate uneven heating.

[0018] Step 4: The reaction is terminated upon completion. Heating is stopped, and cooling water is injected into the outer tube and the interior of the hollow shaft of the reactor to cool them down. Once the temperature and pressure are stable, the outlet is opened to discharge the polyphenylene sulfide-containing material, which is then sent to the subsequent separation and purification process to complete a single reaction.

[0019] The beneficial effects of this invention are:

[0020] The internal temperature control structure, composed of a hollow shaft and a U-shaped tube, along with a water distribution sleeve, allows the temperature control medium to be directly delivered to various areas inside the reactor, unaffected by the rotation of the hollow shaft. This enables multi-directional heat transfer from the inside of the material to the outside or from the outside to the inside, rather than the traditional unidirectional diffusion from the reactor wall. This shortens the heat transfer path, reduces heat loss, and allows materials in different areas of the reactor to quickly and uniformly reach the set temperature. This shortens the heating time, improves the material reaction efficiency, and consequently shortens the entire reaction cycle, increasing the equipment's capacity per unit time.

[0021] Efficient mixing is achieved through the cooperation of the mixing pusher, the pressure-bearing component, and the external mixer, eliminating the need for a large number of mixing blades. This significantly reduces the rotational resistance of the hollow shaft 3, decreases the motor's output power requirements, and lowers equipment energy consumption. It also reduces the torque on the hollow bearing, preventing shaft wear caused by long-term operation and reducing equipment load. Furthermore, the intermittent disturbance method breaks the excessively stable state of material circulating only within a fixed circulation path during mixing, creating a disturbed flow trajectory for the material inside the reactor. This allows the material in the central area to contact the material in the edge area and near the U-shaped tube more quickly and frequently, as well as the outer wall of the reactor, fully absorbing the heat transferred by the temperature control medium. It also promotes component exchange between materials in different areas, effectively improving the uniformity of material mixing and the synchronicity of the reaction.

[0022] By combining the pusher, the pressure-bearing component, and the upper and lower arc blocks, the external mixer achieves stable intermittent rotation, reducing energy consumption during operation and meeting energy-saving and environmentally friendly production requirements. This lowers production costs for enterprises. Even with increased vessel volume and higher material viscosity, the extensive distribution of U-shaped tubes and the efficient agitation of the external mixer ensure good temperature control and mixing effects. This avoids the problems of reduced circulation efficiency and extended heating time caused by increased vessel volume and material viscosity in existing technologies, thus improving the applicability and production stability of the equipment. Attached Figure Description

[0023] Figure 1 This is a three-dimensional structural diagram of the reactor from a first-person perspective.

[0024] Figure 2 This is a schematic diagram of the internal structure of the reactor;

[0025] Figure 3 This is a top view of the water distribution sleeve of the reactor.

[0026] Figure 4 For the reaction vessel Figure 3 Sectional view at point BB;

[0027] Figure 5 This is a schematic diagram of the mixing pusher in the reactor.

[0028] Figure 6 This is a schematic diagram of the structure of the external mixer of the reactor;

[0029] Figure 7 For the reaction vessel Figure 2 Enlarged view of point A in the middle;

[0030] Figure 8 For the reaction vessel Figure 4 Enlarged diagram of point C in the middle.

[0031] In the picture:

[0032] 1. Reactor; 2. Water distribution sleeve; 21. Lower storage area; 22. Upper storage area; 201. Inlet pipe; 202. Outlet pipe; 3. Hollow shaft; 31. Separating vertical plate; 32. Cross-sectional arc plate; 33. Support rod; 301. Inlet; 302. Outlet; 303. Water distribution pipe; 311. Inlet area; 312. Outlet area; 4. Motor; 5. U-shaped tube; 6. Collar; 7. Mixing pusher; 71. Sleeve rod; 72. Vertical push plate; 73. Spring; 8. External mixer; 81. Arc-shaped protruding rod; 9. Pressure-bearing component; 91. Straight rod; 92. Rotary wheel; 10. Upper arc block; 11. Lower arc block. Detailed Implementation

[0033] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.

