Efficient acetone washing production device and method for refining polyether-ether-ketone

The high-efficiency acetone washing process addresses inefficiencies in PEEK production by using a controlled temperature setup with multiple vessels and efficient filtration, reducing energy use and pipe blockages while enabling direct reuse of biphenyl sulfone, thereby enhancing production efficiency.

CN120306318AActive Publication Date: 2025-07-15JILIN HENGNUO TECHNOLOGY DEVELOPMENT CENTER (LLP)
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Patent Information

Application Number
CN202510461789.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-14
Publication Date
2025-07-15
Estimated Expiration
2045-04-14

AI Technical Summary

Technical Problem

The existing acetone washing process has many tanks, separated diphenyl sulfone needs to be cooled with a tablet and all of them need to be distilled before they can be put back into use. The diphenyl sulfone crystals are prone to block the pipeline, have low production efficiency, high energy consumption, and there is no device and method for efficient acetone washing according to the solubility of diphenyl sulfone in acetone solution at different temperatures.

Method used

A highly efficient acetone washing production device for polyether ether ketone purification is designed, including acetone washing kettle, filter, cooling crystal tank, acetone storage tank, centrifugal separation device and acetone delivery pump. By controlling the temperature of the acetone washing kettle and the temperature of the cooling crystal tank, combining multiple sets of acetone washing groups and multiple filters, an efficient acetone washing process is achieved.

Benefits of technology

The number of equipment and containers is reduced, diphenylsulfone crystal blockage is avoided, energy consumption is reduced, production safety and efficiency is improved, and acetone consumption is reduced.

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Abstract

The invention discloses an efficient acetone washing production device and method for refining polyether-ether-ketone, and belongs to the technical field of polyether-ether-ketone production. The efficient acetone washing production device comprises an acetone washing kettle, a filter, a cooling crystallization tank, an acetone storage tank, a centrifugal separation device and an acetone conveying pump. The efficient acetone washing production device and the efficient acetone washing production method are designed by utilizing known solubility curves and dissolution rate curves of diphenyl sulfone in an acetone solution at different temperatures. The device and the method for efficiently washing the acetone for refining the polyether-ether-ketone have the following advantages: 1) the process route is short, and few equipment and containers are used; 2) the acetone tank reserves less; 3) most of crystallized diphenyl sulfone does not need to be finely distilled; (4) blockage caused by diphenyl sulfone crystallization in the pipeline is avoided; 5) the refining amount of diphenyl sulfone is reduced, and the production energy consumption is greatly reduced; 6) the consumption of acetone is reduced.
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Description

Technical Field

[0001] The present invention belongs to the technical field of polyether ether ketone production, and particularly relates to an efficient acetone washing production device and method for refining polyether ether ketone. Background Art

[0002] As a special engineering plastic, polyether ether ketone is widely used in many fields such as aerospace, robotics, machinery, and medicine, and shows great development potential. The production of polyether ether ketone mainly includes two steps: polymerization reaction and refining. Refining means separating the solvent and by-products during polymerization from polyether ether ketone. Among them, the solvent diphenyl sulfone is usually leached with solvents such as acetone and ethanol, which is the first step of refining. Acetone has advantages such as low boiling point and low energy consumption compared to ethanol and is widely used. There are different methods for acetone washing and they have been applied to a certain extent. The literature [Wang Shujiang, Wang Zhe, Ma Lanxu. Leaching process of diphenyl sulfone in polyether ketone synthesis products [J]. Chemical Industry and Engineering, 2010, 27(6): 504 - 509. etc.] has detailed descriptions, and its process is as Figure 1 shown. In this acetone washing process, there are the following technical defects: 1), there are many acetone storage tanks, the process route is long, and the storage capacity of acetone tanks is large, increasing the safety risk at the production site. 2), the acetone washing temperature is high and the energy consumption is high; at the same time, when discharging, when the material temperature drops, diphenyl sulfone crystals appear in the pipeline, blocking the pipeline, resulting in a long production time and reduced production efficiency. 3), the direct reuse rate of diphenyl sulfone is low, the purification and distillation temperature is high, the processing volume is large, and the energy consumption is extremely high. 4), the production cycle is relatively long and the production efficiency is low. Therefore, there is an urgent need for a new technical solution in the existing technology to solve this problem.

