CN113680128A - Continuous washing and purifying system and purifying method for polyarylene sulfide resin - Google Patents
Continuous washing and purifying system and purifying method for polyarylene sulfide resin Download PDFInfo
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- CN113680128A CN113680128A CN202110850039.2A CN202110850039A CN113680128A CN 113680128 A CN113680128 A CN 113680128A CN 202110850039 A CN202110850039 A CN 202110850039A CN 113680128 A CN113680128 A CN 113680128A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/04—Filters with filtering elements which move during the filtering operation with filtering bands or the like supported on cylinders which are impervious for filtering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/44—Regenerating the filter material in the filter
- B01D33/46—Regenerating the filter material in the filter by scrapers, brushes nozzles or the like acting on the cake-side of the filtering element
- B01D33/466—Regenerating the filter material in the filter by scrapers, brushes nozzles or the like acting on the cake-side of the filtering element scrapers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/58—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element
- B01D33/60—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element for washing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/58—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element
- B01D33/62—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element for drying
- B01D33/66—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element for drying by gases or by heating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/58—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element
- B01D33/62—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element for drying
- B01D33/66—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element for drying by gases or by heating
- B01D33/663—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element for drying by gases or by heating by direct contact with a fluid
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
- C08G75/02—Polythioethers
- C08G75/0204—Polyarylenethioethers
- C08G75/0277—Post-polymerisation treatment
- C08G75/0281—Recovery or purification
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Abstract
The invention discloses a continuous washing and purifying system and a purifying method of polyarylene sulfide resin, which comprises the following steps: (1) filtering the polyarylene sulfide resin through a first closed belt filter, washing the polyarylene sulfide resin with a hot solvent, purging the polyarylene sulfide resin with high-temperature nitrogen, and stripping the polyarylene sulfide resin to obtain a filter cake containing the polyarylene sulfide resin and sodium chloride; (2) fully dissolving and mixing the filter cake through a dissolved salt mixing tank; (3) filtering the dissolved and mixed slurry through a second closed belt filter, washing the solvent, and stripping to obtain wet resin; (4) the wet resin obtained by the gas dryer is dried to obtain a refined PPS resin. The invention adopts the continuous closed belt filter to continuously complete the working procedures of filtering, washing, purging and the like on the continuous filter belt; efficiently separating a reaction solvent, an oligomer and a catalyst, and directly using the reaction solvent, the oligomer and the catalyst in a condensation reaction; the filtered resin is washed and continuously dried, so that the working efficiency is high, the separation effect is good, the purity of the resin product is high, the cost is low, and the method is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of purification of high molecular polymer products, and particularly relates to a continuous washing and purifying system and a purifying method for polyarylene sulfide resin, aiming at obtaining a high-quality polyarylene sulfide resin product.
Background
The polyarylene sulfide is a novel high-performance thermoplastic resin, has excellent electrical insulation, chemical corrosion resistance, heat resistance and flame retardance, is widely applied to the fields of automobiles, electronic and electrical products, machinery, rail transit, aerospace, military industry and the like, is called as 'sixth engineering plastic' in the world, is also one of eight aerospace materials, is a strategic new material which is greatly supported and developed by China, and has the synthesis method which is valued by various countries.
At present, the synthesis method of the polyarylene sulfide is mainly a sodium sulfide method, namely, dihalobenzene, sodium sulfide/sodium hydrosulfide are used as raw materials, lithium chloride is used as a catalyst, and NMP is used as a catalyst to carry out condensation reaction under the alkaline condition; after the condensation reaction is finished, the liquid slurry is separated, the solid is mainly polyarylene sulfide resin containing oligomer and byproduct salt, and the liquid is NMP solution containing catalyst and oligomer. In order to obtain a purer resin product, the resin slurry after the condensation reaction has been completed must be washed and purified. In the conventional process for producing polyarylene sulfide resin, a method is used in which a large amount of water is directly added to the slurry after the polymerization reaction is completed, and then solid-liquid separation is performed. The polyarylene sulfide resin obtained by the treatment method has low purity, high salt content and poor color. Therefore, there is a need for a more efficient process for obtaining pure polyarylene sulfide resins, which is critical to the production of polyarylene sulfide resins.
