A polyether ether ketone refined high-efficiency acetone washing production device and method

CN120306318BActive Publication Date: 2026-09-18JILIN HENGNUO TECHNOLOGY DEVELOPMENT CENTER (LLP)
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Patent Information

Application Number
CN202510461789.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-04-14
Publication Date
2026-09-18
Estimated Expiration
2045-04-14

AI Technical Summary

Technical Problem

[0004]本发明所要解决的技术问题是:提供一种聚醚醚酮精制的高效丙酮洗生产装置及方法用于解决现有的丙酮洗工艺使用的罐多,分离后的二苯砜需用结片机冷却,还要全部进行精馏才能重新投入使用,二苯砜结晶物容易堵塞管路,生产效率低、能耗高;目前还没有根据已有文献提出的不同温度下二苯砜在丙酮溶液中的溶解度进行高效丙酮洗的装置和方法等技术问题

Benefits of technology

[0025] The high efficiency described in this invention has two aspects: first, the acetone operating route is short, and the washing liquid after acetone washing can be used as a solvent for the next purification after crystallization separation; second, the separated diphenyl sulfone can be directly recycled, avoiding large-scale distillation and the resulting high energy consumption. The method disclosed in this invention is designed based on the following... Figure 2 and Figure 3 The solubility curves and dissolution rate curves of diphenyl sulfone in acetone solution at different temperatures are shown.

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Abstract

The application relates to a polyether ether ketone refined high-efficiency acetone washing device and method, and belongs to the technical field of polyether ether ketone production, which 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 high-efficiency acetone washing device and method are designed by using known solubility curves and dissolution speed curves of diphenyl sulfone in acetone solutions at different temperatures. The high-efficiency acetone washing device and method have the following advantages: 1) a short process route and less equipment and containers are used; 2) the acetone tank has a small storage capacity; 3) most of the crystallized diphenyl sulfone does not need to be refined; 4) the blockage caused by the crystallization of diphenyl sulfone in pipelines is avoided; 5) the refined amount of diphenyl sulfone is reduced, and the production energy consumption is greatly reduced; and 6) the acetone consumption is reduced.
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Description

Technical Field

[0001] This invention belongs to the field of polyether ether ketone (PEEK) production technology, and in particular relates to a high-efficiency acetone washing production apparatus and method for purifying PEEK. Background Technology

[0002] Polyetheretherketone (PEEK), as a special engineering plastic, is widely used in aerospace, robotics, machinery, medical and other fields, and has shown great development potential. The production of PEEK mainly involves two steps: polymerization and refining. Refining refers to separating the solvent and byproducts from the PEEK during polymerization. Diphenyl sulfone, the solvent, is usually leached using acetone or ethanol, which is the first step in refining. Acetone is widely used due to its lower boiling point and lower energy consumption compared to ethanol. There are different methods for acetone washing, and they have been applied to some extent. The literature [Wang Shujiang, Wang Zhe, Ma Lanxu, leaching process of diphenyl sulfone in PEEK synthesis products [J]. Chemical Industry and Engineering, 2010, 27(6): 504-509, etc.] provides a detailed description of the process, such as... Figure 1 As shown, this acetone washing process has the following technical drawbacks: 1) Multiple acetone storage tanks, a long process route, and large acetone storage capacity increase safety risks at the production site. 2) High acetone washing temperature leads to high energy consumption; simultaneously, during discharge, as the material temperature decreases, diphenyl sulfone crystals appear in the pipelines, clogging them, resulting in long production times and reduced production efficiency. 3) The direct reuse rate of diphenyl sulfone is low, purification and distillation temperatures are high, and the processing volume is large, leading to extremely high energy consumption. 4) The production cycle is relatively long, resulting in low production efficiency. Therefore, a new technical solution is urgently needed to address these issues.

