Polysulfone particulate washing apparatus

Abstract

The utility model discloses a kind of polysulfone granular material washing devices, relate to polysulfone production equipment technical field.Polysulfone granular material washing device, including washing kettle, heat preservation device and washing liquid circulating device, the upper portion of washing kettle is provided with feed inlet, top is provided with eluent outlet, bottom is provided with washing liquid inlet, the lower portion in washing kettle is provided with first perforated plate, upper portion is provided with second perforated plate, second perforated plate can be moved back and forth along the axial direction of washing kettle;Heat preservation device is set on washing kettle;Washing liquid circulating device includes the cooler, solid-liquid separator, washing liquid tank, circulating pump and heater connected in sequence.The technical scheme of the utility model adopts the mode of ethanol countercurrent circulation flow to wash polysulfone granular material in washing kettle, and when washing, limit the polysulfone granular material to be washed between first perforated plate and second perforated plate, can more fully elute diphenyl sulfone on polysulfone granular material, guarantee the washing effect.

Description

Technical Field

[0001] This utility model relates to the technical field of polysulfone production equipment, and in particular to a polysulfone particulate washing device. Background Technology

[0002] Currently, the main industrial production process for polysulfone is the one-step synthesis method, which mainly consists of 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 materials are heated to undergo a polymerization reaction. After the polymerization reaction is complete, the polymerization reaction solution is sent to the post-processing stage.

[0003] Commonly used solvents in the polymerization process include dimethyl sulfoxide, N,N-dimethylformamide, N,N-dimethylacetamide, N-methylpyrrolidone, sulfolane, and diphenyl sulfone. Since higher polymerization temperatures result in faster reaction rates and shorter polymerization times, 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 this polymerization temperature. However, at temperatures above 210°C, sulfolane decomposes, causing the polymerization solution to turn black and affecting product quality. Therefore, diphenyl sulfone is chosen as the solvent for polymerization reactions above 210°C.

[0004] Diphenyl sulfone is used as the solvent in the polymerization reaction. After the polymerization reaction, the conventional post-processing steps are as follows: the polymerization solution is diluted with a solvent, and the diluted solution is filtered to remove by-products and impurities such as solid salts. The filtered polysulfone polymer solution is added to water, methanol, or ethanol, and solidification occurs to precipitate a solid. The solid is then pulverized to form a solid powder with a certain particle size, on which diphenyl sulfone residue remains. Since diphenyl sulfone is insoluble in water, an organic solvent, such as hot ethanol, is required for elution. Current methods of using ethanol washing to remove diphenyl sulfone involve distilling the eluent under normal or reduced pressure to separate the diphenyl sulfone and ethanol. However, distillation is time-consuming and has a low ethanol recovery rate, affecting the recycling of ethanol during the washing process. Utility Model Content

[0005] The main purpose of this invention is to propose a polysulfone particulate washing device, which aims to solve the problem that the eluent generated when using ethanol to wash diphenyl sulfone requires distillation separation, which is time-consuming and has a low ethanol recovery rate, thus affecting the recycling of ethanol during the washing process.

[0006] To achieve the above objectives, this utility model proposes a polysulfone particulate matter washing device, comprising:

[0007] A washing vessel has a feed inlet at the top, an eluent outlet at the top, and a washing liquid inlet at the bottom. A first perforated plate is provided in the lower part of the washing vessel, and a second perforated plate is provided in the upper part. The second perforated plate can move back and forth along the axial direction of the washing vessel.

[0008] A heat preservation device is installed on the washing vessel; and,

[0009] The washing liquid circulation device, along the material transfer direction, includes a cooler, a solid-liquid separator, a washing liquid tank, a circulation pump, and a heater connected in sequence. The inlet of the cooler is connected to the washing liquid outlet through a connecting pipe, and the outlet of the heater is connected to the washing liquid inlet through a pipe.