Disclosure of Invention
The invention provides a polyarylene sulfide resin continuous washing and purifying system and a purifying method, wherein the continuous closed belt filter is adopted, reasonable process conditions are controlled, and the working procedures of filtering, washing, purging and the like are continuously completed on a continuous filter belt; efficiently separating a reaction solvent, an oligomer and a catalyst, and directly using the mixture in condensation reaction; washing the filtered resin, and continuously drying the resin in a drying procedure; high working efficiency, good separation effect, high purity of resin products, low cost and suitability for industrial production.
In order to achieve the purpose, the invention adopts the following technical scheme:
a continuous scrubbing purification system for polyarylene sulfide resins comprising:
the first closed belt filter is obliquely and upwards arranged from the feed inlet to the discharge outlet and sequentially comprises a filtering section, a solvent washing section, a nitrogen purging section and a stripping section from bottom to top;
a feed inlet of the dissolved salt slurry mixing tank is connected with a discharge outlet of the first closed belt filter, and a stirring assembly is arranged in the dissolved salt slurry mixing tank;
a feed inlet of the second closed belt filter is connected with a discharge outlet of the dissolved salt slurry mixing tank and is arranged from the feed inlet to the discharge outlet in an inclined upward manner, and the second closed belt filter sequentially comprises a filtering section, a solvent washing section and a stripping section from bottom to top;
and a feed inlet of the gas dryer is connected with a discharge outlet of the second closed belt filter.
As a further description of the above technical solution: and a feed inlet of the first closed belt filter is provided with a distributing device, and polymer slurry is conveyed into the distributing device through a high-temperature slurry pump and enters the first closed belt filter from the distributing device.
As a further description of the above technical solution: the first closed belt filter comprises a filter belt which is obliquely arranged from bottom to top, and a solvent spraying and washing assembly is arranged above the solvent washing section of the first closed belt filter; a high-pressure nitrogen blowing assembly is arranged above the nitrogen blowing section of the first closed belt filter; and a positioning scraper matched with a filter belt is arranged at the stripping section of the first closed belt filter.
As a further description of the above technical solution: the first closed belt filter is provided with liquid outlet pipes in the filtering section, the solvent washing section and the nitrogen purging section respectively, and the three liquid outlet pipes are connected with a filtrate temporary storage tank respectively.
As a further description of the above technical solution: the feed inlet of the second closed belt filter is connected with the discharge outlet of the dissolved salt slurry mixing tank through a pipeline and a high-temperature slurry pump.
As a further description of the above technical solution: the second closed belt filter comprises a filter belt which is obliquely arranged from bottom to top, and a process soft water spraying and washing assembly is arranged above the solvent washing section of the second closed belt filter; and a positioning scraper matched with a filter belt is arranged at the stripping section of the second closed belt filter.
As a further description of the above technical solution: the first closed belt filter is provided with liquid outlet pipes at the filtering section and the solvent washing section respectively, and the two liquid outlet pipes are connected with a filtrate temporary storage tank respectively.
As a further description of the above technical solution: the gas dryer comprises an ebullated bed or flash dryer.
As a further description of the above technical solution: the exit end of gas desicator is connected with cyclone, cyclone's air inlet is equipped with the draught fan, gas desicator's air inlet is equipped with the gas filtration heater.
