Post-treatment system for polysulfone polymer liquid

Abstract

The invention discloses a post-treatment system for polysulfone polymer liquid, and relates to the technical field of polysulfone production equipment. The polysulfone polymer liquid post-treatment system comprises a kettle body, a hopper, a crushing pump and a washing liquid circulating device, a first liquid inlet and a material return port are formed in the upper part of the kettle body, a liquid outlet channel, a washing liquid inlet and a first liquid outlet are formed in the bottom of the kettle body, an eluent outlet is formed in the top of the kettle body, and a first porous plate is arranged at the lower part in the kettle body; a second perforated plate capable of moving up and down is arranged at the upper part; the middle part of the hopper is communicated with the liquid outlet channel, the upper part of the hopper is provided with a feed port, and the lower part is provided with a discharge port; the feeding end of the smashing pump is connected with the discharging port, and the discharging end of the smashing pump is connected with the material returning port. According to the technical scheme provided by the invention, integrated operation of curing, crushing, gathering and washing of the polysulfone polymer liquid can be realized, the problem of low production efficiency caused by material transfer is effectively avoided, and repeated utilization of ethanol can also be realized.

Description

Technical Field

[0001] The present invention relates to the technical field of polysulfone production equipment, in particular to a polysulfone polymerization liquid post-processing system. Background Art

[0002] Currently, the main industrial production process for polysulfone is a one-step synthesis method, which is mainly divided into a polymerization stage and a post-processing stage. In the polymerization stage, bisphenol monomer, 4,4'-dichlorodiphenyl sulfone, an alkaline catalyst, a solvent, and a dehydrating agent are mixed. Under nitrogen protection and stirring, the raw materials are heated to cause a polymerization reaction. After the polymerization reaction is completed, the polymerization liquid is subjected to a post-processing stage.

[0003] Common solvents used in the polymerization process include dimethyl sulfoxide, N,N-dimethylformamide, N,N-dimethylacetamide, N-methylpyrrolidone, sulfolane, and diphenyl sulfone. Since higher polymerization temperatures increase the reaction rate and correspondingly shorten the polymerization time, the system temperature is often controlled above 210°C. Considering the boiling point of the solvent, sulfolane or diphenyl sulfone are the appropriate solvents for polymerization at these temperatures. Furthermore, since sulfolane decomposes at temperatures above 210°C, causing the polymerization solution to darken, affecting product quality, diphenyl sulfone is the solvent of choice for polymerization reactions above 210°C.

[0004] Using diphenyl sulfone as the solvent for the polymerization reaction, after completion of the polymerization, the conventional post-processing steps include: diluting the polymer solution with a solvent and filtering the diluted solution to remove impurities such as side reaction products and solid salts. The filtered polysulfone polymer solution is then added to water, methanol, or ethanol to form a solid product, which is then pulverized to form a solid powder of a certain particle size, containing residual diphenyl sulfone. Since diphenyl sulfone is insoluble in water, it must be eluted with an organic solvent, such as hot ethanol.

[0005] When ethanol washing is used to remove diphenyl sulfone, the resulting eluent is distilled at atmospheric or vacuum pressure to separate diphenyl sulfone and ethanol. However, distillation takes a long time and has a low ethanol recovery rate, which limits the recycling of ethanol during the washing process. Furthermore, existing polysulfone polymer solutions often require separate equipment for solidification and pulverization, and washing, which reduces production efficiency due to the material transfer and re-dosing. Summary of the Invention

[0006] The main purpose of the present invention is to propose a polysulfone polymerization liquid post-processing system, aiming to solve the problems of low production efficiency caused by the transfer and re-feeding of materials during the solidification, crushing and washing processes of the existing polysulfone polymerization liquid, and the need for distillation separation of the eluate generated when eluting diphenyl sulfone, which is time-consuming and has a low ethanol recovery rate, affecting the recycling of ethanol in the washing process.