[0034] Example 1, refer to Figures 1-8 This first embodiment of the invention provides a reaction vessel for preparing polyphenylene sulfide, including a reactor 1, a water-distributing sleeve 2 fixedly connected to the top of the reactor 1, a hollow shaft 3 rotatably connected inside the reactor 1, a motor 4 fixedly connected to the top of the hollow shaft 3, multiple U-shaped tubes 5 vertically and equidistantly arranged and fixedly connected to the outside of the hollow shaft 3, two collars 6 fixedly connected inside the reactor 1, two mixing pushers 7 connected to the hollow shaft 3, an external mixer 8 rotatably connected between the two collars 6, and two mixers respectively connected to the corresponding mixing pushers. The pusher 7 is connected to the pressure-bearing component 9, and the upper arc block 10 and lower arc block 11 are fixedly connected to the collar 6. The output end of the motor 4 is fixedly connected to the hollow shaft 3. A vertical row of U-shaped tubes 5 is a module. There are two modules and they are symmetrical about the central axis of the hollow shaft 3. Multiple U-shaped tubes 5 are interconnected with the interior of the hollow shaft 3. The top of the hollow shaft 3 is interconnected with the interior of the water distribution sleeve 2. The temperature inside the reactor 1 is controlled by the hollow shaft 3 and the U-shaped tubes 5. When the hollow shaft 3 rotates, the mixing pusher 7 drives the external mixer 8 to rotate intermittently by centrifugal force and in cooperation with the upper arc block 10 and lower arc block 11.

[0035] Specifically, the temperature control medium is high-temperature heat transfer oil during heating and low-temperature coolant during cooling, collectively referred to as water, though other media can also be used. The temperature control medium flowing within the U-shaped tube 5 exchanges heat with the material inside the reactor 1 through the tube wall of the U-shaped tube 5. When heating is required, the water releases heat, which is transferred to the surrounding material through the tube wall of the U-shaped tube 5. Because the U-shaped tubes 5 are widely distributed inside the reactor 1 and have a large contact area with the material, and because the U-shaped tubes 5 rotate with the hollow shaft 3, heat can be quickly and evenly transferred to the material in all areas inside the reactor 1, effectively shortening the heat transfer path and reducing heat loss during the transfer process. When cooling is required, the low-temperature coolant absorbs heat from the material and, similarly, is transferred through the U-shaped tubes 5 and the hollow shaft 3, ultimately being discharged from the water distribution sleeve 2, achieving rapid cooling of the material inside the reactor 1 and meeting the temperature control requirements at different stages of the reaction process.

[0036] In addition, no components are installed on the outside of the U-tube 5. Initially, a mixing plate was installed on the outside of the U-tube 5, but this affected the heat distribution effect of the U-tube 5. Therefore, it is not necessary to install other components on the outside of the U-tube 5 to ensure the heat distribution of the U-tube 5.

[0037] Reference Figures 2-4 The interior of the water distribution sleeve 2 is divided into a lower storage area 21 and an upper storage area 22. The lower storage area 21 is not connected to the upper storage area 22. The water distribution sleeve 2 is equipped with an inlet pipe 201 and an outlet pipe 202. The inlet pipe 201 is connected to the lower storage area 21, and the outlet pipe 202 is connected to the upper storage area 22. The top of the hollow shaft 3 is located inside the water distribution sleeve 2. The water injection equipment connected to the outside of the inlet pipe 201 and the outlet pipe 202 needs to ensure sufficient pressure.

[0038] The hollow shaft 3 has an inlet 301 and an outlet 302 at its top. The inlet 301 is located inside the lower storage area 21, and the outlet 302 is located inside the upper storage area 22. Multiple water distribution pipes 303 are provided on the outside of the hollow shaft 3. The number of water distribution pipes 303 is twice that of the U-shaped pipes 5. Both ends of the multiple U-shaped pipes 5 are connected to two water distribution pipes 303 to form a loop. The water entering from the hollow shaft 3 passes through the water distribution pipes 303 and enters the U-shaped pipe 5. Then, it enters a vertical section of the U-shaped pipe 5 through the water distribution pipe 303 at one end of the U-shaped pipe 5. It then flows downward along the pipe section. After passing through the curved part at the bottom of the U-shaped pipe 5, it flows upward to the vertical section at the other end of the U-shaped pipe 5. Finally, it flows back to the internal cavity of the hollow shaft 3 through the water distribution pipe 303 at that end.