A method for continuously washing and purifying polyarylene sulfide resin, comprising the following steps:
(1) after the poly (arylene sulfide) resin synthesis polycondensation reaction is finished, uniformly distributing polymer slurry at a certain temperature (150-250 ℃) on a filter belt of a first closed belt filter which continuously runs by using a high-temperature slurry pump and a distributor; with the movement of the filter belt, the filter belt sequentially passes through a filtering section, a solvent washing section, a nitrogen purging section and a stripping section; the high-temperature filtrate separated in the filtering section is dissolved with a catalyst, an auxiliary agent and an active oligomer, and directly circulated to the condensation reaction process for recycling; in a solvent washing section, continuously spraying, washing and filtering a filter cake on a filter belt by using a hot solvent (120-180 ℃), and removing the solvent and the auxiliary agent remained on the filter cake; part of the filtrate of the solvent washing section is recycled to the condensation reaction process, and is recycled, and part of the filtrate is removed from the solvent for recovery; in the nitrogen purging section, purging the filter cake by using high-purity nitrogen to remove the residual solvent in the filter cake; in the stripping section, a positioning scraper is utilized to strip filter cake solids which are filtered and washed, and the main components of the filter cake solids are polyarylene sulfide resin and sodium chloride;
(2) continuously feeding the filter cake solid obtained in the step (1) and process soft water/dilute brine into a salt dissolving and pulp mixing tank according to a certain proportion, and fully stirring and dissolving sodium chloride salt in the filter cake solid under stirring and temperature control of 30-80 ℃; adding a low-foaming amide surfactant or an ethylene oxide-propylene oxide block copolymer nonionic surfactant into process soft water or dilute brine to help wetting and improve the salt-dissolving washing effect; the addition amount of the surfactant in the water phase is 10-40 g/m3(ii) a The mass of the water phase is 4-7 times of that of the solid filter cake; the temperature in the salt dissolving and pulp conditioning tank is 30-80 ℃, and the retention time of the materials is 30 minutes;
(3) maintaining the continuous and uniform stirring, temperature and liquid level in the salt dissolving and pulp mixing tank in the step (2); continuously extracting slurry by using a slurry pump at the bottom of the dissolved salt size mixing tank, conveying the slurry to a second closed belt filter, and uniformly distributing the slurry on a continuously running filter belt; the filter belt moves forwards and sequentially passes through a filtering section, a process soft water spraying and washing section and a stripping section; the filtrate obtained in the filtering section, namely the strong brine, continuously enters a strong brine storage tank and is sent to be refined and recycled to obtain sodium chloride; the filtrate in the soft water spraying and washing section is dilute brine containing a small amount of sodium chloride, and is circulated to the dissolved salt pulp mixing tank in the step (2) for recycling; the stripped purified filter cake is refined polyarylene sulfide resin and is continuously sent to a resin drying procedure for drying;
(4) and (4) continuously feeding the wet resin obtained after the water washing in the step (3) into a drying process, and drying by adopting a fluidized bed or an air flow dryer. Controlling the drying temperature of the resin to be 130-150 ℃ during the drying of the fluidized bed, and keeping the resin for 15-40 minutes; when the airflow drying is adopted, the drying temperature is 150-180 ℃, and the retention time is 3-10 minutes.
The invention has the following beneficial effects:
1. the washing solvent adopted by the invention can remove most of oligomers and salts mixed in the resin after the condensation reaction is finished, and solves the problems of low product purity and poor color after the traditional resin washing is finished.
2. The method realizes the continuous washing and purification of the polyarylene sulfide resin, improves the production efficiency and the equipment utilization rate, and effectively reduces the production cost of the polyarylene sulfide resin.
3. The yield of the PPS resin obtained by the invention can reach 95%, and the content of oligomer is less than or equal to 3%.
Drawings
FIG. 1 is a schematic structural diagram of a continuous scrubbing purification system for polyarylene sulfide resin disclosed in the present invention.
Reference numerals: 1-a distributor; 2-solvent spray washing assembly; 3-a high pressure nitrogen gas blowing component; 4-fixing an outer scraper; 5-a salt dissolving and pulp mixing tank; 6-gas dryer; 7-gas filtration heater; 8-a cyclone separator; 9-a draught fan; 10-filtrate buffer tank; 11-a filter belt; 12-high temperature slurry pump.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The polyarylene sulfide resin is obtained by industrially carrying out a high-temperature polycondensation reaction in a polar aprotic solvent NMP or HMPTA in the presence of lithium chloride or sodium acetate with anhydrous sodium sulfide, crystalline sodium sulfide or sodium hydrosulfide or a sodium hydrosulfide aqueous solution as a sulfur source compound and p-dichlorobenzene, p-chlorobiphenyl and the like as chlorine-containing monomers. The resin contains a large amount of impurities such as oligomer, inorganic salt, pigment and the like, which seriously affect the processing performance, application performance and electrical performance of the resin, worsen the processing and use environment of the resin and corrode processing and application equipment. Therefore, the resin must be washed and purified.