[0003] The literature [Wang Shujiang, Dai Xun, Zhang Honggang. Research on refining process of PEK [J]. Engineering Plastics Application, 2010(38)12:35-38] discloses the solubility curves of diphenyl sulfone in acetone solution at different temperatures, as shown in the figure. Figure 2 As shown, and the dissolution rate curve, as... Figure 3 As shown in the figures, these two curves reveal that when acetone is heated to approximately 40°C, its diphenyl sulfone solubility is close to 750 g / L, while when cooled to approximately 20°C, the solubility drops to 120 g / L, with a dissolution rate of slightly over 1 hour. In production, the acetone washing solution is heated to 40°C for 1 hour. At this point, 80% of the diphenyl sulfone in the polyetheretherketone (PEEK) particles enters the acetone solution, and since the diphenyl sulfone content is not yet saturated, even if the acetone solution temperature decreases slightly during discharge, no diphenyl sulfone will precipitate, preventing clogging of the filter tube. Furthermore, a mere 20°C temperature drop in acetone is sufficient to reduce the diphenyl sulfone content from 750 mg to 120 mg, meaning that 59% of the diphenyl sulfone in the PEEK particles is separated. Currently, no method for acetone washing based on this characteristic has been proposed. Summary of the Invention

[0004] The technical problem to be solved by this invention is to provide a high-efficiency acetone washing production device and method for refining polyetheretherketone (PEEK) to address the problems of existing acetone washing processes that use multiple tanks, require cooling of separated diphenyl sulfone using a flocculant, and necessitate complete distillation before reuse, and where diphenyl sulfone crystals easily clog pipelines, resulting in low production efficiency and high energy consumption; and the lack of a device and method for high-efficiency acetone washing based on the solubility of diphenyl sulfone in acetone solution at different temperatures as proposed in existing literature.

[0005] A high-efficiency acetone washing production device for polyetheretherketone (PEEK) refining includes at least one acetone washing assembly. Each assembly comprises an acetone washing kettle, a filter, a cooling crystallization tank, an acetone storage tank, a centrifugal separator, an acetone centrifugal liquid storage tank, and an acetone transfer pump. The acetone washing kettle is externally jacketed, through which a heating medium is circulated to maintain the temperature within a set range. The upper part of the acetone washing kettle is connected to a PEEK granular buffer tank. The acetone washing kettle also has an acetone inlet and a secondary washing liquid inlet pipeline. The lower outlet of the acetone washing kettle is connected to a filter. The outlet of the filter is connected to two pipelines via a T-junction. One pipeline connects to the inlet of the centrifugal separator, and the other pipeline is sequentially connected to acetone... The acetone storage tank has a first inlet and a cooling crystallizer; the outlet of the cooling crystallizer is connected to the inlet of a centrifugal separator; the outlet of the cooling crystallizer is connected to the inlet pipe of the centrifugal separator; the outlet of the centrifugal separator is connected to an acetone centrifugal liquid storage tank; the input end of the acetone transfer pump is connected to the acetone centrifugal liquid storage tank via a pipe, and the output end of the acetone transfer pump is connected to a secondary washing liquid addition pipe; the lower outlet of the acetone storage tank is connected to the input pipe of the acetone transfer pump, and the upper second inlet of the acetone storage tank is connected to the output pipe of the acetone transfer pump via a pipe; valves are installed at the inlet and outlet ends of the acetone storage tank, the cooling crystallizer, and the acetone washing kettle.

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

[0007] The heat exchanger is provided with a heat exchange jacket on the outside; cold water or cold air is circulated in the heat exchange jacket.

[0008] Heating steam is introduced into the jacket outside the acetone washing tank to maintain the temperature of the acetone solution inside the tank at 35℃~45℃.

[0009] The acetone washing tank is equipped with a stirring section; the stirring motor connected to the stirring section is located outside the acetone washing tank.

[0010] The cooling crystallizer is equipped with a condensation jacket on the outside; cold water or cold air is circulated into the condensation jacket to maintain the temperature inside the cooling crystallizer at 10℃~15℃.