[0007] To achieve the above object, the present invention provides a polysulfone polymerization liquid post-processing system, comprising: A kettle body is provided with a first liquid inlet and a return port at the top, a liquid outlet channel, a washing liquid inlet and a first liquid discharge port at the bottom, and an eluent outlet at the top. Control valves are provided on the first liquid inlet, the liquid outlet channel, the washing liquid inlet and the first liquid discharge port. A first porous plate is provided at the lower part of the kettle body and a second porous plate is provided at the upper part. The second porous plate can move back and forth along the axial direction of the kettle body. A hopper is provided on one side of the kettle body, the middle portion of the hopper is connected to the liquid outlet channel, the upper portion of the hopper is provided with a feed port, and the lower portion of the hopper is provided with a discharge port; A pulverizing pump, the feed end of which is connected to the discharge port, and the discharge end of which is connected to the return port; a washing liquid circulation device, the feed end of which is connected to the eluent outlet, and the discharge end of which is connected to the washing liquid inlet; and The heat preservation device is arranged on the outer wall of the kettle body.

[0008] In one embodiment, the polysulfone polymerization liquid post-processing system further comprises a spoiler. A second liquid inlet connected to the liquid outlet channel is provided in the middle of the hopper. The spoiler is disposed above the second liquid inlet and is tilted downwardly away from the kettle at an angle α, where 0°<α≤45°. Preferably, 30°≤α≤45°.

[0009] In one embodiment, the upper end of the hopper is located above the first porous plate.

[0010] In one embodiment, the feed end of the pulverizing pump is connected to the discharge port through a first connecting pipe, and the discharge end is connected to the return port through a reflux pipe; the lower end of the first connecting pipe and the lower end of the reflux pipe are both provided with a drain port, and each of the drain ports is provided with a control valve.

[0011] In one embodiment, along the transfer direction of the material, the washing liquid circulation device includes a cooler, a solid-liquid separator, a washing liquid tank, a circulation pump and a heater connected in sequence.

[0012] In one embodiment, the feed port of the cooler is connected to the eluent outlet via a second connecting pipe, the second connecting pipe is provided with a sampling port, and the sampling port is provided with a control valve.

[0013] In one embodiment, a discharge port is provided on the side wall of the kettle body above the first porous plate, and a control valve is provided on the discharge port.

[0014] In the technical solution of the present invention, in the initial state, the second porous plate is located above the first liquid inlet and the return port. During the solidification and pulverization operation, the control valve on the first liquid inlet is opened, and ethanol is fed into the kettle through the first liquid inlet until the ethanol liquid level is in the middle of the kettle. The control valve on the first liquid inlet is closed, the control valve on the liquid outlet channel is opened, and the pulverization pump is started. Ethanol can flow into the hopper through the liquid outlet channel. The ethanol in the hopper enters the pulverization pump through the outlet port and then flows back into the kettle through the return port, thereby forming a circulation of materials in the kettle and hopper, and the ethanol entering the hopper forms a disturbed state. Afterwards, the polysulfone polymerization liquid is added to the hopper through the feed port, and the polysulfone polymerization liquid falls into the disturbed and circulating ethanol, where it can be fully solidified and form linear solids. The grinding pump grinds the linear solids in the ethanol to form solid powder after grinding. The grinding pump sends the ground product to the return port, and the ethanol containing the solid powder flows back into the kettle body through the return port. The first porous plate intercepts the solid powder, and the ethanol can pass through the first porous plate and flow into the hopper through the liquid outlet channel. This cycle is repeated to solidify, grind and aggregate the polysulfone polymerization liquid.

[0015] After the solidification and pulverization process is completed, the control valve on the liquid outlet is closed, the pulverization pump stops operating, and the control valve on the first liquid outlet is opened to drain the ethanol from the kettle. The second porous plate is controlled to move downward, toward the first porous plate, until the second porous plate applies a predetermined pressure to the solid powder (polysulfone particles), confining the polysulfone particles to be washed between the first and second porous plates. The control valve on the washing liquid inlet is opened, and the washing liquid circulation device and the heat preservation device are activated. The washing liquid circulation device feeds hot ethanol into the washing kettle through the washing liquid inlet. The hot ethanol dissolves diphenyl sulfone. As the liquid level in the kettle continues to rise, the ethanol containing dissolved diphenyl sulfone (eluent) flows out of the kettle through the eluent outlet. The washing liquid circulation device cools the eluent, separates the solid and liquid, and heats the ethanol obtained after solid-liquid separation before feeding it back into the kettle. This ensures the recycling of the ethanol washing liquid while more effectively washing the polysulfone particles in the kettle. The heat preservation device also keeps the ethanol in the kettle warm.