[0039] Specifically, after water enters through the inlet pipe 201, the water enters the lower storage area 21. The inlet 301 is located inside the lower storage area 21, allowing the water to enter the interior of the hollow shaft 3 through the inlet 301. The water entering the hollow shaft 3 will then enter the interior of the U-shaped pipe 5 through the distribution pipe 303, and flow using the loop formed by the U-shaped pipe 5.

[0040] Among them, the U-shaped pipe 5 is U-shaped and has no holes on its surface. Therefore, the two ends of a single U-shaped pipe 5 refer to the ports of two vertical pipe sections, which are connected by the bend at the bottom. At the same time, one end of each water distribution pipe 303 is connected to the internal cavity of the hollow shaft 3. The connection is sealed by welding to prevent the medium from leaking at the connection. Furthermore, the ports of the water distribution pipe 303 and the U-shaped pipe 5 are connected by threads or flanges, and the connection is equipped with a high-temperature resistant sealing gasket to further enhance the sealing performance and prevent the medium from leaking under high temperature and high pressure.

[0041] Reference Figures 2-8 The hollow shaft 3 is fixedly connected to a partition vertical plate 31, which divides the interior of the hollow shaft 3 into an inlet area 311 and an outlet area 312. The bottom ends of the inlet area 311 and the outlet area 312 are interconnected, the inlet 301 is interconnected with the top end of the inlet area 311, and the outlet 302 is interconnected with the top end of the outlet area 312. Multiple cross-sectional arc plates 32 are provided on the outside of the partition vertical plate 31. The number of cross-sectional arc plates 32 is equal to that of the U-shaped tube 5. The cross-sectional arc plates 32 are used for flow guidance to ensure that the medium does not have insufficient flow or too short residence time in the tube when it flows in the U-shaped tube 5, thus ensuring the heat exchange effect. Multiple support rods 33 are provided on the outside of the hollow shaft 3, and the mixing pusher 7 is connected to the outside of the support rods 33.

[0042] Specifically, the central axis of the dividing vertical plate 31 coincides with the central axis of the hollow shaft 3. The U-shaped pipes 5 within the module are symmetrical about the central axis of the dividing vertical plate 31. The water distribution pipe 303 is also divided into two equal parts, one part of which communicates with the inlet area 311, and the other part communicates with the outlet area 312. Simultaneously, the cross-sectional arc plate 32 and the water distribution pipe 303 are at the same height, ensuring that water must enter the water distribution pipe 303. Since the U-shaped pipe 5 is connected to the water distribution pipe 303, water is ensured to enter the U-shaped pipe 5. The water flow process inside the hollow shaft 3 and the U-shaped pipe 5 is as follows: water reaches the interior of the lower storage area 21, allowing it to pass through the inlet 301. The inlet 301 only communicates with the inlet area 311, allowing water to enter the inlet area 311. The water enters the corresponding U-shaped pipe 5 through the water distribution pipe 303 of the inlet area 311. When the water reaches the bottom of the hollow shaft 3, the water has completely flowed through the inlet area 311 and the U-shaped pipe 5 connected to it. The bottom of the inlet area 311 and the outlet area 312 are interconnected, and the water enters the outlet area 312. Similarly, the cross-sectional arc plate 32 is used to introduce the water into the water distribution pipe 303, so that the water enters the U-shaped pipe 5 connected to the outlet area 312. Finally, the water completes the circulation and passes through the outlet 302 to the interior of the upper storage area 22, and is discharged through the outlet pipe 202 to form a circulation. When the hollow shaft 3 rotates, it can drive the U-shaped pipe 5 to rotate synchronously, while the water distribution sleeve 2 will not rotate, so it will not affect the water supply and collection pipe outside the reactor 1.