[0003] The literature [Wang Shujiang, Dai Xun, Zhang Honggang. Research on the refining process of PEK [J]. Engineering Plastics Application, 2010(38)12: 35 - 38] discloses the solubility curve of diphenyl sulfone in acetone solution at different temperatures as Figure 2 shown, and the dissolution rate curve, as Figure 3 shown. From these two curves, it can be obtained that when acetone is heated to about 40 °C, the solubility of diphenyl sulfone is close to 750 g / L, and when it is cooled to about 20 °C, the solubility drops to 120 g / L, and its dissolution rate is a little more than 1 h. In production, the acetone washing solution is heated to 40 °C and the treatment time is 1 h. At this time, 80% of the diphenyl sulfone in the polyether ether ketone particles enters the acetone solution, and the diphenyl sulfone has not reached saturation. Therefore, when discharging, even if the temperature of the acetone solution drops slightly, there will be no precipitation of diphenyl sulfone, and the filter pipe will not be blocked. Moreover, when the acetone temperature drops by only 20 °C, the diphenyl sulfone content drops from 750 mg to 120 mg, that is, 59% of the diphenyl sulfone in the polyether ether ketone particles is separated. Currently, no method for acetone washing based on this characteristic has been proposed. Summary of the Invention

[0004] The technical problems to be solved by the present invention are as follows: to provide a high-efficiency acetone washing production device and method for refining polyetheretherketone, which are used to solve the problems that the existing acetone washing process uses many tanks, the diphenyl sulfone after separation needs to be cooled by a flaker, and all of it needs to be rectified before it can be reused. The diphenyl sulfone crystals are easy to block the pipeline, resulting in low production efficiency and high energy consumption; at present, there is no device and method for high-efficiency acetone washing according to the solubility of diphenyl sulfone in acetone solution at different temperatures proposed in the existing literature and other technical problems.

[0005] A high-efficiency acetone washing production device for refining polyetheretherketone includes at least one group of acetone washing units. Each acetone washing unit includes an acetone washing kettle, a filter, a cooling crystallization tank, an acetone storage tank, a centrifugal separation device, an acetone centrifugate temporary storage tank, and an acetone delivery pump. The outside of the acetone washing kettle is provided with a jacket, and a heat medium is introduced into the jacket to keep the temperature inside the acetone washing kettle within a set temperature range. The upper part of the acetone washing kettle is connected to a polyetheretherketone pellet buffer tank. The acetone washing kettle is also provided with an acetone inlet and a secondary washing liquid addition pipeline. The liquid outlet at the lower part of the acetone washing kettle is connected to the filter; the liquid outlet of the filter is connected to two pipelines through a tee. One of the pipelines is connected to the inlet of the centrifugal separation device, and the other pipeline is sequentially connected to the first inlet of the acetone storage tank and the cooling crystallization tank; the discharge port of the cooling crystallization tank is connected to the inlet of the centrifugal separation device; the discharge port of the cooling crystallization tank is connected to the inlet pipeline of the centrifugal separation device; the outlet of the centrifugal separation device is connected to the acetone centrifugate temporary storage tank; the input end of the acetone delivery pump is connected to the acetone centrifugate temporary storage tank through a pipeline, and the output end of the acetone delivery pump is connected to the secondary washing liquid addition pipeline; the lower outlet of the acetone storage tank is connected to the pipeline of the input end of the acetone delivery pump, and the second inlet provided at the upper part of the acetone storage tank is connected to the pipeline of the output end of the acetone delivery pump through a pipeline; valves are provided at the inlet and outlet ends of the acetone storage tank, the cooling crystallization tank, and the acetone washing kettle.

[0006] The upper part of the acetone washing kettle is also connected with a heat exchanger, which receives the vaporized acetone in the acetone washing kettle and condenses and returns it to the acetone washing kettle.

[0007] The outside of the heat exchanger is provided with a heat exchange jacket; cold water or cold air is introduced into the heat exchange jacket.

[0008] Heating steam is introduced into the jacket provided outside the acetone washing kettle to keep the temperature of the acetone solution in the acetone washing kettle at 35°C to 45°C.

[0009] A stirring part is arranged in the acetone washing kettle; the stirring motor connected to the stirring part is arranged outside the acetone washing kettle.

[0010] The outside of the cooling crystallization tank is provided with a condensation jacket; cold water or cold air is introduced into the condensation jacket to keep the temperature inside the cooling crystallization tank at 10°C to 15°C.

[0011] A stirring part I is arranged inside the cooling and crystallization tank; a stirring motor I connected to the stirring part I is arranged outside the cooling and crystallization tank.