[0010] In one embodiment, the polysulfone particulate washing device further includes a telescopic rod disposed on the washing vessel, and the bottom of the telescopic rod is connected to the second perforated plate.

[0011] In one embodiment, the telescopic rod is the piston rod of a hydraulic cylinder.

[0012] In one embodiment, a sampling port is provided on the connecting pipe, and a second control valve is provided on the sampling port.

[0013] In one embodiment, the heat preservation device includes a heat preservation jacket disposed on the outer wall of the washing vessel. The lower part of the heat preservation jacket is provided with a heat exchange medium inlet, and the upper part is provided with a heat exchange medium outlet.

[0014] In one embodiment, the diameter of the through holes on both the first porous plate and the second porous plate is less than 40 μm.

[0015] In one embodiment, the bottom of the washing tank is further provided with a washing liquid discharge port, and a third control valve is provided on the washing liquid discharge port.

[0016] In one embodiment, a discharge port is provided on the side wall of the washing vessel above the first perforated plate, and a fourth control valve is provided on the discharge port.

[0017] In the technical solution of this utility model, in the initial state, the second porous plate is located above the feed inlet. The polysulfone particles to be washed are fed into the washing tank through the feed inlet. After the feeding is completed, the second porous plate is controlled to move downward, that is, move towards the direction of the first porous plate, until the second porous plate acts on the polysulfone particles to confine the polysulfone particles to be washed between the first porous plate and the second porous plate. The washing liquid circulation device and the heat preservation device are activated. The circulation pump sends the ethanol stored in the washing liquid tank into the heater, which heats the ethanol. The heated ethanol enters the washing vessel from the washing liquid inlet. The hot ethanol dissolves diphenyl sulfone. As the liquid level in the washing vessel rises, the ethanol containing dissolved diphenyl sulfone (eluent) flows out of the washing vessel from the eluent outlet. After being cooled by the cooler, the diphenyl sulfone solidifies. The ethanol containing the diphenyl sulfone solid is sent to the solid-liquid separator. The ethanol obtained after solid-liquid separation is sent back to the washing liquid tank. The circulation pump sends the ethanol from the washing liquid tank to the heater, and after heating, it is sent to the washing vessel. In this way, the ethanol washing liquid is recycled while the polysulfone particles between the first and second porous plates are thoroughly washed. The heat preservation device maintains the temperature of the ethanol washing liquid in the washing vessel to ensure the washing effect of the ethanol.

[0018] The technical solution of this utility model uses a countercurrent circulation of ethanol to wash polysulfone particles in the washing vessel. During washing, the polysulfone particles to be washed are confined between the first porous plate and the second porous plate, which can effectively remove diphenyl sulfone from the polysulfone particles, ensuring the washing effect. In addition, with the washing liquid circulation device, the problem of excessive separation time and low ethanol recovery rate caused by distillation separation is effectively avoided, and the recycling effect of ethanol is effectively improved. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of an embodiment of a polysulfone particulate washing device provided by this utility model.

[0020] Explanation of icon numbers:

[0021] 1. Washing vessel; 11. Feed inlet; 111. First control valve; 12. Washing liquid inlet; 13. Eluent outlet; 14. Discharge outlet; 141. Third control valve; 15. Washing liquid discharge outlet; 151. Fourth control valve; 16. First perforated plate; 17. Second perforated plate; 171. Oil cylinder; 172. Telescopic rod; 18. Insulation jacket; 181. Heat exchange medium inlet; 182. Heat exchange medium outlet; 2. Cooler; 21. Connecting pipe; 22. Sampling port; 221. Second control valve; 3. Solid-liquid separator; 31. Solid material outlet; 331. Fifth control valve; 4. Washing liquid tank; 41. Liquid inlet; 5. Circulating pump; 6. Heater; 7. Dryer; 71. Feed pipe.