[0043] Reference Figures 2-7 Both the two mixing pushers 7 and the pressure-bearing member 9 are symmetrical about the central axis of the hollow shaft 3. The mixing pushers 7 and the U-shaped tube 5 are arranged in staggered positions. The pressure-bearing member 9 is divided into an upper pressure-bearing member 9 and a lower pressure-bearing member 9. The upper pressure-bearing member 9 is connected to the top of the corresponding mixing pusher 7, and the lower pressure-bearing member 9 is connected to the bottom of the corresponding mixing pusher 7.

[0044] Specifically, the installation position of the support rod 33 avoids the distribution area of ​​the U-shaped tube 5 and the water distribution pipe 303, so as to avoid collision or interference with the temperature control components during rotation. At the same time, the mixing pusher 7 can stably contact the upper arc block 10 and the lower arc block 11 during rotation, realizing the intermittent rotation of the external mixer 8. The temperature control system achieves uniform temperature control through the U-shaped tube 5, and the stirring system achieves efficient mixing through the mixing pusher 7 and the external mixer 8. The two do not interfere with each other and cooperate with each other to improve the overall performance of the reactor.

[0045] Reference Figures 2-7The mixing pusher 7 includes a sleeve rod 71 slidably connected between two support rods 33, a vertical push plate 72 fixedly connected to one side of the sleeve rod 71, and a spring 73 connected between the sleeve rod 71 and the support rods 33. When the hollow shaft 3 rotates, it will drive the mixing pusher 7 to rotate as a whole. Under the influence of centrifugal force, the sleeve rod 71 and the vertical push plate 72 slide along the path of the support rods 33. At the same time, the sleeve rod 71 will compress the spring 73 when it slides. When the hollow shaft 3 rotates, the vertical push plate 72 is used to mix the internal materials. When the vertical push plate 72 moves with the sleeve rod 71, it will gradually approach the outer mixer 8, thereby cooperating with the upper arc block 10 and the lower arc block 11 to intermittently drive the outer mixer 8 to rotate.

[0046] Specifically, the intermittent rotation design of the external mixer 8, combined with the internal stirring of the vertical push plate 72 and the temperature equalization effect of the rotating disturbance of the U-shaped tube 5, can break the laminar flow state of the material and form local turbulence, promoting the full mixing and heat and component exchange of the material inside the reactor 1. At the same time, the vertical push plate 72 is affected by centrifugal force, which can control the rotation speed of the hollow shaft 3 to determine whether the vertical push plate 72 drives the external mixer 8, reducing the equipment load and ensuring the uniformity of material mixing in different areas. This effectively solves the problem of reaction process differences and reduces the asynchronous situation where some materials have reacted and some materials have not reacted.

[0047] Reference Figures 1-8 The pressure-bearing component 9 includes a straight rod 91 fixedly connected to the sleeve rod 71 at one end, and a rotating wheel 92 rotatably connected to the other end of the straight rod 91. The rotating wheel 92 is tangent to the side of the vertical push plate 72 away from the sleeve rod 71. The top surface of the upper straight rod 91 is at the same height as the top surface of the upper arc block 10, and the bottom surface of the lower straight rod 91 is at the same height as the bottom surface of the lower arc block 11.

[0048] The outer mixer 8 is composed of multiple mixing plates and rings. An arc-shaped protrusion 81 is fixedly connected to the outer mixer 8. The side of the arc-shaped protrusion 81 near the hollow shaft 3 is tangent to the end of the pressure-bearing component 9 away from the hollow shaft 3. The vertical push plate 72 only contacts the arc-shaped protrusion 81. That is, after the sleeve rod 71 fully compresses the spring 73, the vertical push plate 72 will still not contact the outer mixer 8, thus avoiding collision between the vertical push plate 72 and the mixing plates of the outer mixer 8.

[0049] Specifically, the side of the vertical push plate 72 away from the sleeve rod 71 is covered with soft silicone to reduce wear and impact when the vertical push plate 72 collides with the arc-shaped protrusion rod 81. When the vertical push plate 72 approaches the external mixer 8, the vertical push plate 72 will contact the side of the arc-shaped protrusion rod 81. At this time, the vertical push plate 72 rotates with the hollow shaft 3, and then the vertical push plate 72 will synchronously drive the external mixer 8 to rotate, so that the reactor 1 is in a strong mixing state, and with the temperature uniformity effect of the U-shaped tube 5, the reactivity of the material is enhanced.