[0012] The number of acetone storage tanks in each acetone washing group is more than two, and the acetone washing solutions separated in the previous acetone washings are respectively stored in the acetone storage tanks.

[0013] The number of filters in each acetone washing group is more than two, and the more than two filters are arranged in parallel to prevent the filters from being blocked during the filtering process, which affects the discharging and slows down the discharging progress.

[0014] An efficient acetone washing production method for refining polyether ether ketone, using the efficient acetone washing production device for refining polyether ether ketone as described above, includes the following steps, and the following steps are carried out sequentially:

[0015] Step 1: The crushed polyether ether ketone material is buffered and decelerated in the polyether ether ketone pellet buffer tank. The stirring motor of the acetone washing kettle is started, and an acetone solution is added into the acetone washing kettle through the acetone adding port. The valve between the polyether ether ketone pellet buffer tank and the acetone washing kettle is opened, so that the polyether ether ketone pellets flow into the acetone washing kettle.

[0016] Step 2: A heat medium is introduced into the jacket of the acetone washing kettle to make the temperature of the acetone solution in the kettle reach and be maintained at 35°C to 45°C, and stirring is continued for a set time. The bottom discharging valve of the acetone washing kettle is opened, and the acetone solution containing a small amount of diphenyl sulfone in the kettle enters the cooling and crystallization tank through filtration and is cooled at 10°C to 15°C.

[0017] Step 3: The stirring motor I arranged on the cooling and crystallization tank is started. After the acetone solution containing a small amount of diphenyl sulfone entering the cooling tank is cooled for 10 min to 15 min, diphenyl sulfone crystallizes. Under the stirring action, the crystallized diphenyl sulfone particles are in a dispersed flocculent state, which is beneficial to the separation of acetone and diphenyl sulfone.

[0018] Step 4: The bottom valve of the cooling and crystallization tank is opened, and the liquid material in Step 3 is put into the centrifugal separation device to separate diphenyl sulfone and the acetone solution containing a small amount of diphenyl sulfone. The diphenyl sulfone is taken out and put into a dryer for drying and waiting to be recycled. The acetone solution containing a small amount of diphenyl sulfone is discharged into the acetone centrifugate temporary storage tank, and then pumped into the first acetone storage tank through an acetone delivery pump for later use.

[0019] Step 5: Through observation through the window, when the acetone in the acetone washing kettle is completely discharged, the discharging valve at the bottom of the acetone washing kettle is closed, and an acetone solution is added into the acetone washing kettle through the acetone adding port. Repeat Steps 2 to 4 to carry out the second acetone wash and discharge the acetone solution containing a small amount of diphenyl sulfone into the acetone centrifugate temporary storage tank, and then pump it into the second acetone storage tank through an acetone delivery pump.

[0020] Step 6. Through observation, when the acetone in the acetone washing kettle is drained completely, close the discharging valve at the bottom of the acetone washing kettle. Then, add the acetone solution containing a small amount of diphenyl sulfone in the first acetone storage tank into the acetone washing kettle via the secondary washing liquid adding pipeline by means of an acetone transfer pump. Repeat Steps 2 to 4 to conduct the third acetone washing. After passing through the cooling crystallization tank and the centrifugal separation device, pump the acetone solution containing a small amount of diphenyl sulfone discharged into the acetone centrifugate storage tank into the first acetone storage tank by means of an acetone transfer pump for later use.

[0021] Step 7. Through observation, when the acetone in the acetone washing kettle is drained completely, close the discharging valve at the bottom of the acetone washing kettle. Then, add the acetone solution containing a small amount of diphenyl sulfone in the second acetone storage tank into the acetone washing kettle via the secondary washing liquid adding pipeline by means of an acetone transfer pump. Repeat Steps 2 to 4 to conduct the fourth acetone washing. After passing through the cooling crystallization tank and the centrifugal separation device, pump the acetone solution containing a small amount of diphenyl sulfone discharged into the acetone centrifugate storage tank into the second acetone storage tank by means of an acetone transfer pump for later use.

