Production process of high-purity polyarylene ether nitrile

Through the process of multiple alcohol washing, water washing and pickling washing in the synthesis of polyarylether nitrile, the problem of low purity of polyarylether nitrile is solved, and the high purity production of the product is achieved.

CN119529267APending Publication Date: 2025-02-28SHANDONG WEUNITE BIOTECH CO LTD
View PDF 0 Cites 1 Cited by

Patent Information

Application Number
CN202411799656.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-09
Publication Date
2025-02-28

AI Technical Summary

Technical Problem

The purity of polyarylethernitrile synthesis is not high, mainly due to the incomplete washing of separation and washing steps, resulting in the incomplete removal of impurities.

Method used

The polyarylethernitrile product was gradually purified to improve its purity by purifying the solid-liquid mixture after multiple alcohol washing, followed by multiple water washing and pickling washing.

Benefits of technology

Through multiple alcohol washing, water washing and pickling washing processes, impurities in polyarylether nitriles are effectively removed, and the purity of the product is significantly improved.

✦ Generated by Eureka AI based on patent content.
Patent Text Reader

Abstract

The invention discloses a production process of high-purity polyarylene ether nitrile, and relates to the field of production of polyarylene ether nitrile, and the production process comprises a feeding process, a synthesis process, a grain-sized dicing process and a separating and washing process. A solvent in the filter is transferred to a dealcoholization tower kettle to be rectified and recycled, and is mechanically applied after being recycled in an alcohol tank of a granulator, so that the alcohol washing effect is improved, and then the solid material subjected to alcohol washing is dried; then washing the solid material subjected to alcohol washing with water for multiple times, washing with acid after washing, then drying, and finally drying the solid material, so that impurities in the polyarylene ether nitrile product are purified, and the purity of the polyarylene ether nitrile is improved.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention relates to the technical field of polyarylethernitrile production, and in particular to a production process of high-purity polyarylethernitrile. Background Art

[0002] Polyarylethernitrile (PEEN) is a linear aromatic polymer compound. It is a high temperature resistant thermoplastic with a high glass transition temperature (175°C) and melting point (353°C). The load heat deformation temperature is as high as 260°C. It can be used under pressure at 230°C for a long time. PEEN resin is not only better in heat resistance than other high temperature resistant plastics, but also has high strength, high modulus, high fracture toughness and excellent dimensional stability. In addition, PEEN also has excellent properties such as good self-lubrication, easy processing, stable insulation and hydrolysis resistance. It has a wide range of applications in the fields of industry, aerospace, automobile manufacturing, electronics and electrical, medical and food processing, and its development and utilization prospects are very broad.

[0003] At present, the purity of poly (arylether ether nitrile) synthesis process has not been high. There are many reasons for this, among which the washing is not thorough in the separation and washing process: in the separation and washing processes such as water washing and drying and alcohol washing and drying, if the washing times are insufficient, by-products and impurities such as salts produced during the reaction process will reduce the purity of the product. Summary of the invention

[0004] The present invention aims to solve one of the technical problems in the related art at least to a certain extent.

[0005] To this end, the object of the present invention is to provide a production process for high-purity polyarylethernitrile, wherein the present invention performs multiple alcohol washing on the solid-liquid mixture after pelletizing, and then performs multiple water washing on the solid material after alcohol washing, and then performs acid washing after water washing, thereby purifying impurities in the polyarylethernitrile product and improving the purity of the polyarylethernitrile.