[0016] The technical solution of the present invention can realize the integrated operation of solidification, crushing, aggregation and washing of polysulfone polymer liquid, effectively avoids the problem of low production efficiency caused by material transfer and re-dispensing, and can also realize the reuse of ethanol. During solidification and crushing, the polysulfone polymer liquid is added to the disturbed and circulating ethanol liquid, which can make the polysulfone polymer liquid more fully solidify and precipitate, ensure that the size range of the solidified precipitate is more concentrated, and reduce the burden of subsequent crushing treatment. The polysulfone particles in the kettle are washed by ethanol countercurrent circulation, and during washing, the polysulfone particles to be washed are confined between the first porous plate and the second porous plate, which can more fully remove the diphenyl sulfone on the polysulfone particles and ensure the washing effect. The washing liquid circulation device is used to realize the countercurrent circulation of ethanol, avoids the problems of long separation time and low ethanol recovery rate caused by distillation separation, and effectively improves the recycling effect of ethanol. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 A schematic structural diagram of an embodiment of a polysulfone polymerization liquid post-processing system provided by the present invention; Figure 2 for Figure 1 Schematic diagram of the structure of the middle hopper.

[0018] Description of Figure Numbers: 1. Kettle; 11. First liquid inlet; 111. First control valve; 12. Liquid outlet; 121. Second control valve; 13. Feed return port; 14. Washing liquid inlet; 141. Third control valve; 15. First liquid discharge port; 151. Fourth control valve; 16. Discharge port; 161. Ninth control valve; 17. First porous plate; 18. Second porous plate; 19. First insulation jacket; 191. First thermal oil inlet; 192. First thermal oil outlet; 110. Eluent outlet; 2. Oil cylinder; 21. Telescopic rod; 3. Hopper; 31. Cylinder; 32. Cone; 33. Cover plate; 34. Feed port; 35. Second liquid inlet; 36. Discharge port; 37. Spoiler; 4. Crushing pump; 41. A connecting pipe; 42, reflux pipe; 43, second liquid discharge port; 431, sixth control valve; 44, third liquid discharge port; 441, seventh control valve; 5, polymerization liquid tank; 51, feeding port; 511, fifth control valve; 52, discharge pipe; 521, flow regulating valve; 53, second insulation jacket; 531, second thermal oil inlet; 532, second thermal oil outlet; 61, cooler; 611, second connecting pipe; 612, sampling port; 613, eighth control valve; 62, solid-liquid separator; 621, solid discharge port; 622, tenth control valve; 63, washing liquid tank; 631, third liquid inlet; 64, circulation pump; 65, heater; 7, dryer; 71, feed pipe; 72, feed pump.

[0019] The purpose, features and advantages of the present invention will be further described with reference to the accompanying drawings and in conjunction with the embodiments. DETAILED DESCRIPTION

[0020] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts shall fall within the scope of protection of the present invention.

[0021] It should be noted that if the embodiments of the present invention involve directional indications (such as up, down, left, right, front, back, etc.), the directional indications are only used to explain the relative position relationship, movement status, etc. between the various components under a certain specific posture. If the specific posture changes, the directional indications will also change accordingly.

[0022] In addition, if there are descriptions involving "first", "second", etc. in the embodiments of the present invention, the descriptions of "first", "second", etc. are only for descriptive purposes and cannot be understood as indicating or suggesting their relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features limited to "first" and "second" may explicitly or implicitly include at least one of such features. In addition, if "and / or" or "and / or" appears in the full text, its meaning includes three parallel solutions. Taking "A and / or B" as an example, it includes solution A, solution B, or solutions that satisfy both A and B. In addition, the technical solutions between the various embodiments can be combined with each other, but it must be based on the ability of ordinary technicians in this field to implement. When the combination of technical solutions is mutually contradictory or cannot be implemented, it should be deemed that such a combination of technical solutions does not exist and is not within the scope of protection required by the present invention.