[0022] Step 8. Repeat Step 6 and Step 7 at least once. In the last remaining set number of acetone washings, alternately pump the acetone solutions containing a small amount of diphenyl sulfone in the first acetone storage tank and the second acetone storage tank into the acetone washing kettle. After the acetone washing for the set time, the acetone solution containing a small amount of diphenyl sulfone discharged is filtered through a filter and then directly enters the centrifugal separation device and the acetone centrifugate storage tank, and then is stored in the first acetone storage tank and the second acetone storage tank for subsequent acetone washings until the acetone solutions containing a small amount of diphenyl sulfone obtained in the last two acetone washings are respectively stored in the first acetone storage tank and the second acetone storage tank, waiting to be used for the acetone washing in the next cycle.

[0023] Step 9. Take out the polyether ether ketone obtained in the last acetone washing, put it into a centrifugal separator, spin off the acetone, and then transport it to a water washing kettle for water washing and air drying to obtain the refined polyether ether ketone.

[0024] Through the above design scheme, the present invention can bring the following beneficial effects:

[0025] The high efficiency described in the present invention has two meanings. One is that the running route of acetone is short, and the washing liquid after acetone washing can be used as the next refining solvent after crystallization separation; the other is that the separated diphenyl sulfone can be directly recycled, avoiding its large-scale rectification and generating a large amount of energy consumption. The design basis of the method disclosed in the present invention is the solubility curve and dissolution rate curve of diphenyl sulfone in an acetone solution at different temperatures as shown in Figure 2 and Figure 3 shown.

[0026] As can be seen from the method disclosed by the present invention, multiple groups of acetone washing units can be set up in the workshop. With fewer storage tanks used and lower acetone reserves, the production safety is higher. The diphenyl sulfone obtained by cooling crystallization can be directly put into the polymerization kettle as a solvent for reaction after drying. At the same time, to a certain extent, the quantity of diphenyl sulfone for rectification recovery is reduced, the energy consumption is lowered, and the recovery cost is decreased. During the acetone washing at about 40°C for 40 minutes, about 75% of the diphenyl sulfone in the polyether ether ketone particles has been dissolved in the acetone, far from reaching the saturation level. Even when the temperature is lowered to 30°C, no diphenyl sulfone crystallization will occur, completely avoiding the problems of diphenyl sulfone crystallization when discharging acetone, clogging the pipeline, and reducing the filtration efficiency. After discharging the acetone-washed material, a large amount of acetone is contained between the polyether ether ketone particles. After centrifugal separation, the acetone is separated out, preventing it from entering the water during the water washing process and reducing the acetone consumption by about 15%.

[0027] It can be further concluded from this that the high-efficiency acetone washing production device and method for refining polyether ether ketone disclosed by the present invention have the following advantages: 1) The process route is short, and fewer equipment and containers are used; 2) The storage capacity of the acetone tank is small; 3) Most of the crystallized diphenyl sulfone does not require rectification; 4) Avoid clogging caused by diphenyl sulfone crystallization in the pipeline; 5) The refined quantity of diphenyl sulfone is reduced, and the production energy consumption is greatly lowered; 6) The acetone consumption is reduced. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] The present invention will be further described below in conjunction with the drawings and specific embodiments:

[0029] Figure 1 It is a schematic diagram of the device for the leaching process of diphenyl sulfone in the polyether ketone synthesis product in the existing literature;

[0030] Figure 2 It is a solubility curve diagram of diphenyl sulfone in acetone solution at different temperatures;

[0031] Figure 3 It is a dissolution rate curve diagram of diphenyl sulfone in acetone solution at different temperatures;

[0032] Figure 4 It is a schematic diagram of the device in the embodiment of the high-efficiency acetone washing production device and method for refining polyether ether ketone of the present invention;

[0033] Figure 5 It is a schematic diagram of the structure of the cooling crystallization tank in the high-efficiency acetone washing production device and method for refining polyether ether ketone of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0034] Figure 1 In it, R101 is a traditional acetone washing kettle, R102 is an evaporation kettle, C101 is a traditional heat exchanger, and A, B, C, D, and E are acetone storage tanks arranged in sequence.

[0035] Figure 3 In it, line 1 is the dissolution rate curve of diphenyl sulfone in an acetone solution at 25 °C, line 2 is the dissolution rate curve of diphenyl sulfone in an acetone solution at 40 °C, and line 3 is the dissolution rate curve of diphenyl sulfone in an acetone solution at 56 °C.

[0036] Example

[0037] Taking the setting of two groups of acetone washing groups in the workshop as an example, a high-efficiency acetone washing production device and method for refining polyether ether ketone of the present invention will be further described.