[0022] The realization of the purpose, functional features and advantages of this utility model will be further explained in conjunction with the embodiments and with reference to the accompanying drawings. Detailed Implementation

[0023] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present utility model.

[0024] It should be noted that if the embodiments of this utility model involve directional indicators (such as up, down, left, right, front, back, etc.), the directional indicators are only used to explain the relative positional relationship and movement of the components in a specific posture. If the specific posture changes, the directional indicators will also change accordingly.

[0025] Furthermore, if the embodiments of this utility model involve descriptions such as "first" or "second," these descriptions are for descriptive purposes only and should not be construed as indicating or implying their relative importance or implicitly specifying the number of technical features indicated. Therefore, a feature defined with "first" or "second" may explicitly or implicitly include at least one of those features. Additionally, the use of "and / or" or "and / or" throughout the text includes three parallel solutions. For example, "A and / or B" includes solution A, solution B, or a solution where both A and B are satisfied simultaneously. Furthermore, the technical solutions of the various embodiments can be combined with each other, but this must be based on the ability of those skilled in the art to implement them. When the combination of technical solutions is contradictory or impossible to implement, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection claimed by this utility model.

[0026] Please see Figure 1This utility model proposes a polysulfone particulate matter washing device, comprising: a washing tank 1, a heat preservation device, and a washing liquid circulation device. The washing tank 1 has a feed inlet 11 at its upper part, an eluent outlet 13 at its top, and a washing liquid inlet 12 at its bottom. A first perforated plate 16 is located in the lower part of the washing tank 1, and a second perforated plate 17 is located in the upper part of the washing tank 1. The second perforated plate 17 can move back and forth along the axial direction of the washing tank 1. The heat preservation device is disposed on the washing tank 1. Along the material transfer direction, the washing liquid circulation device includes a cooler 2, a solid-liquid separator 3, a washing liquid tank 4, a circulation pump 5, and a heater 6 connected in sequence. The feed inlet 11 of the cooler 2 is connected to the eluent outlet 13 via a connecting pipe 21, and the outlet of the heater 6 is connected to the washing liquid inlet 12 via a pipe.

[0027] In the technical solution of this utility model, in the initial state, the second porous plate 17 is located above the feed inlet 11, providing polysulfone particles to be washed and anhydrous ethanol at 25±2℃, with a mass ratio of polysulfone particles to anhydrous ethanol of 1:(6~10). The polysulfone particles to be washed are fed into the washing vessel 1 through the feed inlet 11. After feeding is completed, the second porous plate 17 is controlled to move downward, that is, move towards the first porous plate 16, until the second porous plate 17 acts on the polysulfone particles with a pressure of 19.6~39.2N, so as to confine the polysulfone particles to be washed between the first porous plate 16 and the second porous plate 17. Anhydrous ethanol is added to the washing liquid tank 4. The washing liquid circulation device and the heat preservation device are started. The circulation pump 5 sends the ethanol stored in the washing liquid tank 4 to the heater 6. The heater 6 heats the ethanol to 30~50℃. The heated ethanol enters the washing vessel 1 from the washing liquid inlet 12. The heat preservation device keeps the ethanol in the washing vessel 1 warm. The hot ethanol can dissolve diphenyl sulfone, allowing it to detach from the polysulfone particles. As hot ethanol continuously enters the washing vessel 1, the liquid level in the washing vessel 1 continuously rises. The ethanol containing dissolved diphenyl sulfone (eluent) flows out of the washing vessel 1 from the eluent outlet 13 and enters the cooler 2. Cooler 2 lowers the temperature of the eluent to 20-25°C, causing diphenyl sulfone to solidify into a solid. Ethanol containing the diphenyl sulfone solid enters solid-liquid separator 3. The ethanol obtained after solid-liquid separation is sent to washing liquid tank 4. Circulation pump 5 sends the ethanol in washing liquid tank 4 to heater 6. After heating, it is sent to washing vessel 1. In this way, the ethanol washing liquid is recycled while the polysulfone particles between the first porous plate and the second porous plate are thoroughly washed.