[0023] See also Figure 1 and Figure 2The present invention proposes a polysulfone polymerization liquid post-processing system, comprising: a kettle body 1, a hopper 3, a crushing pump 4, a washing liquid circulation device and a heat preservation device. The upper part of the kettle body 1 is provided with a first liquid inlet 11 and a return port 13, the bottom of the kettle body 1 is provided with a liquid outlet channel 12, a washing liquid inlet 14 and a first liquid discharge port 15, the top of the kettle body 1 is provided with an eluent outlet 110, the first liquid inlet 11, the liquid outlet channel 12, the washing liquid inlet 14 and the first liquid discharge port 15 are all provided with control valves, the lower part of the kettle body 1 is provided with a first porous plate 17, the upper part of the kettle body 1 is provided with a second porous plate 18, and the second porous plate 18 can move back and forth along the axial direction of the kettle body 1; The hopper 3 is arranged on one side of the kettle body 1, the middle part of the hopper 3 is connected to the liquid outlet channel 12, the upper part of the hopper 3 is provided with a feed port 34, and the lower part of the hopper 3 is provided with a discharge port 36; the feed end of the pulverizing pump 4 is connected to the discharge port 36, and the discharge end of the pulverizing pump 4 is connected to the return port 13; the feed end of the washing liquid circulation device is connected to the eluent outlet 110, and the discharge end of the washing liquid circulation device is connected to the washing liquid inlet 14; the insulation device is arranged on the outer wall of the kettle body 1.

[0024] In the technical solution of the present invention, a first control valve 111 is provided at the first liquid inlet 11, a second control valve 121 is provided at the liquid outlet 12, a third control valve 141 is provided at the washing liquid inlet 14, and a fourth control valve 151 is provided at the first liquid outlet 15. Along the material transfer direction, the washing liquid circulation device includes a cooler 61, a solid-liquid separator 62, a washing liquid tank 63, a circulation pump 64, and a heater 65, which are connected in sequence.

[0025] In the initial state, the second porous plate 18 is located above the first liquid inlet 11 and the return port 13. During the solidification and pulverization operation, the first control valve 111 is opened, and anhydrous ethanol at a temperature of 25±2°C is fed into the kettle 1 through the first liquid inlet 11. The ethanol liquid level is in the middle of the kettle 1. The first control valve 111 is closed, the second control valve 121 on the liquid outlet channel 12 is opened, and the pulverization pump 4 is started. The ethanol can flow into the hopper 3 through the liquid outlet channel 12. The ethanol in the hopper 3 enters the pulverization pump 4 through the discharge port 36 and then flows back into the kettle 1 through the return port 13. This circulates the ethanol material in the kettle 1 and hopper 3, and the ethanol entering the hopper 3 forms a disturbed state. Afterwards, the polysulfone polymerization liquid is added to the hopper 3 through the feed port 34, and the polysulfone polymerization liquid falls into the disturbed and circulating ethanol, where it can be fully solidified and form linear solids. The pulverizing pump 4 pulverizes the linear solids in the ethanol, and the linear solids are pulverized to form solid powder. The pulverizing pump 4 sends the pulverized product to the return port 13, and the ethanol containing the solid powder flows back into the kettle body 1 through the return port 13. The first porous plate 17 intercepts the solid powder, and the ethanol can pass through the first porous plate 17 and flow into the hopper 3 through the liquid outlet channel 12. This cycle is repeated to solidify, pulverize and aggregate the polysulfone polymerization liquid.