[0038] Considering from the aspects of equipment layout and floors, the first floor of the workshop has a larger space, the second floor is relatively compact, and there are more equipment on the third floor. The workshop is set as a three-story non-equal-height building. The height of the third floor is 2 meters higher than that of the first and second floors.

[0039] As Figure 4 shown, in the two groups of acetone washing groups, the polyether ether ketone pellet buffer tanks are respectively represented by LLG-101 and LLG-102, the acetone washing kettles are respectively represented by BTXG-101 and BTXG-1102; the heat exchangers are respectively represented by HG-101 and HG-102, the filters are respectively represented by GL-1, GL-2, GL-3, GL-4, GL-5, and GL-6, and the filtration size is 5 μm; the cooling crystallization tanks are respectively represented by LQG-101 and LQG-102. To ensure the smooth discharge of the crystallization product, a stirring device is set up in the cooling crystallization tank. The acetone storage tanks are respectively represented by CG-101, CG-102 and CG-103, CG-104; the centrifugal separation devices are respectively represented by LX-101 and LX-102, and the acetone centrifugate temporary storage tanks are respectively represented by ZCG-101 and ZCG-102; the acetone transfer pumps are respectively represented by B-101 and B-102.

[0040] In addition, the materials are directly discharged from the acetone washing kettles BTXG-101 and BTXG-102 into the cooling crystallization tanks LQG-101 and LQG-102 without the need for pump transportation; and they are also discharged from the cooling crystallization tanks LQG-101 and LQG-102 into the centrifugal separation devices LX-101 and LX-102 without the need for pump transportation.

[0041] A high-efficiency acetone washing production method for refining polyether ether ketone includes the following steps, and the following steps are carried out sequentially:

[0042] Step 1: The pulverized polyetheretherketone materials are evenly transported by air flow to the polyetheretherketone pellet buffer tanks LLG-101 and LLG-102 in the refining workshop. Acetone is pumped into the acetone washing kettles BTXG-101 and BTXG-102 respectively. The stirring motors of the two acetone washing kettles are started, and the discharging valves of the polyetheretherketone pellet buffer tanks are opened to allow the granular polyetheretherketone to flow into the corresponding acetone washing kettles. Note: Do not add the granular material first to prevent the failure of starting the stirring.

[0043] Step 2: Heating steam is introduced into the jackets of the acetone washing kettles BTXG-101 and BTXG-102 to raise the temperature of the acetone solution in the kettles to 40°C and maintain this temperature. After 40 minutes, the bottom discharging valves of the acetone washing kettles BTXG-101 and BTXG-102 are opened, and the acetone solutions containing a small amount of diphenyl sulfone in the kettles respectively enter the corresponding cooling and crystallization tanks LQG-101 and LQG-102 through the filters GL-1, GL-2, GL-3 and GL-4, GL-5, GL-6 for cooling.

[0044] The filters GL-1, GL-2, GL-3 and GL-4, GL-5, GL-6 are three independent filters corresponding to BTXG-101 and BTXG-102 respectively, which can prevent the filters from being blocked during the filtering process, affecting the discharging and slowing down the discharging progress.

[0045] The cooling of the cooling and crystallization tanks LQG-101 and LQG-102 can adopt Figure 5 the coiled cooling method to accelerate the cooling speed. Before November to May in winter in the north, external air is used for cooling and crystallization, and cooling water is used for cooling from May to November.

[0046] Step 3: When it is observed through the viewing window that the acetone in the acetone washing kettles BTXG-101 and BTXG-102 is almost drained, the discharging valves at the bottoms of the two kettles are closed, and the same amount of acetone is injected into the above-mentioned acetone washing kettles BTXG-101 and BTXG-102 again for the second acetone washing.

[0047] Step 4: After the acetone solutions containing a small amount of diphenyl sulfone entering the cooling and crystallization tanks LQG-101 and LQG-102 are cooled, diphenyl sulfone quickly crystallizes. This liquid material is put into the centrifugal separation devices LX-101 and LX-102 to separate diphenyl sulfone and the acetone solutions containing a small amount of diphenyl sulfone. Diphenyl sulfone enters the dryer for drying, and the acetone solutions are respectively pumped into the acetone storage tanks CG-101 and CG-104 through the acetone transfer pumps B-101 and B-102, waiting to enter the acetone washing kettles BTXG-101 and BTXG-102 again for acetone washing.