[0006] To achieve the above object, the present invention proposes a production process of high-purity poly(arylene ether nitrile), comprising the following steps: S1, feeding process: dichlorobenzonitrile, hydroquinone, and potassium carbonate are put into the dehydration kettle while stirring; then toluene is put into the dehydration kettle; and NMP is put into the dehydration kettle; S2, synthesis process: the temperature in the dehydration kettle is controlled at 140-150°C, the dehydration time is 1.5-2.5 hours, and the material is transferred to the polycondensation kettle for condensation polymerization reaction; then the temperature in the polycondensation kettle is controlled at 185-190°C, and then toluene is extracted and cooled; then NMP is injected to clean the polycondensation kettle, and wait for pelletizing; S3, pelletizing process: open the methanol pump to inject methanol into the alcohol tank of the pelletizer, and then perform pelletizing to form a solid-liquid mixture; after all the materials are pelletized, continue to clean the crushed materials in the pelletizer by injecting NMP until no solid materials appear in the discharge, and then turn off the pelletizer; S4, separation and washing process: washing the solid-liquid mixture after pelletizing with alcohol, washing the solid material after alcohol washing with water for multiple times, and then drying it, and finally drying the solid material.

[0007] Further, in step S4, the step of alcohol washing is: S41, transferring the solid-liquid mixture after pelletizing to a filter, first starting the filter to stir, soaking and extracting for 3 to 5 hours, then transferring the filtrate in the filter to an alcohol cutting solvent intermediate tank, and the filtrate is then transferred to the dealcoholization tower bottom for distillation and reuse; S42. Pour fresh methanol into the filter until the material is completely soaked in methanol, stir it, and after soaking for 0.5 to 1 hour, open the filter and transfer the filtrate to the alcohol washing solvent intermediate tank. The filtrate is then transferred to the pelletizer alcohol tank via the alcohol washing solvent for application.

[0008] Further, the solid material after alcohol washing is dried, and the specific steps are as follows: S43, releasing the solid material after alcohol washing into the alcohol washing and drying system to wait for drying, turning on the alcohol washing vacuum pump, heating and drying the material, and when the liquid level in the alcohol washing and drying receiving tank no longer increases, the drying is completed; S44, after drying, the solid materials in the alcohol washing and drying system are raked out and transferred to the filter, the bottom valve of the alcohol washing and drying receiving tank is opened, and the received methanol is transferred to the alcohol receiving tank of the dealcoholization tower.

[0009] Further, in step S4, the steps of multiple washings are: S401. Pour fresh water into the filter, slowly add hydrochloric acid to the filter, control the pH value to 7-8, heat to 80°C and stir for 10 minutes, then stop heating and perform filtering operation, put the first washing liquid with the highest salt concentration into the primary washing liquid tank for application, open the nitrogen valve at the end of filtration and use nitrogen to filter, repeat the above several times, and press the filter liquid into the secondary washing liquid tank for application.

[0010] Further, the material after multiple washings is pickled, and the specific steps are as follows: S402, starting from the material to be pickled, the water used is the water in the primary washing liquid tank, the water is pumped into the filter, hydrochloric acid is slowly added to the filter, the pH value is controlled to be 7-8, heated to 80°C and stirred for 10 minutes, then the heating is stopped, and the hot filtering operation is performed, the waste brine is placed in the primary washing liquid tank for filtration, and then filtered with nitrogen. After the filter pressure is completed, the water is pumped into the waste brine feed tank for subsequent salt distillation treatment; S403, multiple washing: pump the application water into the filter, soak for 0.5 to 1 hour, then filter through nitrogen, press the filter liquid into the washing liquid tank, and repeat multiple times.

[0011] Further, in step S4, the solid material drying step is: S4001. Place the wet material in the filter into the product drying system and wait for drying; turn on the product drying system and maintain the inner drying temperature at 120-130°C; S4002, start the product drying system, the drying temperature is 105 ~ 120 ℃, dry for two hours, measure the remaining moisture of the product after drying, control the water mass ratio ≤ 0.5%, and stop drying; S4003. Open the product drying system and transfer the polyarylethernitrile material to the mixer for temporary storage.

[0012] Beneficial effects: The present invention performs alcohol washing for multiple times on the solid-liquid mixture after pelletizing, and transfers the solvent in the filter to the dealcoholization tower bottom for distillation and reuse, and applies it to the alcohol tank of the pelletizer, so as to improve the alcohol washing effect, and then dry the solid material after the alcohol washing; then wash the solid material after the alcohol washing with water for multiple times, and then acid wash it after the water washing, and then dry it, and finally dry the solid material, thereby purifying impurities in the polyarylethernitrile product and improving the purity of the polyarylethernitrile.