As shown in fig. 1, a continuous scrubbing purification system for polyarylene sulfide resin, comprising:
the first closed belt filter is obliquely and upwards arranged from the feed inlet to the discharge outlet and sequentially comprises a filtering section, a solvent washing section, a nitrogen purging section and a stripping section from bottom to top;
a feed inlet of the dissolved salt slurry mixing tank is connected with a discharge outlet of the first closed belt filter, and a stirring assembly is arranged in the dissolved salt slurry mixing tank;
a feed inlet of the second closed belt filter is connected with a discharge outlet of the dissolved salt slurry mixing tank and is arranged from the feed inlet to the discharge outlet in an inclined upward manner, and the second closed belt filter sequentially comprises a filtering section, a solvent washing section and a stripping section from bottom to top;
and a feed inlet of the gas dryer is connected with a discharge outlet of the second closed belt filter.
In this embodiment, the feed inlet of the first closed belt filter is provided with a distributor 1, and the polymer slurry is conveyed into the distributor 1 by a high-temperature slurry pump and enters the first closed belt filter from the distributor 1.
In the embodiment, the first closed belt filter comprises a filter belt 11 which is obliquely arranged from bottom to top, and a solvent spraying and washing assembly 2 is arranged above the solvent washing section of the first closed belt filter; a high-pressure nitrogen blowing assembly 3 is arranged above the nitrogen blowing section of the first closed belt filter; and a positioning scraper 4 matched with a filter belt is arranged at the stripping section of the first closed belt filter.
In this embodiment, first airtight belt filter is equipped with the drain pipe respectively in filter segment, solvent washing section, nitrogen gas sweep the section, and three drain pipes are connected with filtrating scratch pad 10 respectively.
In this embodiment, the inlet of the second closed belt filter is connected with the outlet of the dissolved salt slurry mixing tank through a pipeline and a high-temperature slurry pump 12.
In this embodiment, the second closed belt filter includes a filter belt inclined from bottom to top, and a process soft water spray washing assembly is disposed above the solvent washing section of the second closed belt filter; and a positioning scraper matched with a filter belt is arranged at the stripping section of the second closed belt filter.
In this embodiment, first airtight belt filter is equipped with the drain pipe respectively in filter stage, solvent washing section, and two drain pipes are connected with filtrating jar of keeping in respectively.
In this embodiment, the gas dryer 6 comprises an ebullated bed or flash dryer.
In this embodiment, the exit end of gas desicator 6 is connected with cyclone 8, cyclone 8's air inlet is equipped with draught fan 9, gas desicator 8's air inlet is equipped with gas filtration heater 7.