[0048] Specifically, when the acetone solution containing diphenyl sulfone enters the condensation tank, diphenyl sulfone rapidly crystallizes. Under the action of stirring, the crystallized diphenyl sulfone particles are in a dispersed flocculent state, rather than large chunks or large flakes of crystals. This is very conducive to separating the acetone therein and is more conducive to the reuse of diphenyl sulfone as a solvent during polymerization. This is also the greatest advantage of this process.

[0049] Step 5: The acetone solution containing a small amount of diphenyl sulfone from the secondary acetone wash is discharged into the emptied cooling and crystallization tanks LQG-101 and LQG-102 for cooling and crystallization. Similarly, separation is carried out through the centrifugal separation devices LX-101 and LX-102. The separated acetone solution is temporarily stored in the acetone centrifugate temporary storage tanks ZCG-101 and ZCG-102, and then pumped into the acetone storage tanks CG-102 and CG-103 respectively through the acetone transfer pumps B-101 and B-102 as raw materials for the third acetone wash.

[0050] After the crystallized diphenyl sulfone is centrifugally separated by the centrifugal separation devices LX-101 and LX-102, it all enters the diphenyl sulfone recovery tank. Since the mother liquor after rectification has more impurities, the crystallized diphenyl sulfone at this time cannot be directly reused in the polymerization reaction and can be used as a polymerization solvent after rectification.

[0051] Step 6: Observe that the acetone in the acetone wash kettles BTXG-101 and BTXG-102 is drained, then close the discharge valves at the bottom of the acetone wash kettles. The acetone solution containing a small amount of diphenyl sulfone in the acetone storage tanks CG-101 and CG-104 is added to the acetone wash kettles BTXG-101 and BTXG-102 through the acetone transfer pumps B-101 and B-102 via the secondary wash liquid addition pipeline for the third acetone wash. Similarly, after cooling crystallization and centrifugal separation, the acetone solution containing a small amount of diphenyl sulfone in the acetone centrifugate temporary storage tanks ZCG-101 and ZCG-102 is pumped into the acetone storage tanks CG-101 and CG-104 for standby.

[0052] Step 7: Observe that the acetone in the acetone wash kettles BTXG-101 and BTXG-102 is drained, then close the discharge valves at the bottom of the acetone wash kettles. The acetone solution containing a small amount of diphenyl sulfone in the acetone storage tanks CG-102 and CG-103 is added to the acetone wash kettles through the acetone transfer pumps via the secondary wash liquid addition pipeline for the fourth acetone wash. After passing through the cooling crystallization tank and the centrifugal separation devices LX-101 and LX-102, the acetone solution containing a small amount of diphenyl sulfone discharged into the acetone centrifugate temporary storage tanks ZCG-101 and ZCG-102 is pumped into the acetone storage tanks CG-102 and CG-103 through the acetone transfer pumps B-101 and B-102 for standby.

[0053] Step 8: Repeat Steps 6 and 7 once more. Respectively store the acetone solutions containing a small amount of diphenyl sulfone after cooling, crystallization, and centrifugal separation in acetone storage tanks CG-101, CG-104, and CG-102, CG-103.

[0054] Step 9: For the remaining acetone washes, pump the acetone solutions containing a small amount of diphenyl sulfone in acetone storage tanks CG-101, CG-104, and CG-102, CG-103 into acetone washing kettles BTXG-101 and BTXG-102 in two batches for 40 minutes of acetone washing. Then, the discharged acetone solutions containing a small amount of diphenyl sulfone are filtered through filters GL-1, GL-2, GL-3 and GL-4, GL-5, GL-6. Instead of entering cooling and crystallization tanks LQG-101 and LQG-102, they directly enter acetone centrifugate temporary storage tanks ZCG-101 and ZCG-102 through centrifugal separation devices LX-101 and LX-102 as transfer channels. Then, they are respectively pumped into acetone storage tanks CG-101, CG-104, and CG-102, CG-103 through acetone transfer pumps B-101 and B-102. After the last two acetone washes, when the acetone solutions containing a small amount of diphenyl sulfone are stored in acetone storage tanks CG-101, CG-104, and CG-102, CG-103, they are not discharged and wait to be used for the acetone wash in the next cycle to respectively replace the acetone solutions in the first two times.

[0055] Step 10: The polyether ether ketone obtained from the last acetone wash is directly placed in centrifugal separation devices LX-101 and LX-102. After the acetone is centrifuged out, it is transported to a water washing kettle for water washing and drying to obtain refined polyether ether ketone.