[0013] Additional aspects and advantages of the present invention will be given in part in the following description and in part will be obvious from the following description, or will be learned through practice of the present invention. DETAILED DESCRIPTION

[0014] Embodiments of the present invention are described in detail below, examples of which are shown in the scheme, wherein the same or similar reference numerals throughout represent the same or similar elements or elements with the same or similar functions. The embodiments described below by reference to the scheme are exemplary and are intended to be used to explain the present invention, and should not be construed as limiting the present invention.

[0015] The production process of high-purity poly(arylene ether nitrile) according to an embodiment of the present invention is described below in conjunction with the scheme.

[0016] The production process of polyarylether nitrile is as follows: 1. Feeding process Inspection and preparation: Before starting up for the first time or after the application is completed, carefully check that all pipelines and valves are open and closed normally, that there is no leakage in the pipeline flange, and that the instruments are normal before starting to feed.

[0017] Put the materials into the dehydration kettle; open the butterfly valves for stirring and feeding of the dehydration kettle, turn on the vacuum feeder P401 and the vacuum pump, and put the measured ton bags of dichlorobenzonitrile, hydroquinone, and potassium carbonate into the dehydration kettle while stirring (first put potassium carbonate to fill the bottom discharge port of the kettle to short-circuit the dead corner), and close the butterfly valve for feeding after the materials are put in.

[0018] Toluene delivery (first start-up); turn on the toluene pump and toluene feed pump in the tank area, and at the same time open the toluene metering tank inlet shut-off valve to pump toluene into the toluene metering tank for metering. After the metering is completed, turn off the feed pump and shut-off valve, open the toluene metering tank outlet bottom valve to put toluene into the dehydration kettle.

[0019] At the first start-up or after distillation, NMP (NMP: the abbreviation of N-methylpyrrolidone) is added: open the NMP pump in the tank area, open the NMP feed pump after distillation, and open the NMP metering tank inlet shut-off valve to pump NMP into the NMP metering tank for measurement. After the measurement is completed, close the feed pump and shut-off valve, open the NMP metering tank outlet bottom valve to put NMP into the dehydration kettle.

[0020] 2. Synthesis process Dehydration kettle temperature rise and reaction control: open the dehydration kettle thermal oil inlet cut-off valve and thermal oil outlet valve, adjust the thermal oil regulating valve oil temperature to 175℃, and slowly raise the liquid phase temperature in the dehydration kettle to 145℃. After the material begins to react to generate water and carbon dioxide, open the dehydration kettle condenser circulating water ball valve and the dehydration reflux water tank inlet ball valve for condensation and reflux, and adjust the thermal oil regulating valve to control the temperature in the dehydration kettle at 140-150℃, and dehydrate for 2.5 hours. When the water level in the water tank no longer increases, open the insulation ball valve and nitrogen valve at the bottom of the dehydration kettle to transfer the material to the polycondensation kettle.

[0021] Polycondensation kettle reaction and toluene treatment: Open the heat transfer oil inlet cut-off valve and heat transfer oil outlet valve of the polycondensation kettle, adjust the oil temperature of the heat transfer oil regulating valve to 205℃, and control the temperature in the polycondensation kettle at about 185℃. Open the circulating water ball valve of the polycondensation kettle condenser and the inlet ball valve of the polycondensation reflux water separation tank to extract toluene, and the extraction time is 1 hour. Then open the outlet ball valve of the polycondensation reflux water separation tank, evaporate and collect toluene in the toluene receiving tank for natural cooling. When the toluene drops to room temperature, open the bottom ball valve to recover it to the toluene recovery tank (it can be replenished when the liquid level of the toluene recovery tank is lower than 50%).