[0050] Since the straight rod 91 is fixedly connected to the sleeve rod 71, when the sleeve rod 71 moves, the straight rod 91 will also move synchronously. Therefore, when the straight rod 91 moves, the sleeve rod 71 will also move with it. As the straight rod 91 and the rotating wheel 92 gradually approach the outer mixer 8, since both the upper arc block 10 and the lower arc block 11 are fixedly connected to the collar 6, the straight rod 91 and the rotating wheel 92 also gradually approach the upper arc block 10 and the lower arc block 11. Simultaneously, the pressure member 9 is divided into an upper pressure member 9 and a lower pressure member 9. Therefore, the upper pressure member 9 will only contact the upper arc block 10, and the lower pressure member 9 will only contact the lower arc block 11. At this time, if the vertical push plate 72 is in contact with the arc-shaped protrusion 81, when the straight rod 91 and the rotating wheel 92 rotate with the sleeve rod 71, the upper rotating wheel 92 will contact the upper arc block 10, and the upper rotating wheel 92 will be subjected to... When the surface path of the upper arc block 10 is sufficient and obstructed, it moves back, causing the sleeve rod 71 to move back along the path of the support rod 33. The vertical push plate 72 also moves back with the sleeve rod 71, and then the sleeve rod 71 will separate from the arc-shaped protrusion 81. The outer mixer 8 is no longer driven. At this time, the outer mixer 8 will rotate due to inertia. The rotation speed of the outer mixer 8 and the hollow shaft 3 are different. When the upper pressure member 9 is no longer in contact with the upper arc block 10, the vertical push plate 72 will contact the arc-shaped protrusion 81 again due to centrifugal force, and then the outer mixer 8 will be driven again. The lower pressure member 9 and the lower arc block 11 cooperate in the same way. It can be understood that the sleeve rod 71 connected to the lower pressure member 9 is longer than the sleeve rod 71 connected to the upper pressure member 9 due to the installation position. However, the two have the same structure and function, and only the length is locally adjusted according to the installation requirements.

[0051] Furthermore, the upper pressure-bearing component 9 only contacts the upper arc block 10, and the lower pressure-bearing component 9 only contacts the lower arc block 11, forming independent upper and lower cooperation to ensure that the two sets of pressure-bearing components 9 will not interfere with each other. When the vertical push plate 72 is completely separated from the arc-shaped protrusion 81, the outer mixer 8 does not immediately stop rotating, but continues to rotate around the collar 6 under the action of inertia. Since the inertial speed of the outer mixer 8 is different from the rotational speed of the hollow shaft 3, a speed difference is formed between the two. This speed difference further breaks the stable circulation state of the material, causing the material in the reactor 1 to... The internal turbulence is more complex, continuously improving the mixing effect. When the sleeve rod 71 moves back to the initial position, as the hollow shaft 3 continues to rotate, the sleeve rod 71 slides away from the hollow shaft 3 again under the action of centrifugal force, repeating the cycle of contact drive, guide return and inertial rotation. The cooperation process between the lower pressure member 9 and the lower arc block 11 is completely consistent with that of the upper pressure member 9. Through the alternation of the upper and lower pressure members 9, the external mixer 8 can continuously obtain intermittent driving force to achieve a high-efficiency and stable mixing effect.

[0052] Reference Figures 1-8The two collars 6 are divided into an upper collar 6 and a lower collar 6, with the outer mixer 8 located between them. The upper arc block 10 is fixedly connected to the upper collar 6, and the lower arc block 11 is fixedly connected to the lower collar 6. The upper arc block 10 and the lower arc block 11 have the same shape, and their positions are symmetrical about the central axis of the collar 6.

[0053] Specifically, due to the influence of inertia, the position of the external mixer 8 will be random. If only the arc-shaped protrusion 81 of the external mixer 8 coincides with the upper arc block 10, the sleeve 71 connected to the upper pressure member 9 will always be affected by the upper arc block 10, causing the vertical push plate 72 to be unable to contact the arc-shaped protrusion 81. At this time, the sleeve 71 connected to the lower pressure member 9 can be used. Since it is only restricted by the lower arc block 11, the vertical push plate 72 can push the arc-shaped protrusion 81 to make the external mixer 8 rotate and complete the external mixing work. If the arc-shaped protrusion 81 coincides with the lower arc block 11, the opposite is true.