[0011] The cooling crystallization tank is equipped with a stirring section I inside; the stirring motor I connected to the stirring section I is located outside the cooling crystallization tank.

[0012] The number of acetone storage tanks in each acetone washing group is more than two, and the acetone storage tanks store the acetone washing liquid separated from the previous acetone washings.

[0013] The number of filters in each acetone washing group is more than two, and the two or more filters are set in parallel to prevent the filters from being blocked during the filtration process, which would affect the discharge and slow down the discharge progress.

[0014] A method for producing high-efficiency acetone wash from refined polyetheretherketone (PEEK) using the aforementioned high-efficiency acetone wash production apparatus includes the following steps, which are performed sequentially:

[0015] Step 1: The crushed polyether ether ketone material is buffered and decelerated in the polyether ether ketone granule buffer tank. The stirring motor of the acetone washing kettle is turned on, and acetone solution is added into the acetone washing kettle through the acetone inlet. The valve between the polyether ether ketone granule buffer tank and the acetone washing kettle is opened to allow the polyether ether ketone granules to flow into the acetone washing kettle.

[0016] Step 2: Introduce a heating medium into the jacket of the acetone washing kettle to raise and maintain the temperature of the acetone solution inside the kettle to 35℃~45℃. Stir continuously 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 then enters a cooling crystallization tank to be cooled at 10℃~15℃.

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

[0018] Step 4: Open the bottom valve of the cooling crystallization tank and put the liquid from Step 3 into the centrifugal separator to separate diphenyl sulfone and acetone solution containing a small amount of diphenyl sulfone. Take out the diphenyl sulfone and put it into the dryer to dry for recycling. The acetone solution containing a small amount of diphenyl sulfone is discharged into the acetone centrifugal liquid temporary storage tank and then pumped into the first acetone storage tank through the acetone transfer pump for later use.

[0019] Step 5: Observe through the viewing window. Once the acetone in the acetone washing kettle has been completely drained, close the discharge valve at the bottom of the acetone washing kettle. Add acetone solution into the acetone washing kettle through the acetone inlet. Repeat steps 2 to 4 to perform a second acetone wash and discharge the acetone solution containing a small amount of diphenyl sulfone into the acetone centrifuge temporary storage tank. Then, pump the solution into the second acetone storage tank through the acetone transfer pump.

[0020] Step 6: After observing that the acetone in the acetone washing kettle has been completely drained, close the discharge valve at the bottom of the acetone washing kettle. Add the acetone solution containing a small amount of diphenyl sulfone from the first acetone storage tank to the acetone washing kettle through the secondary washing liquid addition pipeline via the acetone transfer pump. Repeat steps 2 to 4 to perform the third acetone washing. After passing through the cooling crystallization tank and centrifugal separation device, pump the acetone solution containing a small amount of diphenyl sulfone discharged into the acetone centrifugal liquid temporary storage tank into the first acetone storage tank via the acetone transfer pump for later use.

[0021] Step 7: After observing that the acetone in the acetone washing kettle has been completely drained, close the discharge valve at the bottom of the acetone washing kettle. Add the acetone solution containing a small amount of diphenyl sulfone from the second acetone storage tank to the acetone washing kettle through the secondary washing liquid addition pipeline via the acetone transfer pump. Repeat steps 2 to 4 to perform the fourth acetone washing. After passing through the cooling crystallization tank and centrifugal separation device, pump the acetone solution containing a small amount of diphenyl sulfone discharged into the acetone centrifugal liquid temporary storage tank into the second acetone storage tank via the acetone transfer pump for later use.

[0022] Step 8: Repeat steps 6 and 7 at least once. During the last set number of acetone washes, alternately pump the acetone solution containing a small amount of diphenyl sulfone from the first and second acetone storage tanks into the acetone washing vessel. After the set acetone washing time, the acetone solution containing a small amount of diphenyl sulfone released is filtered and then directly enters the centrifuge and acetone centrifuge liquid storage tank. It is then stored in the first and second acetone storage tanks for subsequent acetone washes until the acetone solution containing a small amount of diphenyl sulfone obtained from the last two acetone washes is stored in the first and second acetone storage tanks respectively, waiting to be used for the next cycle of acetone washing.