[0026] After the solidification and pulverization process is completed, second control valve 121 is closed, pulverization pump 4 stops operating, and fourth control valve 151 is opened to drain the ethanol from kettle 1. Fourth control valve 151 is closed, and second porous plate 18 is controlled to move downward, that is, toward first porous plate 17, until second porous plate 18 applies a pressure of 19.6 to 39.2 N to the solid powder (polysulfone particles), thereby confining the polysulfone particles to be washed between first and second porous plates 17, 18. Opening third control valve 141 activates the washing liquid circulation system and heat preservation device. Circulating pump 64 delivers anhydrous ethanol (25±2°C) stored in washing liquid tank 63 to heater 65, which heats the ethanol to 30-50°C. The heated ethanol then enters kettle 1 through washing liquid inlet 14. The hot ethanol dissolves diphenyl sulfone. As the liquid level in kettle 1 continues to rise, the ethanol containing dissolved diphenyl sulfone (eluent) flows out of kettle 1 through eluent outlet 110 and into cooler 61. Cooler 61 lowers the temperature of the eluent to 20-25°C, causing the diphenyl sulfone to solidify. The ethanol containing the diphenyl sulfone solids is then delivered to solid-liquid separator 62. The ethanol obtained after solid-liquid separation is then delivered to washing liquid tank 63. Circulating pump 64 delivers the ethanol from washing liquid tank 63 to heater 65, where it is heated and then delivered to kettle 1. This achieves recycling of the ethanol washing liquid.

[0027] After the washing operation is completed, the third control valve 141 is closed, the washing liquid circulation device and the insulation device stop working, the second porous plate 18 is controlled to move upward to reset, and the fourth control valve 151 is opened to discharge the ethanol in the kettle body 1. After that, the fourth control valve 151 is closed to discharge the polysulfone particles accumulated on the first porous plate 17.

[0028] It can be understood that, during solidification and pulverization, the ratio of the volume of the polysulfone polymer solution added to the hopper 3 to the volume of the anhydrous ethanol added to the kettle body 1 through the first liquid inlet 11 is 1:(3-6). The preparation of the polysulfone polymerization liquid includes: adding 200-230 kg of 4,4′-dichlorodiphenyl sulfone, 180-185 kg of bisphenol S, 90 kg of potassium hydroxide, 1500 L of diphenyl sulfone and 100 L of xylene (CAS number 1330-20-7) into a reactor; heating the reaction mixture to 140° C. under nitrogen protection and stirring, and maintaining the temperature for 4 hours; further heating the reaction mixture to 210-230° C. under nitrogen protection and stirring, and maintaining the temperature for 6 hours to obtain a polyethersulfone viscous liquid; adding molten diphenyl sulfone (temperature of 200-250° C.) into the polyethersulfone viscous liquid, and fully stirring the mixture to dilute the polyethersulfone viscous liquid to obtain a polyethersulfone diluted liquid, wherein the mass ratio of the molten diphenyl sulfone to the polyethersulfone viscous liquid is 1:(1.5-2.5). The polyethersulfone dilution liquid is filtered at a temperature of 200-250°C to achieve solid-liquid separation to remove impurities such as side reaction products and solid salts. The filtrate obtained by filtration is the polysulfone polymerization liquid.

[0029] It should be noted that the outer diameters of the first and second porous plates 17, 18 are compatible with the inner diameter of the kettle body 1. The apertures of the through-holes in the first and second porous plates 17, 18 are smaller than the particle size of the solid powder. For example, if the particle size of the solid powder is 50-80 μm, the apertures of the through-holes in the first and second porous plates 17, 18 are 10-30 μm. The hopper 3 comprises a connected barrel 31 and a conical body 32, with the conical body 32 positioned below the barrel 31. The upper end of the barrel 31 constitutes the upper end of the hopper 3, while the lower end of the conical body 32 constitutes the lower end of the hopper 3. The upper end of the barrel 31 is positioned above the first porous plate 17. A cover plate 33 is provided at the upper end of the barrel 31, on which the feed port 34 is disposed. The lower end of the conical body 32 is provided with the discharge port 36. A second liquid inlet 35 is provided on the side wall of the middle portion of the cylinder 31 . The second liquid inlet 35 is communicated with the liquid outlet channel 12 . The liquid outlet channel 12 is provided horizontally.