A method for continuously washing and purifying polyarylene sulfide resin, comprising the following steps:
(1) after the poly (arylene sulfide) resin synthesis polycondensation reaction is finished, uniformly distributing polymer slurry at a certain temperature (150-250 ℃) on a filter belt of a first closed belt filter which continuously runs by using a high-temperature slurry pump and a distributor 1; with the movement of the filter belt, the filter belt sequentially passes through a filtering section, a solvent washing section, a nitrogen purging section and a stripping section; the high-temperature filtrate separated in the filtering section is dissolved with a catalyst, an auxiliary agent and an active oligomer, and directly circulated to the condensation reaction process for recycling; in a solvent washing section, continuously spraying, washing and filtering a filter cake on a filter belt by using a hot solvent (120-180 ℃), and removing the solvent and the auxiliary agent remained on the filter cake; part of the filtrate of the solvent washing section is recycled to the condensation reaction process, and is recycled, and part of the filtrate is removed from the solvent for recovery; in the nitrogen purging section, purging the filter cake by using high-purity nitrogen to remove the residual solvent in the filter cake; in the stripping section, a positioning scraper 4 is utilized to strip filter cake solids washed by filtration, wherein the main components of the filter cake solids are polyarylene sulfide resin and sodium chloride;
(2) continuously feeding the filter cake solid obtained in the step (1) and process soft water/dilute brine into a salt dissolving and slurry mixing tank according to a certain proportion, and fully stirring and dissolving the filter cake solid under stirring and temperature control of 30-80 DEG CSodium chloride, a medium salt; adding a low-foaming amide surfactant or an ethylene oxide-propylene oxide block copolymer nonionic surfactant into process soft water or dilute brine to help wetting and improve the salt-dissolving washing effect; the addition amount of the surfactant in the water phase is 10-40 g/m3(ii) a The mass of the water phase is 4-7 times of that of the solid filter cake; the temperature in the salt dissolving and pulp conditioning tank is 30-80 ℃, and the retention time of the materials is 30 minutes;
(3) maintaining the continuous and uniform stirring, temperature and liquid level in the salt dissolving and pulp mixing tank in the step (2); continuously extracting slurry by using a slurry pump at the bottom of the dissolved salt size mixing tank, conveying the slurry to a second closed belt filter, and uniformly distributing the slurry on a continuously running filter belt; the filter belt moves forwards and sequentially passes through a filtering section, a process soft water spraying and washing section and a stripping section; the filtrate obtained in the filtering section, namely the strong brine, continuously enters a strong brine storage tank and is sent to be refined and recycled to obtain sodium chloride; the filtrate in the soft water spraying and washing section is dilute brine containing a small amount of sodium chloride, and is circulated to the dissolved salt pulp mixing tank in the step (2) for recycling; the stripped purified filter cake is refined polyarylene sulfide resin and is continuously sent to a resin drying procedure for drying;
(4) and (4) continuously feeding the wet resin obtained after the water washing in the step (3) into a drying process, and drying by adopting a fluidized bed or an air flow dryer. Controlling the drying temperature of the resin to be 130-150 ℃ during the drying of the fluidized bed, and keeping the resin for 15-40 minutes; when the airflow drying is adopted, the drying temperature is 150-180 ℃, and the retention time is 3-10 minutes.
Example 1
A continuous washing and purifying technology for polyarylene sulfide resin comprises the following steps:
adding sodium sulfide, sodium hydrosulfide or sodium hydrosulfide aqueous solution, dihalogenated aromatic hydrocarbon, sodium hydroxide, solvent NMP or HMPTA, lithium chloride or sodium acetate into a condensation reaction kettle, and controlling the temperature to be 150-280 ℃ to carry out high-temperature polycondensation reaction to obtain polyarylene sulfide resin slurry;
(1) after the polycondensation reaction of the polyphenylene sulfide resin is finished, when the temperature is reduced to 150 ℃, the polyarylene sulfide resin slurry is conveyed to a first closed belt filter which continuously operates by using a high-temperature slurry pump and cloth, solid-liquid separation is firstly carried out on the first closed belt filter, the liquid obtained by separation enters a high-temperature filtrate storage tank (namely a filtrate temporary storage tank 1), the solid resin is continuously conveyed to a solvent washing section of a belt, 20 wt% of 120 ℃ hot solvent is used for continuously spraying, washing and filtering the solid, the filtered liquid enters a solvent storage tank (namely a filtrate temporary storage tank 2), the solid is continuously conveyed to a nitrogen purging section, a filter cake is purged by using high-purity nitrogen with constant flow, and the purged liquid enters a filtrate temporary storage tank 3.
(2) And (2) continuously conveying the filter cake obtained by sweeping in the step (1) to a dissolved salt slurry mixing tank by using a positioning scraper, simultaneously adding soft water with the mass 5 times that of the feed inlet, adding 0.002 wt% of amide surfactant into the soft water, keeping the liquid level in the slurry mixing tank constant, keeping the temperature at about 85-90 ℃, and keeping the material retention time for 30 min.