[0022] After all the oil is extracted, adjust the heat transfer oil regulating valve to raise the temperature to 185-190℃, keep it warm for 2 hours, observe the viscosity change in real time and take samples to test the intrinsic viscosity, and adjust the speed according to the viscosity change. After the viscosity counter value and current value are stable, add appropriate NMP to terminate the reaction.

[0023] Polycondensation kettle cleaning and material transfer: After the polycondensation kettle reaction is completed, open the thermal oil cut-off valve of the buffer kettle, and adjust the thermal oil regulating valve to control the temperature in the buffer kettle to about 135°C. Open the nitrogen valve and the bottom insulation valve of the polycondensation kettle, and press the material into the buffer kettle for temporary storage. Then open the valve of the spray device on the polycondensation kettle and the NMP cleaning pump, and spray the wall of the polycondensation kettle with NMP. After the cleaned kettle liquid is placed in the buffer kettle, stop spraying, close the discharge valve of the polycondensation kettle, and wait for the pelletizer to be debugged before sending the material to the next process.

[0024] 3. Pelletizing process Methanol circulation and pelletizing preparation (first start-up or after distillation): for the first start-up, open the methanol pump in the tank area to fill the alcohol recovery tank of the dealcoholization tower. After distillation, open the alcohol pump of the dealcoholization tower and open the alcohol tank inlet ball valve of the pelletizer to fill it. Open the pelletizer alcohol pump to replenish methanol to the sedimentation tank to maintain a suitable liquid level. Open the circulating feed pump and the cooling water valve on the methanol heat exchanger to cool the methanol and then pass it into the methanol intermediate tank. After a vortex is formed in the buffer kettle at the inlet of the pulverizer, open the pulverizer to pump methanol to the filter (a, b). After being filtered by the filter, the methanol enters the sedimentation tank to form a methanol circulation loop. Adjust the pulverizer parameters to maintain the liquid level of the buffer kettle at the inlet of the pulverizer unchanged. Open the insulation valve at the bottom of the buffer kettle and the nitrogen valve at the top to feed the pelletizer.

[0025] Material crushing speed adjustment: The material crushing speed can be adjusted by adjusting the feed valve of the buffer kettle at the inlet of the crusher. While ensuring that the crusher and the pipeline to the two-in-one filter are not blocked, as much material as possible is fed to increase the crushing speed.

[0026] Filtrate treatment and filter switching: Open the discharge valve on the south side of the bottom of the two-in-one filter to filter out the filtrate in the solid-liquid mixture after pelletizing to the sedimentation tank below for further pelletizing. Observe the filtering situation of filter a through the sight glass. When the filter is about to be full, adjust the valve to guide the material to filter b for filtration.

[0027] End of pelletizing operation: After the pelletizing of buffer kettle material is completed, open the valve of NMP feed pipeline, the valve of spray system on the top of buffer kettle and NMP cleaning pump, continue the crushing operation with NMP until no solid material appears in the sight glass of crusher outlet, close pelletizer, pelletizer heat oil valve, bottom butterfly valve of solid-liquid separator, empty methanol in sedimentation tank and add fresh methanol to flush methanol heat exchanger, pelletizer and solid-liquid separator, and finally enter the two-in-one filter.

[0028] 4. Separation and washing process Alcohol washing and drying: First alcohol washing: After the solid-liquid mixture after pelletizing is transferred to filters a and b, start the stirring of filter a. After soaking and extracting for 3 hours, open the filtrate outlet valve on the side of the filter and the nitrogen valve on the top, transfer the filtrate to the alcohol cutting solvent intermediate tank, and then transfer it to the dealcoholization tower bottom for distillation and reuse.

[0029] Second alcohol washing: open the pelletizer alcohol pump to pump fresh methanol into filters a and b until the material is completely soaked in methanol, turn on stirring, and after soaking for 0.5 hours, open the filtrate outlet valve on the side of the filter and the nitrogen valve on the top, transfer the filtrate to the alcohol washing solvent intermediate tank, and then transfer it to the pelletizer alcohol tank through the alcohol washing solvent pump for application.