[0028] It should be noted that a first control valve 111 is provided on the feed inlet 11. Under normal conditions, the first control valve 111 is in the closed state. When it is necessary to add polysulfone particles to be cleaned into the washing tank 1, the first control valve 111 is in the open state. The pore size of the through holes on the first porous plate 16 and the second porous plate 17 is smaller than the particle size of the polysulfone particles. For example, if the particle size of the polysulfone particles is 50~80μm, the pore size of the through holes on the first porous plate 16 and the second porous plate 17 is 10~30μm. A liquid inlet 41 is provided at the top of the washing liquid tank 4. A control valve is provided on the liquid inlet 41. Under normal conditions, the control valve is in the closed state. When it is necessary to add ethanol washing liquid into the washing liquid tank 4, the control valve is opened to add the washing liquid into the washing liquid tank 4. When performing the next washing operation, considering the residual ethanol in the pipes and containers after the previous washing, the amount of ethanol added to the washing liquid tank 4 can be reduced. That is, the mass ratio of the polysulfone particles to be washed to the anhydrous ethanol added to the washing liquid tank 4 through the inlet 41 is 1:(5~8). The outer diameters of the first and second porous plates are adapted to the inner diameter of the washing vessel.

[0029] In order to better drive the second porous plate 17 to move back and forth along the axial direction of the washing tank 1, that is, to drive the second porous plate 17 to move upward or downward, the polysulfone particulate washing device also includes a telescopic rod 172, which is disposed on the washing tank 1 and the bottom of the telescopic rod 172 is connected to the second porous plate 17.

[0030] By adopting the above technical solution, the bottom of the telescopic rod 172 extends into the washing tank 1 and is connected to the second perforated plate 17. By controlling the extension or shortening of the telescopic rod 172, the second perforated plate 17 can be moved upward or downward.

[0031] Specifically, the telescopic rod 172 is the piston rod of the hydraulic cylinder 171. The hydraulic cylinder 171 is installed on the outer wall of the top of the washing vessel 1, and the piston rod of the hydraulic cylinder 171 constitutes the telescopic rod 172. By controlling the extension and retraction of the piston rod, the second perforated plate 17 can be moved downward or upward.

[0032] In order to better keep the ethanol in the washing vessel 1 warm, the heat preservation device includes a heat preservation jacket 18, which is disposed on the outer wall of the washing vessel 1. The lower part of the heat preservation jacket 18 is provided with a heat exchange medium inlet 181, and the upper part is provided with a heat exchange medium outlet 182.

[0033] By adopting the above technical solution, during the washing operation, the heat transfer oil at 60~70℃ enters the insulation jacket 18 through the heat exchange medium inlet 181 and flows out from the heat exchange medium outlet 182. In this way, the ethanol in the washing tank 1 is kept warm, ensuring the washing effect of the hot ethanol.

[0034] In order to better determine whether the diphenyl sulfone on the polysulfone particles has been washed off, a sampling port 22 is provided on the connecting pipe 21, and a second control valve 221 is provided on the sampling port 22.

[0035] By adopting the above technical solution, under normal conditions, the second control valve 221 is in the closed state. During the washing process, the second control valve 221 can be opened periodically as needed to take out eluent samples for testing. After the samples are taken, the second control valve 221 is closed. The taken-out eluent samples are tested. If the eluent contains diphenyl sulfone, it means that the diphenyl sulfone has not been completely removed, and the washing operation needs to continue. If the eluent does not contain diphenyl sulfone, it means that the diphenyl sulfone has been completely removed, the washing device can be turned off, the second porous plate 17 is reset, and the washing operation ends.

[0036] Furthermore, the bottom of the washing vessel 1 is provided with a washing liquid discharge port 15, and a third control valve 141 is provided on the washing liquid discharge port 15.