[0030] In order to ensure that the polysulfone polymer solution can be fully solidified when it falls into ethanol, the polysulfone polymer solution solidification and crushing device further includes a spoiler 37, which is arranged at the upper end of the second liquid inlet 35, and the spoiler 37 is tilted downward at an angle α in the direction away from the kettle body 1, and the angle 0°<α≤45°.

[0031] By adopting the above technical solution, the ethanol in the kettle body 1 flows through the liquid outlet channel 12 to the second liquid inlet 35, and then contacts the spoiler 37. The spoiler 37 arranged at a downward angle can change the flow direction and flow rate of the ethanol fluid, so as to more fully disturb the ethanol entering the hopper 3. The polysulfone polymer liquid enters the disturbed ethanol flow and can be more fully solidified to form a linear solid body, which is convenient for the crushing pump 4 to crush the linear solid body.

[0032] It is understood that the shape of the spoiler 37 is adapted to the cross-sectional shape of the liquid outlet channel 12. In one embodiment, the cross-sectional shape of the liquid outlet channel 12 is circular, the spoiler 37 is in the shape of a pancake, and the cross-sectional diameter of the spoiler 37 is slightly larger than the cross-sectional diameter of the liquid outlet channel 12.

[0033] In order to stably add the polysulfone polymerization liquid into the hopper 3 , a polymerization liquid tank 5 is further included. A discharge pipe 52 is provided at the bottom of the polymerization liquid tank 5 . A flow regulating valve 521 is provided on the discharge pipe 52 . The discharge end of the discharge pipe 52 is connected to the feed port 34 .

[0034] By adopting the above technical solution, the polysulfone polymerization liquid to be processed is added to the polymerization liquid tank 5. By controlling the opening of the flow regulating valve 521, the flow rate of the polysulfone polymerization liquid entering the hopper 3 can be controlled to effectively ensure the curing effect of the polysulfone polymerization liquid. It will be understood that the top of the polymerization liquid tank 5 is provided with a feed port 51, through which the polysulfone polymerization liquid to be processed is added to the polymerization liquid tank 5. The feed port 51 is provided with a fifth control valve 511. Under normal circumstances, the fifth control valve 511 is in a closed state. When the polysulfone polymerization liquid needs to be added to the polymerization liquid tank 5, the fifth control valve 511 is opened.

[0035] It can be understood that under normal circumstances, the flow regulating valve 521 is in a closed state. When solidification and crushing operations are required, after the ethanol in the kettle body 1 and the hopper 3 form a circulation, the opening of the flow regulating valve 521 is controlled to allow the polysulfone polymerization liquid in the polymerization liquid tank 5 to flow into the ethanol flowing in the hopper 3.

[0036] In order to allow the polysulfone polymerization liquid stored in the polymerization liquid tank 5 to flow smoothly into the hopper 3 , the polymerization liquid tank 5 is located directly above the hopper 3 .

[0037] In order to keep the polysulfone polymerization liquid stored in the polymerization liquid tank 5 in an optimal flow state, a second insulation jacket 53 is provided on the outer wall of the polymerization liquid tank 5, a second heat transfer oil inlet 531 is provided at the lower part of the second insulation jacket 53, and a second heat transfer oil outlet 532 is provided at the upper part of the second insulation jacket 53. Heat transfer oil at 200~250℃ flows into the second insulation jacket 53 through the second heat transfer oil inlet 531, and after heat exchange, flows out from the second heat transfer oil outlet 532.

[0038] Furthermore, the feed end of the pulverizing pump 4 is connected to the discharge port 36 through a first connecting pipe 41, and the discharge end of the pulverizing pump 4 is connected to the return port 13 through a return pipe 42; the lower end of the first connecting pipe 41 and the lower end of the return pipe 42 are both provided with a drainage port, and each of the drainage ports is provided with a control valve.