[0030] Drying: Release the solid material after alcohol washing through the side discharge valve into the alcohol washing and drying system below, open the gas phase valve of the alcohol washing and drying system, the cooling water valve of the alcohol washing and drying condenser, the inlet valve of the alcohol washing and drying receiving tank and the vacuum pipeline valve, turn on the alcohol washing vacuum pump, put the drying system in a vacuum state, then open the steam inlet valve and steam condensate outlet valve of the alcohol washing and drying system to heat the dry material, and when the liquid level in the alcohol washing and drying receiving tank no longer increases, the drying is completed.

[0031] Material transfer and methanol recovery: After drying, close the air inlet valve on the alcohol washing vacuum buffer tank, open the vent pipe valve of the alcohol washing and drying receiving tank, rake out the solid materials in the alcohol washing and drying system, and manually transfer them to filter b, open the bottom valve of the alcohol washing and drying receiving tank, and transfer the received methanol to the alcohol receiving tank of the dealcoholization tower.

[0032] Wash and dry (use fresh water in the brine recovery tank for the first start-up): Acid washing and filtration for the first start-up: open the valve at the bottom of the tank and the brine pump, pump fresh water into filter c or filter d (the liquid level just submerges the material), turn on the filter stirring and the hydrochloric acid metering tank discharge valve, slowly add hydrochloric acid to filter c or d, and after the system is neutralized (the liquid surface no longer bubbles) and the pH value reaches 7-8, close the hydrochloric acid metering tank discharge valve, take samples and analyze them after they are qualified, open the steam inlet valve of the filter while stirring, heat to 80°C and stir for 10 minutes, then stop heating and perform filtering operations.

[0033] Treatment of primary washing liquid: Open the valve to the primary washing liquid tank in the filtrate discharge valve on the side of filter c or filter d, put the first washing liquid with the highest salt concentration into the primary washing liquid tank for application, open the nitrogen valve to filter with nitrogen at the later stage of filtration, and close the valve to the primary washing liquid tank after the filtration is completed.

[0034] Secondary washing: open the bottom valve of the brine recovery tank and the brine pump, pump fresh water into filter c or filter d (the liquid level just submerges the material), stir while washing, soak for 0.5 hours, pass nitrogen pressure filtration, open the valve in the filtrate discharge valve leading to the secondary washing liquid tank, press the filtrate liquid into the secondary washing liquid tank, and close the valve after filtration.

[0035] Three washings: open the bottom valve of the brine recovery tank and the brine pump, pump fresh water into filter c or filter d (the liquid level just covers the material), stir while washing, soak for 0.5 hours, pass nitrogen pressure filtration, open the valve in the filtrate discharge valve leading to the three washing liquid tank, press the filtrate liquid into the three washing liquid tank, and close the valve after filtration.

[0036] Four washings: Open the bottom valve of the brine recovery tank and the brine feed pump, pump fresh water into filter c or filter d (the liquid level just covers the material), start stirring while washing and soaking for 0.5 hours, then filter with nitrogen, open the valve in the filtrate discharge valve leading to the four washing liquid tank, press the filter liquid into the four washing liquid tank, and close the valve after filtration.

[0037] Acid washing (starting from the second batch of materials): open the valve at the bottom of the tank and the primary washing liquid pump, pump the coating water into filter c or filter d (the liquid level just immerses the material), open the filter stirring and the hydrochloric acid metering tank discharge valve, slowly add hydrochloric acid to filter c or d, and after the system is neutralized to a pH value of 7-8, close the hydrochloric acid metering tank discharge valve, and after the sampling and analysis are qualified, open the steam inlet valve of the filter while stirring, heat to 80°C and stir for 10 minutes, then stop heating, filter while hot, open the valve to the primary washing liquid tank in the filtrate discharge valve on the side of filter c or filter d, put the waste brine into the primary washing liquid tank, open the nitrogen valve in the later stage of filtration to filter with nitrogen pressure, close the valve to the primary washing liquid tank after the pressure filtration, open the primary washing liquid pump, and pump the coating water into the waste brine feed tank for salt steaming.