[0056] In the present invention, after the acetone solution containing diphenyl sulfone is cooled, diphenyl sulfone quickly crystallizes to form fine particles. After separation and drying, diphenyl sulfone can directly enter the polymerization process and be reused as a polymerization solvent, reducing the energy-consuming process that requires rectification before use. At the same time, the separated acetone can also be returned to the acetone washing kettle for another acetone wash. This saves the consumption of acetone, reduces the storage volume of the acetone tank, shortens the process to the greatest extent, and saves energy.

Claims

1. An efficient acetone washing production device for the refinement of polyether ether ketone, characterized in that: It includes at least one set of acetone washing group, and the acetone washing group includes an acetone washing kettle, a filter, a cooling crystallization tank, an acetone storage tank, a centrifugal separation device, an acetone centrifugate temporary storage tank and an acetone transfer pump. A jacket is arranged outside the acetone washing kettle, and a heat medium is introduced into the jacket to keep the temperature inside the acetone washing kettle within a set temperature range. The upper part of the acetone washing kettle is connected to a polyether ether ketone pellet buffer tank. An acetone inlet and a secondary washing liquid adding pipeline are also arranged on the acetone washing kettle. The liquid outlet at the lower part of the acetone washing kettle is connected to the filter; the liquid outlet of the filter is connected to two pipelines through a tee. One of the pipelines is connected to the inlet of the centrifugal separation device, and the other pipeline is sequentially connected to the first inlet of the acetone storage tank and the cooling crystallization tank; the discharge port of the cooling crystallization tank is connected to the inlet of the centrifugal separation device; the discharge port of the cooling crystallization tank is connected to the inlet pipeline of the centrifugal separation device; the outlet of the centrifugal separation device is connected to the acetone centrifugate temporary storage tank; the input end of the acetone transfer pump is connected to the acetone centrifugate temporary storage tank through a pipeline, and the output end of the acetone transfer pump is connected to the secondary washing liquid adding pipeline; the lower outlet of the acetone storage tank is connected to the pipeline at the input end of the acetone transfer pump, and the second inlet arranged at the upper part of the acetone storage tank is connected to the pipeline at the output end of the acetone transfer pump through a pipeline; valves are arranged at the inlets and outlets of the acetone storage tank, the cooling crystallization tank and the acetone washing kettle.

2. The high-efficiency acetone washing production device for refining polyether ether ketone according to claim 1, characterized in that: A heat exchanger is also connected to the upper part of the acetone washing kettle, and the heat exchanger receives the vaporized acetone in the acetone washing kettle and condenses and returns it to the acetone washing kettle.

3. The high-efficiency acetone washing production device for refining polyether ether ketone according to claim 1 is characterized in that: A heat exchange jacket is arranged outside the heat exchanger; cold water or cold air is introduced into the heat exchange jacket.

4. An efficient acetone washing production device for refining polyetheretherketone according to claim 1, characterized in that: Heating steam is introduced into the jacket arranged outside the acetone washing kettle to keep the temperature of the acetone solution in the acetone washing kettle at 35°C to 45°C.

5. The high-efficiency acetone washing production device for refining polyetheretherketone according to claim 1, characterized in that: A stirring part is arranged in the acetone washing kettle; the stirring motor connected to the stirring part is arranged outside the acetone washing kettle.

6. The high-efficiency acetone washing production device for refining polyether ether ketone according to claim 1, characterized in that: A condensation jacket is arranged outside the cooling crystallization tank; cold water or cold air is introduced into the condensation jacket to keep the temperature inside the cooling crystallization tank at 10°C to 15°C.

7. The high-efficiency acetone washing production device for refining polyether ether ketone according to claim 1, characterized in that: A stirring part I is arranged inside the cooling crystallization tank; the stirring motor I connected to the stirring part I is arranged outside the cooling crystallization tank.

8. The high-efficiency acetone washing production device for refining polyether ether ketone according to claim 1, wherein: The number of acetone storage tanks in each acetone washing group is more than two, and the acetone washing liquid separated from the previous acetone washings is respectively stored in the acetone storage tanks.

9. The high-efficiency acetone washing production device for refining polyether ether ketone according to claim 1, wherein: The number of filters in each acetone washing group is more than two, and more than two filters are arranged in parallel to prevent the filters from being blocked during the filtering process, affecting the discharging and slowing down the discharging progress.