[0054] The working principle of this invention is as follows: Motor 4 starts, and its output drives the hollow shaft 3 to rotate. The hollow shaft 3 synchronously drives the external U-shaped tube 5 to rotate. The temperature control medium is injected through the inlet pipe 201 on the water distribution sleeve 2, flowing directly into the lower storage area 21 inside the water distribution sleeve 2. As the inlet pipe 201 continuously supplies water, the water level in the lower storage area 21 gradually rises until it submerges the inlet 301 at the top of the hollow shaft 3. Under water pressure, the water in the lower storage area 21 enters the water inlet area 311 inside the hollow shaft 3 through the inlet 301. Because the internal partition plate 31 of the hollow shaft 3 divides it into the water inlet area 311 and the water outlet area 312, and the inlet 301 only communicates with the water inlet area 311, the water can only enter the water inlet area 311 first, and then pass through the water inlet area 311 and the transverse arc... Under the guiding action of plate 32, the water flows into the U-shaped pipe 5 through the corresponding water distribution pipe 303. After one end of a single U-shaped pipe 5 is connected to the water body through the water distribution pipe 303, the water body flows downward along a vertical section of the U-shaped pipe 5. After passing through the bottom bend section, it flows upward to the vertical section at the other end of the U-shaped pipe 5. The water body flowing through the U-shaped pipe 5 flows back to the water inlet area 311 of the hollow shaft 3 through the water distribution pipe 303 at the other end, and continues to flow downward to the bottom end of the hollow shaft 3. Since the bottom end of the water inlet area 311 and the water outlet area 312 are interconnected, the water body enters the water outlet area 312. At this time, the water body flows upward and flows back into the U-shaped pipe 5 through the water distribution pipe 303 corresponding to the water outlet area 312. At the same time, the stirring action of the external mixer 8 can accelerate the contact between the material and the pipe wall of the U-shaped pipe 5, improve the heat exchange efficiency, and complete the process. After the secondary heat exchange, the water flows back to the outlet area 312 along the water distribution pipe 303, then flows upward along the outlet area 312, flows into the upper storage area 22 of the water distribution sleeve 2 through the outlet 302, and is discharged through the outlet pipe 202, completing the entire cycle. During the rotation of the U-shaped pipe 5, the temperature is controlled by heat exchange between the pipe wall and the material in the reactor 1. The support rod 33 drives the mixing pusher 7 to rotate synchronously. The sleeve rod 71 is sleeved on the support rod 33. When the support rod 33 rotates, under the action of centrifugal force, the sleeve rod 71 drives the vertical push plate 72 to slide away from the hollow shaft 3 along the support rod 33, while compressing the spring 73 between the sleeve rod 71 and the support rod 33. During the rotation of the vertical push plate 72, the material in the reactor 1 is initially stirred and pushed. In addition, the sleeve rod 71... During sliding, the straight rod 91 of the pressure-bearing component 9 moves synchronously. The rotating wheel 92 at the other end of the straight rod 91 gradually approaches the outer mixer 8. When the vertical push plate 72 contacts the arc-shaped protrusion 81 of the outer mixer 8, the vertical push plate 72 rotates with the hollow shaft 3, driving the outer mixer 8 to rotate around the collar 6 through the arc-shaped protrusion 81, achieving strong stirring. After the corresponding rotating wheel 92 contacts the upper arc block 10 or the lower arc block 11, it is blocked by its fixed structure, generating a return force in the direction of the hollow shaft 3. This force pushes the collar 71 back along the support rod 33 through the straight rod 91, the spring 73 resets, the vertical push plate 72 separates from the arc-shaped protrusion 81, and the outer mixer 8 loses its driving force. After losing its driving force, the outer mixer 8 continues to rotate around the collar 6 due to inertia, and forms a speed difference with the hollow shaft 3, continuously stirring the material.As the hollow shaft 3 continues to rotate, the sleeve 71 slides again under centrifugal force, repeating the cycle. Simultaneously, the water continues to circulate in the temperature control loop, ensuring continuous operation of the equipment.