[0038] First washing (subsequent batches): Open the bottom valve of the secondary washing liquid tank and the secondary washing liquid pump, pump the application water into filter c or filter d (the liquid level just immerses the material), start stirring while washing and soaking for 0.5 hours, then filter with nitrogen, open the valve in the filtrate discharge valve leading to the primary washing liquid tank, press the filtrate into the primary washing liquid tank, and close the valve after filtration.

[0039] Secondary washing (subsequent batches): Open the bottom valve of the tertiary washing liquid tank and the tertiary washing liquid pump, and pump the application water into filter c or filter d (the liquid level just immerses the material), start stirring while washing and soaking for 0.5 hours, then pass nitrogen pressure filtration, open the valve in the filtrate discharge valve leading to the secondary washing liquid tank, press the filtrate liquid into the secondary washing liquid tank, and close the valve after filtration.

[0040] Three washings (subsequent batches): Open the bottom valve of the four-washing liquid tank and the four-washing liquid pump, pump the application water into filter c or filter d (the liquid level just immerses the material), start stirring while washing and soaking for 0.5 hours, then filter with nitrogen, open the valve in the filtrate discharge valve leading to the three-washing liquid tank, press the filtrate into the three-washing liquid tank, and close the valve after filtration.

[0041] Four washings (subsequent batches): Open the bottom valve of the brine recovery tank and the brine pump, pump fresh water into filter c or filter d (the liquid level just covers the material), stir while washing, soak for 0.5 hours, pass nitrogen pressure filtration, open the valve in the filtrate discharge valve leading to the four washing liquid tank, press the filtrate liquid into the four washing liquid tank, and close the valve after filtration.

[0042] 5. Drying process Material drying preparation: put the wet material in filter c or d into the product drying system below through the discharge valve, open the steam regulating valve and steam inlet switch valve of the steam pipeline of the product drying system, and keep the drying temperature of the inner room at 120℃.

[0043] Drying operation and moisture control: Start the product drying system and dry the product until the remaining moisture meets the requirements (measure moisture, oven at 105°C for two hours, water mass ratio ≤0.5%, optimal 0.1%).

[0044] Gas phase treatment and material transfer: During the drying process, the gas phase enters the tail gas main after passing through the collector. Open the discharge port at the bottom of the product drying system and transfer the polyarylethernitrile material to the conical mixer for temporary storage. If the customer has special needs, additives can be added to the mixer and mixed evenly before granulation. If there is no special need, it can be directly packaged and shipped.

[0045] In summary, the production process of high-purity polyarylethernitrile in the embodiment of the present invention improves the alcohol washing effect by washing the solid-liquid mixture after pelletizing with alcohol for multiple times, and transferring the solvent in the filter to the dealcoholization tower bottom for distillation and reuse, and applying it after the pelletizer alcohol tank, and then drying the solid material after alcohol washing; then washing the solid material after alcohol washing with water for multiple times, acid washing after water washing, and then drying, and finally drying the solid material, thereby purifying impurities in the polyarylethernitrile product and improving the purity of the polyarylethernitrile.

[0046] Although the embodiments of the present invention have been shown and described above, it is to be understood that the above embodiments are exemplary and are not to be construed as limitations of the present invention. A person skilled in the art may change, modify, replace and deform the above embodiments within the scope of the present invention.