[0037] By adopting the above technical solution, under normal conditions, the third control valve 141 is in a closed state. When the washing operation is completed, the third control valve 141 is opened to discharge the ethanol in the washing tank 1. The discharged ethanol can be recycled.

[0038] Furthermore, a discharge port 14 is provided on the side wall of the washing tank 1 above the first porous plate 16, and a fourth control valve 151 is provided on the discharge port 14. Under normal conditions, the fourth control valve 151 is in a closed state. After the washing operation is completed and the ethanol in the washing tank 1 is discharged, the fourth control valve 151 can be opened to discharge the washed polysulfone particles.

[0039] The diphenyl sulfone solid obtained by the solid-liquid separator 3 can be recycled. The solid-liquid separator 3 is provided with a solid discharge port 31 and a fifth control valve 331. Under normal conditions, the fifth control valve 331 is in the closed state. When the washing operation is completed and the diphenyl sulfone solid needs to be removed, the fifth control valve 331 can be opened to remove the diphenyl sulfone solid and dry it for recycling.

[0040] Furthermore, the polysulfone particulate matter washing device 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 31 of the solid-liquid separator. A feed pump is installed on the feed pipe 71. When it is necessary to remove the diphenyl sulfone solids in the solid-liquid separator 3 for drying, the fifth control valve 331 is opened and the feed pump is started, so that the diphenyl sulfone solids in the solid-liquid separator 3 can be sent into the dryer 7 for drying.

[0041] The above description is merely an exemplary embodiment of the present utility model and does not limit the patent scope of the present utility model. Any equivalent structural transformations made based on the technical concept of the present utility model and the contents of the present utility model specification and drawings, or direct / indirect applications in other related technical fields, are included within the patent protection scope of the present utility model.

Claims

1. A polysulfone particulate matter washing device, characterized in that, include: A washing vessel has a feed inlet at the top, an eluent outlet at the top, and a washing liquid inlet at the bottom. A first perforated plate is provided in the lower part of the washing vessel, and a second perforated plate is provided in the upper part. The second perforated plate can move back and forth along the axial direction of the washing vessel. A heat preservation device is installed on the washing vessel; and, The washing liquid circulation device, along the material transfer direction, includes a cooler, a solid-liquid separator, a washing liquid tank, a circulation pump, and a heater connected in sequence. The inlet of the cooler is connected to the washing liquid outlet through a connecting pipe, and the outlet of the heater is connected to the washing liquid inlet through a pipe.

2. The polysulfone particulate matter washing device as described in claim 1, characterized in that, The polysulfone particulate washing device also includes a telescopic rod, which is disposed on the washing tank and the bottom of the telescopic rod is connected to the second porous plate.

3. The polysulfone particulate matter washing device as described in claim 2, characterized in that, The telescopic rod is the piston rod of the hydraulic cylinder.

4. The polysulfone particulate matter washing device as described in claim 1, characterized in that, The connecting pipe is provided with a sampling port, and the sampling port is provided with a second control valve.

5. The polysulfone particulate matter washing device as described in claim 1, characterized in that, The heat preservation device includes a heat preservation jacket, which is disposed on the outer wall of the washing vessel. The lower part of the heat preservation jacket is provided with a heat exchange medium inlet, and the upper part is provided with a heat exchange medium outlet.

6. The polysulfone particulate matter washing device as described in claim 1, characterized in that, The diameter of the through holes on both the first porous plate and the second porous plate is less than 40 μm.

7. The polysulfone particulate matter washing device as described in claim 1, characterized in that, The bottom of the washing tank is also provided with a washing liquid discharge port, and a third control valve is provided on the washing liquid discharge port.

8. The polysulfone particulate matter washing device as described in claim 1, characterized in that, A discharge port is provided on the side wall of the washing vessel above the first perforated plate, and a fourth control valve is provided on the discharge port.

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