[0055] Example 2, refer to Figures 1-8 The second embodiment of the present invention provides a reaction process for preparing polyphenylene sulfide, which uses a reaction vessel for preparing polyphenylene sulfide and includes the following steps:

[0056] Step 1: Pre-treat the raw materials to remove moisture and impurities to avoid affecting reaction efficiency and product purity. Feed the raw materials into reactor 1 through the feed inlet, and add solvent at the same time. After feeding, close the feed inlet and seal reactor 1 to prevent subsequent material leakage or impurities from entering.

[0057] Step 2: By introducing a high-temperature heat source into the outer tube of reactor 1 and the interior of the hollow shaft 3, the temperature inside the reactor is gradually raised to the preset value. The increase in temperature will cause pressure to be generated inside the reactor due to solvent evaporation and gas production from the reaction. To control the internal pressure of reactor 1, it is necessary to monitor and adjust it in real time through the pressure control system to stabilize the pressure and create a suitable temperature and pressure environment for the polymerization reaction.

[0058] Step 3: Start motor 4 to drive hollow shaft 3 to rotate, stir the material, make the material react fully, alleviate uneven heating, and at the same time use online detection devices such as sampling port and temperature sensor to monitor the reaction progress, fine adjust temperature, pressure and stirring parameters to ensure that the polymerization reaction successfully produces polyphenylene sulfide.

[0059] Step 4: The reaction is terminated upon completion. Heating is stopped, and cooling water is injected into the outer tube of reactor 1 and the interior of the hollow shaft 3 to cool them down. Once the temperature and pressure stabilize, the outlet is opened, and the polyphenylene sulfide-containing material is discharged and sent to the subsequent separation and purification process, completing a single reaction. It should be noted that the above embodiments are only used to illustrate the technical solution of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the spirit and scope of the present invention, and all such modifications and substitutions should be covered within the scope of the claims of the present invention.

Claims

1. A reaction vessel for polyphenylene sulfide production, comprising a reactor (1), characterized in that: Also include fixedly connected to the top of the reactor (1) water jacket sleeve (2), rotatably connected inside the reactor (1) hollow shaft (3), fixedly connected to the top of the hollow shaft (3) motor (4), vertically equidistantly arranged multiple and all with the outside of the hollow shaft (3) fixedly connected U-shaped tube (5), provided with two and all fixedly connected inside the reactor (1) ring (6), provided with two and all with the hollow shaft (3) connected mixed push piece (7), rotatably connected between the two ring (6) external mixer (8), provided with two and respectively with the corresponding mixed push piece (7) connected pressure receiving member (9), and with the ring (6) fixedly connected upper arc block (10) and lower arc block (11), the output of the motor (4) and the hollow shaft (3) fixedly connected, a vertical row of U-shaped tube (5) is a group of modules, the module is provided with two and about the central axis of the hollow shaft (3) symmetry, a plurality of the U-shaped tube (5) are all with the inside of the hollow shaft (3) intercommunication, the top of the hollow shaft (3) and the inside of the water jacket sleeve (2) intercommunication, the hollow shaft (3) and U-shaped tube (5) are used for controlling the temperature of the inside of the reactor (1), the mixed push piece (7) is intermittently driven to rotate the external mixer (8) by centrifugal force and cooperates with the upper arc block (10) and the lower arc block (11) when the hollow shaft (3) rotates; The outside of the hollow shaft (3) is provided with a plurality of support rods (33), and the mixed push piece (7) is connected outside the support rod (33); Two of the mixed push piece (7) and the pressure receiving member (9) are symmetrical about the central axis of the hollow shaft (3), the mixed push piece (7) and the U-shaped tube (5) are staggered, the pressure receiving member (9) is divided into upper pressure receiving member (9) and lower pressure receiving member (9), the upper pressure receiving member (9) is connected to the top of the corresponding mixed push piece (7), and the lower pressure receiving member (9) is connected to the bottom of the corresponding mixed push piece (7); The mixed push piece (7) comprises a sleeve rod (71) slidably connected between two support rods (33), a vertical push plate (72) fixedly connected to one side of the sleeve rod (71), and a spring (73) connected between the sleeve rod (71) and the support rod (33); The pressure receiving member (9) comprises a straight rod (91) fixedly connected to one end of the sleeve rod (71), and a rotating wheel (92) rotatably connected to the other end of the straight rod (91), the rotating wheel (92) is tangent to one side of the vertical push plate (72) away from the sleeve rod (71), the top surface of the upper straight rod (91) is at the same height as the top surface of the upper arc block (10), and the bottom surface of the lower straight rod (91) is at the same height as the bottom surface of the lower arc block (11); The external mixer (8) is fixedly connected with an arc convex rod (81), one side of the arc convex rod (81) close to the hollow shaft (3) is tangent to one end of the pressure receiving member (9) away from the hollow shaft (3), and the vertical push plate (72) only contacts the arc convex rod (81).