[0023] Step 9: Take out the polyether ether ketone obtained from the last acetone wash, put it into a centrifuge to remove the acetone, and then transport it to a water washing tank for washing. After drying, you can 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 this invention has two aspects: first, the acetone operating route is short, and the washing liquid after acetone washing can be used as a solvent for the next purification after crystallization separation; second, the separated diphenyl sulfone can be directly recycled, avoiding large-scale distillation and the resulting high energy consumption. The method disclosed in this invention is designed based on the following... Figure 2 and Figure 3 The solubility curves and dissolution rate curves of diphenyl sulfone in acetone solution at different temperatures are shown.

[0026] As can be seen from the method disclosed in this invention, multiple acetone washing groups can be set up in the workshop, requiring fewer storage tanks, resulting in lower acetone storage and higher safety during production. The cooled and crystallized diphenyl sulfone, after drying, can be directly added to the polymerization reactor as a solvent during the reaction. Simultaneously, it reduces the amount of diphenyl sulfone recovered through distillation, lowering energy consumption and recovery costs. Acetone washing at approximately 40°C for 40 minutes dissolves about 75% of the diphenyl sulfone in the polyetheretherketone (PEEK) particles in the acetone, far from reaching saturation. Even when cooled to 30°C, no diphenyl sulfone crystals will precipitate, completely avoiding the problem of diphenyl sulfone crystallization during acetone discharge, which could clog pipelines and reduce filtration efficiency. After acetone washing, the PEEK particles contain a large amount of acetone. After centrifugation, the acetone is separated, preventing it from entering the water during the washing process and reducing acetone consumption by approximately 15%.

[0027] Therefore, it can be further concluded that the high-efficiency acetone washing production apparatus and method for refining polyetheretherketone disclosed in this invention has the following advantages: 1) Short process route, fewer equipment and containers used; 2) Small acetone tank storage capacity; 3) Most of the crystallized diphenyl sulfone does not need to be refined; 4) Avoids blockage caused by diphenyl sulfone crystallization in pipelines; 5) Reduced diphenyl sulfone refining amount, resulting in a significant reduction in production energy consumption; 6) Reduced acetone consumption. Attached Figure Description

[0028] The present invention will be further described below with reference to the accompanying drawings and specific embodiments:

[0029] Figure 1 This is a schematic diagram of the apparatus used for the leaching process of diphenyl sulfone in polyetherketone synthesis products, as described in existing literature.

[0030] Figure 2 The solubility curves of diphenyl sulfone in acetone solution at different temperatures are shown.

[0031] Figure 3 The graph shows the dissolution rate curves of diphenyl sulfone in acetone solution at different temperatures.

[0032] Figure 4 This is a schematic diagram of an embodiment of the high-efficiency acetone washing production apparatus and method for refining polyether ether ketone according to the present invention.

[0033] Figure 5 This is a schematic diagram of the cooling crystallization tank in a high-efficiency acetone washing production device and method for refining polyether ether ketone according to the present invention. Detailed Implementation

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

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

[0036] Example

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

[0038] Considering the equipment layout and floor plan, the first floor of the workshop has a larger space, the second floor is more compact, and the third floor has more equipment. Therefore, the workshop is designed as a three-story structure with different heights. The third floor is 2 meters higher than the first and second floors.