[0039] By adopting the above technical solution, a second drain port 43 is provided at the lower end of the first connecting pipe 41, and a sixth control valve 431 is installed on the second drain port 43. A third drain port 44 is provided at the lower end of the return pipe 42, and a seventh control valve 441 is installed on the third drain port 44. Under normal circumstances, the sixth control valve 431 and the seventh control valve 441 are both in a closed state. After the solidification and pulverization operation is completed, the fourth control valve 151, the sixth control valve 431, and the seventh control valve 441 can be opened to drain the ethanol in the hopper 3 and the first connecting pipe 41, as well as the ethanol in the return pipe 42, thereby achieving ethanol recovery and utilization.

[0040] In order to better drive the second porous plate 18 to move back and forth along the axial direction of the kettle body 1, that is, to drive the second porous plate 18 to move upward or downward, the polysulfone particle washing device also includes a telescopic rod 21, which is arranged on the kettle body 1, and the bottom of the telescopic rod 21 is connected to the second porous plate 18.

[0041] By adopting the above technical solution, the bottom of the telescopic rod 21 extends into the kettle body 1 and is connected to the second porous plate 18. By controlling the extension or shortening of the telescopic rod 21, the second porous plate 18 can be moved upward or downward.

[0042] Specifically, the telescopic rod 21 is the piston rod of the oil cylinder 2. The oil cylinder 2 is arranged on the outer wall of the top of the kettle body 1, and the piston rod of the oil cylinder 2 constitutes the telescopic rod 21. By controlling the extension and contraction of the piston rod, the second porous plate 18 can be moved downward or upward.

[0043] In order to better insulate the ethanol in the kettle body 1, the insulation device includes a first insulation jacket 19, which is arranged on the outer wall of the kettle body 1. The lower part of the first insulation jacket 19 is provided with a first heat transfer oil inlet 191, and the upper part is provided with a first heat transfer oil outlet 192.

[0044] By adopting the above technical solution, during the washing operation, the heat transfer oil at 60~70°C enters the first insulation jacket 19 through the first heat transfer oil inlet 191 and flows out from the first heat transfer oil outlet 192, thereby keeping the ethanol in the kettle body 1 warm and ensuring the washing effect of the hot ethanol.

[0045] Specifically, the feed port 34 of the cooler 61 is connected to the eluent outlet 110 via a second connecting pipe 611 . The second connecting pipe 611 is provided with a sampling port 612 , and the sampling port 612 is provided with an eighth control valve 613 .

[0046] By adopting the above technical solution, under normal circumstances, the eighth control valve 613 is in a closed state. During the washing process, the eighth control valve 613 can be opened periodically according to production needs to remove eluent samples for testing. After the samples are taken, the eighth control valve 613 is closed. The removed eluent samples are tested. If the eluent contains diphenyl sulfone, it indicates that the diphenyl sulfone has not been completely removed and the washing process needs to continue. If the eluent does not contain diphenyl sulfone, it indicates that the diphenyl sulfone has been completely removed and the washing process is complete. The washing liquid circulation device can be closed, the second porous plate 18 can be reset, the third control valve 141 can be closed, and the heat preservation device can be stopped.

[0047] Furthermore, a discharge port 16 is provided on the side wall of the kettle body 1 above the first porous plate 17. A ninth control valve 161 is provided on the discharge port 16. Normally, the ninth control valve 161 is closed. When the washing operation is completed and the washed polysulfone particles need to be discharged, the ninth control valve 161 can be opened.

[0048] The diphenyl sulfone solid obtained by separation in the solid-liquid separator 62 can be recycled. A solid discharge port 621 is provided on the solid-liquid separator 62, and a tenth control valve 622 is provided on the solid discharge port 621. Under normal circumstances, the tenth control valve 622 is in a closed state. When the washing operation is completed and the diphenyl sulfone solid needs to be taken out, the tenth control valve 622 can be opened to take out the diphenyl sulfone solid, and after drying, it can be recycled.