2. The polyphenylene sulfide production reactor of claim 1, wherein: The inner part of the water distribution sleeve (2) is divided into a lower storage area (21) and an upper storage area (22), the lower storage area (21) is not communicated with the upper storage area (22), the water distribution sleeve (2) is provided with a water inlet pipe (201) and a water outlet pipe (202), the water inlet pipe (201) is communicated with the lower storage area (21), and the water outlet pipe (202) is communicated with the upper storage area (22).

3. The polyphenylene sulfide production reactor of claim 2, wherein: The top end of the hollow shaft (3) is provided with a water inlet (301) and a water outlet (302), the water inlet (301) is located in the inside of the lower storage area (21), the water outlet (302) is located in the inside of the upper storage area (22), the outside of the hollow shaft (3) is provided with a plurality of water distribution pipes (303), the number of the water distribution pipes (303) is twice the number of the U-shaped pipes (5), and the two ends of the plurality of U-shaped pipes (5) are connected with the two water distribution pipes (303) to form a loop.

4. The polyphenylene sulfide production reactor of claim 3, wherein: The inside of the hollow shaft (3) is fixedly connected with a partition vertical plate (31), the partition vertical plate (31) divides the inside of the hollow shaft (3) into a water inlet area (311) and a water outlet area (312), the bottom ends of the water inlet area (311) and the water outlet area (312) are communicated, the top end of the water inlet area (311) is communicated with the water inlet (301), the top end of the water outlet area (312) is communicated with the water outlet (302), and the outside of the partition vertical plate (31) is provided with a plurality of cross-arc plates (32), the number of the cross-arc plates (32) is equal to the number of the U-shaped pipes (5), and the cross-arc plates (32) are used for flow guiding.

5. The polyphenylene sulfide preparation reaction kettle according to claim 2, characterized in that: The two sleeve rings (6) are divided into an upper sleeve ring (6) and a lower sleeve ring (6), the upper arc block (10) is fixedly connected with the upper sleeve ring (6), the lower arc block (11) is fixedly connected with the lower sleeve ring (6), the shapes of the upper arc block (10) and the lower arc block (11) are same, and the positions of the upper arc block (10) and the lower arc block (11) are symmetrical about the central axis of the sleeve ring (6).

6. A reaction process for preparing polyphenylene sulfide, using the reaction kettle for preparing polyphenylene sulfide according to claim 1, characterized in that, The method comprises the following steps: Step one: pretreat the raw materials, feed into the reactor (1) through the feeding port, and add the solvent at the same time; after feeding, close the feeding port to seal the reactor (1) to prevent subsequent material leakage or impurities from entering; Step two: pass high-temperature heat source into the outer pipe of the reactor (1) and the inside of the hollow shaft (3), gradually increase the temperature in the kettle to a preset value, and control the internal pressure of the reactor (1) at the same time; Step three: start the motor (4) to drive the hollow shaft (3) to rotate, stir the material, and make the material fully react to relieve uneven heating; Step four: stop the reaction, stop heating, inject cooling water into the outer pipe of the reactor (1) and the inside of the hollow shaft (3) to cool down, open the discharge port when the temperature and pressure are stable, and guide the polyphenylene sulfide to the subsequent separation and purification process to complete a single reaction.

Citation Information

Patent Citations

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