[0039] like Figure 4 As shown, in the two acetone washing groups, the polyetheretherketone (PEEK) granular material buffer tanks are represented by LLG-101 and LLG-102, respectively; the acetone washing kettles are represented by BTXG-101 and BTXG-1102, respectively; the heat exchangers are represented by HG-101 and HG-102, respectively; the filters are represented by GL-1, GL-2, GL-3, GL-4, GL-5, and GL-6, respectively, with a filter size of 5µm; and the cooling crystallization tanks are represented by LQG-101 and LQG-102, respectively. To ensure smooth discharge of crystals, a stirring device is installed in the cooling crystallization tank. Acetone storage tanks are designated as CG-101, CG-102 and CG-103, CG-104 respectively; centrifugal separation devices are designated as LX-101 and LX-102 respectively; acetone centrifugal liquid temporary storage tanks are designated as ZCG-101 and ZCG-102 respectively; and acetone transfer pumps are designated as B-101 and B-102 respectively.

[0040] In addition, materials can be directly transferred from acetone washing tanks BTXG-101 and BTXG-102 into cooling crystallization tanks LQG-101 and LQG-102 without the need for pumps; materials can also be transferred from cooling crystallization tanks LQG-101 and LQG-102 into centrifugal separators LX-101 and LX-102 without the need for pumps.

[0041] A highly efficient method for producing acetone wash from purified polyetheretherketone (PEEK) includes the following steps, which are performed sequentially:

[0042] Step 1: The pulverized polyetheretherketone (PEEK) material is evenly conveyed to the PEEK granule 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 discharge valves of the PEEK granule buffer tanks are opened to allow the granular PEEK to flow into the corresponding acetone washing kettles. Note: Do not add the granules first to prevent the stirring from failing to start.

[0043] Step 2: Introduce heating steam into the jackets of acetone washing reactors BTXG-101 and BTXG-102 to raise the temperature of the acetone solution inside the reactors to 40°C and maintain this temperature. After 40 minutes, open the bottom discharge valves of acetone washing reactors BTXG-101 and BTXG-102. The acetone solution containing a small amount of diphenyl sulfone in the reactors will then pass through filters GL-1, GL-2, GL-3 and GL-4, GL-5, GL-6 respectively into the corresponding cooling crystallization tanks LQG-101 and LQG-102 for cooling.

[0044] Filters GL-1, GL-2, GL-3, GL-4, GL-5, and GL-6 are three independent filters used in conjunction with BTXG-101 and BTXG-102, respectively, to prevent the filters from becoming clogged during the filtration process, which would affect the material discharge and slow down the discharge progress.

[0045] Cooling of cooling crystallization tanks LQG-101 and LQG-102 can be achieved by using... Figure 5 The coiled cooling method aims to accelerate the cooling speed. In northern regions, from November to May before winter, external air cooling is used for crystallization; from May to November, cooling water is used.

[0046] Step 3: Observe through the viewing window that the acetone in the acetone washing tanks BTXG-101 and BTXG-102 is almost completely drained, close the discharge valves at the bottom of the two tanks, and inject the same amount of acetone into the acetone washing tanks BTXG-101 and BTXG-102 again to perform a second acetone wash.

[0047] Step 4: After the acetone solution containing a small amount of diphenyl sulfone enters the cooling crystallization tanks LQG-101 and LQG-102, the diphenyl sulfone rapidly crystallizes. This solution is then placed into centrifugal separators LX-101 and LX-102 to separate the diphenyl sulfone and the acetone solution containing a small amount of diphenyl sulfone. The diphenyl sulfone is dried in a dryer, while the acetone solution is pumped into acetone storage tanks CG-101 and CG-104 via acetone transfer pumps B-101 and B-102, respectively, awaiting further acetone washing in acetone washing kettles BTXG-101 and BTXG-102.

[0048] It should be noted that when the acetone solution containing diphenyl sulfone enters the condenser, the diphenyl sulfone crystallizes rapidly. Under stirring, the crystallized diphenyl sulfone particles are dispersed and flocculent, rather than large lumps or flakes of crystals. This is very beneficial for separating the acetone and for reusing the diphenyl sulfone as a solvent during polymerization. This is the biggest advantage of this process.