10. A high-efficiency acetone washing production method for refining polyetheretherketone, using the high-efficiency acetone washing production device for refining polyetheretherketone described in claim 1, characterized in that: It includes the following steps, and the following steps are carried out sequentially: Step 1: The pulverized polyether ether ketone material is buffered and decelerated in the polyether ether ketone pellet buffer tank. The stirring motor of the acetone washing kettle is started, and an acetone solution is added into the acetone washing kettle through the acetone inlet. The valve between the polyether ether ketone pellet buffer tank and the acetone washing kettle is opened to allow the polyether ether ketone pellets to flow into the acetone washing kettle; Step 2: Introduce a heat medium into the jacket of the acetone washing kettle to raise the temperature of the acetone solution in the kettle to 35°C - 45°C and maintain it. Continuously stir for a set time, then open the bottom discharge valve of the acetone washing kettle. The acetone solution containing a small amount of diphenyl sulfone in the kettle is filtered through a filter and enters the cooling crystallization tank for cooling at 10°C - 15°C. Step 3: Start the stirring motor I installed on the cooling crystallization tank. After the acetone solution containing a small amount of diphenyl sulfone in the cooling tank has been cooled for 10 - 15 minutes, diphenyl sulfone crystallizes. Under the action of stirring, the crystallized diphenyl sulfone particles are in a dispersed flocculent state, which is conducive to the separation of acetone and diphenyl sulfone. Step 4: Open the bottom valve of the cooling crystallization tank to discharge the liquid in Step 3 into the centrifugal separation device to separate diphenyl sulfone and the acetone solution containing a small amount of diphenyl sulfone. The separated diphenyl sulfone is taken out and put into a dryer for drying and recycling. The acetone solution containing a small amount of diphenyl sulfone is discharged into the acetone centrifugate temporary storage tank and then pumped into the first acetone storage tank by an acetone transfer pump for later use. Step 5: Observe through the viewing window. When the acetone in the acetone washing kettle has been completely discharged, close the bottom discharge valve of the acetone washing kettle. Add an acetone solution into the acetone washing kettle through the acetone inlet. Repeat Steps 2 to 4 for the second acetone washing and discharge the acetone solution containing a small amount of diphenyl sulfone into the acetone centrifugate temporary storage tank, then pump it into the second acetone storage tank by an acetone transfer pump. Step 6: Observe. When the acetone in the acetone washing kettle has been completely discharged, close the bottom discharge valve of the acetone washing kettle. Pump the acetone solution containing a small amount of diphenyl sulfone in the first acetone storage tank into the acetone washing kettle through the acetone transfer pump via the secondary washing solution adding pipeline. Repeat Steps 2 to 4 for the third acetone washing. After passing through the cooling crystallization tank and the centrifugal separation device, pump the acetone solution containing a small amount of diphenyl sulfone discharged into the acetone centrifugate temporary storage tank into the first acetone storage tank by an acetone transfer pump for later use. Step 7: Observe. When the acetone in the acetone washing kettle has been completely discharged, close the bottom discharge valve of the acetone washing kettle. Pump the acetone solution containing a small amount of diphenyl sulfone in the second acetone storage tank into the acetone washing kettle through the acetone transfer pump via the secondary washing solution adding pipeline. Repeat Steps 2 to 4 for the fourth acetone washing. After passing through the cooling crystallization tank and the centrifugal separation device, pump the acetone solution containing a small amount of diphenyl sulfone discharged into the acetone centrifugate temporary storage tank into the second acetone storage tank by an acetone transfer pump for later use. Step 8: Repeat Steps 6 and 7 at least once. In the last remaining set number of acetone washings, alternately pump the acetone solutions containing a small amount of diphenyl sulfone in the first acetone storage tank and the second acetone storage tank into the acetone washing kettle. After the acetone washing for the set time, the discharged acetone solution containing a small amount of diphenyl sulfone is filtered through a filter and directly enters the centrifugal separation device and the acetone centrifugate temporary storage tank, and then is stored in the first acetone storage tank and the second acetone storage tank for subsequent acetone washings until the acetone solutions containing a small amount of diphenyl sulfone obtained from the last two acetone washings are respectively stored in the first acetone storage tank and the second acetone storage tank, waiting to be used for the next cycle of acetone washing. Step 9: Take out the polyether ether ketone obtained after the last acetone wash, put it into a centrifuge, spin out the acetone, and then transport it to a water-washing kettle for water washing and air drying to obtain refined polyether ether ketone.

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