Claims

1. A production process for high-purity polyarylethernitrile, characterized in that: Including the following processes: S1, feeding process: dichlorobenzonitrile, hydroquinone, and potassium carbonate are put into the dehydration kettle while stirring; then toluene is put into the dehydration kettle; and NMP is put into the dehydration kettle; S2, synthesis process: transferring the material to a polycondensation kettle for condensation polymerization reaction; then taking out the toluene and cooling it; then injecting NMP to clean the polycondensation kettle; S3, pelletizing process: open the methanol pump to inject methanol into the alcohol tank of the pelletizer, and then pelletize to form a solid-liquid mixture; after all the materials are pelletized, continue to clean the crushed materials in the pelletizer by injecting NMP until no solid materials appear in the discharge, and then stop pelletizing; S4, separation and washing process: washing the solid-liquid mixture after pelletizing with alcohol, washing the solid material after alcohol washing with water for multiple times, and then drying it, and finally drying the solid material.

2. The production process of high-purity polyarylethernitrile according to claim 1, characterized in that: In step S4, the step of alcohol washing is: S41, transferring the solid-liquid mixture after pelletizing to a filter, first starting the filter to stir, soaking and extracting for 3 to 5 hours, then transferring the filtrate in the filter to an alcohol cutting solvent intermediate tank, and the filtrate is then transferred to the dealcoholization tower bottom for distillation and reuse; S42. Pour fresh methanol into the filter until the material is completely soaked in methanol, stir it, and after soaking for 0.5 to 1 hour, open the filter and transfer the filtrate to the alcohol washing solvent intermediate tank. The filtrate is then transferred to the pelletizer alcohol tank via the alcohol washing solvent for application.

3. The production process of high-purity polyarylethernitrile according to claim 2, characterized in that: The solid material after alcohol washing is dried, and the specific steps are as follows: S43, releasing the solid material after alcohol washing into the alcohol washing and drying system to wait for drying, turning on the alcohol washing vacuum pump, heating and drying the material, and when the liquid level in the alcohol washing and drying receiving tank no longer increases, the drying is completed; S44, after drying, the solid materials in the alcohol washing and drying system are raked out and transferred to the filter, the bottom valve of the alcohol washing and drying receiving tank is opened, and the received methanol is transferred to the alcohol receiving tank of the dealcoholization tower.

4. The production process of high-purity polyarylethernitrile according to claim 1, characterized in that: In step S4, the steps of multiple washings are: S401. Pour fresh water into the filter, slowly add hydrochloric acid to the filter, control the pH value to 7-8, heat to 80°C and stir for 10 minutes, then stop heating and perform filtering operation, put the first washing liquid with the highest salt concentration into the primary washing liquid tank for application, open the nitrogen valve at the end of filtration and use nitrogen to filter, repeat the above several times, and press the filter liquid into the secondary washing liquid tank for application.

5. The production process of high-purity polyarylethernitrile according to claim 4, characterized in that: The material after multiple washings is pickled, and the specific steps are as follows: S402, starting from the material to be pickled, the water used is the water in the primary washing liquid tank, the water is pumped into the filter, hydrochloric acid is slowly added to the filter, the pH value is controlled to be 7-8, heated to 80°C and stirred for 10 minutes, then the heating is stopped, and the hot filtering operation is performed, the waste brine is placed in the primary washing liquid tank for filtration, and then filtered with nitrogen. After the filter pressure is completed, the water is pumped into the waste brine feed tank for subsequent salt distillation treatment; S403, multiple washing: pump the application water into the filter, soak for 0.5 to 1 hour, then filter through nitrogen, press the filter liquid into the washing liquid tank, and repeat multiple times.

6. The production process of high-purity poly(arylene ether nitrile) according to claim 1, characterized in that: In step S4, the solid material drying step is: S4001. Place the wet material in the filter into the product drying system and wait for drying; turn on the product drying system and maintain the inner drying temperature at 120-130°C; S4002, start the product drying system, the drying temperature is 105 ~ 120 ℃, dry for two hours, measure the remaining moisture of the product after drying, control the water mass ratio ≤ 0.5%, and stop drying; S4003. Open the product drying system and transfer the polyarylethernitrile material to the mixer for temporary storage.

Citation Information

Cited By

  • Production process for high-purity polyarylene ether nitrile

    WO2026123956A1