[0049] Step 5: The acetone solution containing a small amount of diphenyl sulfone from the second acetone wash is discharged into empty cooling crystallization tanks LQG-101 and LQG-102 for cooling and crystallization. It is then separated by centrifugal separators LX-101 and LX-102. The separated acetone solution is temporarily stored in acetone centrifuge storage tanks ZCG-101 and ZCG-102, and then pumped into acetone storage tanks CG-102 and CG-103 respectively by acetone transfer pumps B-101 and B-102, serving as the raw material for the third acetone wash.

[0050] After being centrifuged by centrifuges LX-101 and LX-102, the crystallized diphenyl sulfone is sent to the diphenyl sulfone recovery tank. Because the mother liquor after distillation contains many impurities, the crystallized diphenyl sulfone cannot be directly reused in the polymerization reaction; however, it can be used as a polymerization solvent after further distillation.

[0051] Step 6: After observing that the acetone in acetone washing tanks BTXG-101 and BTXG-102 has been completely drained, close the discharge valve at the bottom of the acetone washing tanks. Add the acetone solution containing a small amount of diphenyl sulfone from acetone storage tanks CG-101 and CG-104 to acetone washing tanks BTXG-101 and BTXG-102 through the secondary washing liquid addition pipeline via acetone transfer pumps B-101 and B-102 for the third acetone wash. After cooling, crystallization, and centrifugation, pump the acetone solution containing a small amount of diphenyl sulfone from acetone centrifuge temporary storage tanks ZCG-101 and ZCG-102 into acetone storage tanks CG-101 and CG-104 for later use.

[0052] Step 7: After observing that the acetone in the acetone washing tanks BTXG-101 and BTXG-102 has been completely drained, close the discharge valve at the bottom of the acetone washing tanks. Add the acetone solution containing a small amount of diphenyl sulfone from the acetone storage tanks CG-102 and CG-103 to the acetone washing tanks via the secondary washing liquid addition pipeline through the acetone transfer pump for the fourth acetone wash. After passing through the cooling crystallization tanks and centrifugal separation devices LX-101 and LX-102, pump the acetone solution containing a small amount of diphenyl sulfone from the acetone centrifugal liquid temporary storage tanks ZCG-101 and ZCG-102 into the acetone storage tanks CG-102 and CG-103 through the acetone transfer pumps B-101 and B-102 for later use.

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

[0054] Step 9: The remaining acetone washes involve pumping the acetone solutions containing a small amount of diphenyl sulfone from acetone storage tanks CG-101, CG-104, CG-102, and CG-103 into acetone washing vessels BTXG-101 and BTXG-102 in two separate batches for 40 minutes each. The discharged acetone solution containing a small amount of diphenyl sulfone is then filtered through filters GL-1, GL-2, GL-3, GL-4, GL-5, and GL-6. Instead of entering the cooling crystallization tanks LQG-101 and LQG-102, it is centrifuged using centrifugal separator LX-10. 1. LX-102 serves as the transfer channel directly into the acetone centrifuge temporary storage tanks ZCG-101 and ZCG-102. Then, through acetone transfer pumps B-101 and B-102, the acetone is pumped into the acetone storage tanks CG-101 and CG-104, and CG-102 and CG-103, respectively. After the last two acetone washes, the acetone solution containing a small amount of diphenyl sulfone is stored in the acetone storage tanks CG-101, CG-104, CG-102, and CG-103 and is not released. It is reserved for use in the next cycle of acetone washes to replace the acetone solution from the previous two washes.

[0055] Step 10: The polyether ether ketone obtained from the final acetone wash is directly placed into centrifugal separators LX-101 and LX-102 to remove the acetone. Then, it is transported to a water washing tank for washing and drying to obtain the refined polyether ether ketone.