[0049] Furthermore, it also includes a dryer 7 and a feed pipe 71, one end of the feed pipe 71 is connected to the feed end of the dryer 7, and the other end of the feed pipe 71 is connected to the solid discharge port 621 of the solid-liquid separator. A feed pump 72 is provided on the feed pipe 71. When the diphenyl sulfone solid matter in the solid-liquid separator 62 needs to be taken out for drying, the tenth control valve 622 is opened and the feed pump 72 is started to send the diphenyl sulfone solid matter in the solid-liquid separator 62 into the dryer 7 to dry the diphenyl sulfone solid matter.

[0050] It should be noted that during the initial wash, the mass ratio of the polysulfone particles to be washed to the anhydrous ethanol added to the washing liquid tank 63 is 1:(6-10), where the mass of the polysulfone particles to be washed is calculated based on the mass of the polysulfone polymerization liquid. A third liquid inlet 631 is provided at the top of the washing liquid tank 63. A control valve is provided on this third liquid inlet 631. Normally, the control valve is closed. When ethanol washing liquid is needed, the control valve is opened to allow the addition of washing liquid to the washing liquid tank 63, thereby washing the polysulfone particles.

[0051] When the next washing operation is performed, considering that there is residual ethanol in the pipe and the container after the previous washing, the amount of ethanol added to the washing liquid tank can be reduced during the next washing, that is, the mass ratio of the polysulfone particles to be washed and the anhydrous ethanol added to the washing liquid tank through the third liquid inlet is 1: (5~8).

[0052] The above description is merely an exemplary embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural transformation made by utilizing the contents of the present invention's description and drawings under the technical concept of the present invention, or directly / indirectly applied in other related technical fields, is included in the patent protection scope of the present invention.

Claims

1. A polysulfone polymerization liquid post-processing system, characterized in that: include: A kettle body is provided with a first liquid inlet and a return port at the top, a liquid outlet channel, a washing liquid inlet and a first liquid discharge port at the bottom, and an eluent outlet at the top. The first liquid inlet, the liquid outlet channel, the washing liquid inlet and the first liquid discharge port are all provided with control valves. A first porous plate is provided at the lower part of the kettle body, and a second porous plate is provided at the upper part. The second porous plate can move back and forth along the axial direction of the kettle body. A hopper is provided on one side of the kettle body, the middle portion of the hopper is connected to the liquid outlet channel, the upper portion of the hopper is provided with a feed port, and the lower portion of the hopper is provided with a discharge port; A pulverizing pump, the feed end of which is connected to the discharge port, and the discharge end of which is connected to the return port; a washing liquid circulation device, the feed end of which is connected to the eluent outlet, and the discharge end of which is connected to the washing liquid inlet; and The heat preservation device is arranged on the outer wall of the kettle body.

2. The polysulfone polymerization liquid post-processing system according to claim 1, characterized in that: The polysulfone polymerization liquid post-processing system also includes a spoiler. A second liquid inlet connected to the liquid outlet channel is provided in the middle of the hopper. The spoiler is provided at the upper end of the second liquid inlet, and the spoiler is tilted downward at an angle α in the direction away from the kettle body, 0°<α≤45°.

3. The polysulfone polymerization liquid post-processing system according to claim 1, characterized in that: The upper end of the hopper is located above the first porous plate.

4. The polysulfone polymerization liquid post-processing system according to claim 1, characterized in that: The feed end of the pulverizing pump is connected to the discharge port through a first connecting pipe, and the discharge end is connected to the return port through a reflux pipe; the lower end of the first connecting pipe and the lower end of the reflux pipe are both provided with drainage ports, and each drainage port is provided with a control valve.

5. The polysulfone polymerization liquid post-processing system according to claim 1, characterized in that: Along the transfer direction of the material, the washing liquid circulation device includes a cooler, a solid-liquid separator, a washing liquid tank, a circulation pump and a heater which are connected in sequence.

6. The polysulfone polymerization liquid post-processing system according to claim 5, characterized in that: The feed port of the cooler is connected to the eluent outlet via a second connecting pipe. The second connecting pipe is provided with a sampling port, and the sampling port is provided with a control valve.

7. The polysulfone polymerization liquid post-processing system according to claim 1, characterized in that: A discharge port is provided on the side wall of the kettle body above the first porous plate, and a control valve is provided on the discharge port.

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