[0056] In this invention, the acetone solution containing diphenyl sulfone rapidly crystallizes upon cooling, forming fine particles. After separation and drying, the diphenyl sulfone can be directly used as a polymerization solvent, reducing the energy-intensive step of re-distillation. Simultaneously, the separated acetone can be returned to the acetone washing vessel for further acetone washing. This saves acetone consumption, reduces acetone tank inventory, shortens the process time, and conserves energy.

Claims

1. A high-efficiency acetone washing production apparatus for refining polyetheretherketone (PEEK), characterized in that: The system includes at least one acetone washing assembly, comprising an acetone washing vessel, a filter, a cooling crystallization tank, an acetone storage tank, a centrifugal separator, an acetone centrifugal liquid storage tank, and an acetone transfer pump. The acetone washing vessel has an external jacket through which a heating medium is circulated to maintain the temperature within a set range. The upper part of the acetone washing vessel is connected to a polyetheretherketone (PEEK) granular buffer tank. The acetone washing vessel also has an acetone inlet and a secondary washing liquid inlet pipeline. The lower outlet of the acetone washing vessel is connected to a filter. The outlet of the filter is connected to two pipelines via a T-junction; one pipeline connects to the inlet of the centrifugal separator, and the other pipeline connects sequentially to the first inlet of the acetone storage tank and... A cooling crystallization tank is provided; the outlet of the cooling crystallization tank is connected to the inlet of a centrifugal separator; the outlet of the cooling crystallization tank is connected to the inlet pipe of the centrifugal separator; the outlet of the centrifugal separator is connected to an acetone centrifugal liquid storage tank; the input end of the acetone transfer pump is connected to the acetone centrifugal liquid storage tank via a pipe, and the output end of the acetone transfer pump is connected to a secondary washing liquid addition pipe; the lower outlet of the acetone storage tank is connected to the input pipe of the acetone transfer pump, and the second inlet at the upper part of the acetone storage tank is connected to the output pipe of the acetone transfer pump via a pipe; valves are provided at the inlet and outlet ends of the acetone storage tank, the cooling crystallization tank, and the acetone washing kettle. The upper part of the acetone washing tank is also connected to a heat exchanger, which receives the vaporized acetone in the acetone washing tank and condenses it back to the acetone washing tank. The heat exchanger is provided with a heat exchange jacket on the outside; cold water or cold air is circulated in the heat exchange jacket; Heating steam is introduced into the jacket outside the acetone washing tank to maintain the temperature of the acetone solution inside the acetone washing tank at 35℃~45℃. The cooling crystallizer is equipped with a condensation jacket on the outside; cold water or cold air is circulated into the condensation jacket to maintain the temperature inside the cooling crystallizer at 10℃~15℃.

2. The high-efficiency acetone washing production apparatus for polyetheretherketone refining according to claim 1, characterized in that: The acetone washing tank is equipped with a stirring section; the stirring motor connected to the stirring section is located outside the acetone washing tank.

3. The high-efficiency acetone washing production apparatus for polyetheretherketone refining according to claim 1, characterized in that: The cooling crystallization tank is equipped with a stirring section I inside; the stirring motor I connected to the stirring section I is located outside the cooling crystallization tank.

4. The high-efficiency acetone washing production apparatus for refining polyetheretherketone according to claim 1, characterized in that: The number of acetone storage tanks in each acetone washing group is two or more, and the acetone storage tanks store the acetone washing liquid separated from the previous acetone washings.

5. The high-efficiency acetone washing production apparatus for refining polyetheretherketone according to claim 1, characterized in that: The number of filters in each acetone washing group is more than two, and the two or more filters are set in parallel to prevent the filters from being blocked during the filtration process, which would affect the discharge and slow down the discharge progress.

6. A method for producing high-efficiency acetone wash from refined polyetheretherketone (PEEK), utilizing the high-efficiency acetone wash production apparatus for refined PEEK as described in claim 1, characterized in that: The steps include the following, and the steps are performed in sequence: Step 1: The crushed polyether ether ketone material is buffered and decelerated in the polyether ether ketone granule buffer tank. The stirring motor of the acetone washing kettle is turned on, and acetone solution is added into the acetone washing kettle through the acetone inlet. The valve between the polyether ether ketone granule buffer tank and the acetone washing kettle is opened to allow the polyether ether ketone granules to flow into the acetone washing kettle. Step 2: Introduce a heating medium into the jacket of the acetone washing kettle to raise and maintain the temperature of the acetone solution inside the kettle to 35℃~45℃. Stir continuously 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 then enters a cooling crystallization tank to be cooled at 10℃~15℃. Step 3: Turn on the stirring motor I on the cooling crystallization tank. After the acetone solution containing a small amount of diphenyl sulfone in the cooling crystallization tank is cooled for 10 to 15 minutes, diphenyl sulfone crystallizes. Under the stirring action, the crystallized diphenyl sulfone particles are dispersed in a flocculent state, which is conducive to the separation of acetone and diphenyl sulfone. Step 4: Open the bottom valve of the cooling crystallization tank and put the liquid from Step 3 into the centrifugal separator to separate diphenyl sulfone and acetone solution containing a small amount of diphenyl sulfone. Take out the diphenyl sulfone and put it into the dryer to dry for recycling. The acetone solution containing a small amount of diphenyl sulfone is discharged into the acetone centrifugal liquid temporary storage tank and then pumped into the first acetone storage tank through the acetone transfer pump for later use. Step 5: Observe through the viewing window. Once the acetone in the acetone washing kettle has been completely drained, close the discharge valve at the bottom of the acetone washing kettle. Add acetone solution into the acetone washing kettle through the acetone inlet. Repeat steps 2 to 4 to perform a second acetone wash and discharge the acetone solution containing a small amount of diphenyl sulfone into the acetone centrifuge temporary storage tank. Then, pump the solution into the second acetone storage tank through the acetone transfer pump. Step 6: After observing that the acetone in the acetone washing kettle has been completely drained, close the discharge valve at the bottom of the acetone washing kettle. Add the acetone solution containing a small amount of diphenyl sulfone from the first acetone storage tank to the acetone washing kettle through the secondary washing liquid addition pipeline via the acetone transfer pump. Repeat steps 2 to 4 to perform the third acetone washing. After passing through the cooling crystallization tank and centrifugal separation device, pump the acetone solution containing a small amount of diphenyl sulfone discharged into the acetone centrifugal liquid temporary storage tank into the first acetone storage tank via the acetone transfer pump for later use. Step 7: After observing that the acetone in the acetone washing kettle has been completely drained, close the discharge valve at the bottom of the acetone washing kettle. Add the acetone solution containing a small amount of diphenyl sulfone from the second acetone storage tank to the acetone washing kettle through the secondary washing liquid addition pipeline via the acetone transfer pump. Repeat steps 2 to 4 to perform the fourth acetone washing. After passing through the cooling crystallization tank and centrifugal separation device, pump the acetone solution containing a small amount of diphenyl sulfone discharged into the acetone centrifugal liquid temporary storage tank into the second acetone storage tank via the acetone transfer pump for later use. Step 8: Repeat steps 6 and 7 at least once. During the last set number of acetone washes, alternately pump the acetone solution containing a small amount of diphenyl sulfone from the first and second acetone storage tanks into the acetone washing vessel. After the set acetone washing time, the acetone solution containing a small amount of diphenyl sulfone released is filtered and then directly enters the centrifuge and acetone centrifuge liquid storage tank. It is then stored in the first and second acetone storage tanks for subsequent acetone washes until the acetone solution containing a small amount of diphenyl sulfone obtained from the last two acetone washes is stored in the first and second acetone storage tanks respectively, waiting to be used for the next cycle of acetone washing. Step 9: Take out the polyether ether ketone obtained from the last acetone wash, put it into a centrifuge to remove the acetone, and then transport it to a water washing tank for washing. After drying, you can obtain the refined polyether ether ketone.

Citation Information

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