(3) And (3) extracting slurry subjected to water washing and size mixing in the step (2) from the tank bottom, continuously conveying the slurry to a closed belt filter, firstly performing solid-liquid separation, allowing liquid to enter a strong brine storage tank to recover industrial byproduct salt, continuously conveying the solid to a process soft water spraying section, spraying the solid at a high speed by adopting 20 wt% of soft water, allowing filtrate of the spraying section to enter a dilute brine storage tank to be recycled as a solvent for next batch of water washing and size mixing, and continuously conveying a filter cake to a stripping section.
(4) And (4) sending the filter cake obtained in the step (3), namely refined polyphenylene sulfide wet resin, to a fluidized bed dryer through a scraper, wherein the temperature in the dryer is maintained at 140-150 ℃, and the retention time is 15-20 minutes. Thus, a refined polyphenylene sulfide resin product is obtained, and the molecular weight of the polymer is measured to be 41000-45000, and the ash content is 1.09 thousandth.
Example 2
A continuous washing and purifying technology for polyarylene sulfide resin comprises the following steps:
(1) after the polycondensation reaction of the polyphenylene sulfide resin is finished, when the temperature is reduced to 200 ℃, a high-temperature slurry pump and cloth are utilized to convey resin slurry to a continuously running belt filter, solid-liquid separation is firstly carried out on the belt filter, the separated liquid enters a high-temperature filtrate storage tank, the solid resin is continuously conveyed to a solvent washing section of a belt, 18 wt% of 150 ℃ hot solvent is used for continuously spraying, washing and filtering the solid, the filtered liquid enters the solvent storage tank, the solid is continuously conveyed to a nitrogen purging section, and a filter cake is purged by high-purity nitrogen with constant flow.
(2) And (2) continuously conveying the filter cake obtained by sweeping in the step (1) to a dissolved salt slurry mixing tank by using a positioning scraper, simultaneously adding dilute brine with the mass being 6 times that of the feed inlet, adding 0.003 wt% of ethylene oxide-propylene oxide block copolymer nonionic surfactant into soft water, keeping the liquid level in the slurry mixing tank constant, keeping the temperature at about 85-90 ℃, and keeping the material for 30 min.
(3) And (3) extracting slurry subjected to water washing and size mixing in the step (2) from the tank bottom, continuously conveying the slurry to a closed belt filter, firstly performing solid-liquid separation, allowing liquid to enter a strong brine storage tank to recover industrial byproduct salt, continuously conveying the solid to a process soft water spraying section, spraying the solid at a high speed by using 18 wt% of soft water, allowing filtrate of the spraying section to enter a dilute brine storage tank to be recycled as a solvent for next batch of water washing and size mixing, and continuously conveying a filter cake to a stripping section.
(4) And (4) sending the filter cake obtained in the step (3), namely refined polyphenylene sulfide wet resin, to an airflow dryer through a scraper, wherein the drying temperature is 160-170 ℃, and the retention time is 5-10 minutes. Thus, a refined polyphenylene sulfide resin product is obtained, and the molecular weight of the polymer is measured to be 39000-43000, and the ash content is 1.11 per mill.
Example 3
A continuous washing and purifying technology for polyarylene sulfide resin comprises the following steps:
(1) after the polycondensation reaction of the polyphenylene sulfide resin is finished, when the temperature is reduced to 250 ℃, a high-temperature slurry pump and cloth are utilized to convey resin slurry to a continuously running belt filter, solid-liquid separation is firstly carried out on the belt filter, the separated liquid enters a high-temperature filtrate storage tank, the solid resin is continuously conveyed to a solvent washing section of a belt, 15 wt% of 180 ℃ hot solvent is used for continuously spraying, washing and filtering the solid, the filtered liquid enters the solvent storage tank, the solid is continuously conveyed to a nitrogen purging section, and a filter cake is purged by high-purity nitrogen with constant flow.
(2) And (2) continuously conveying the filter cake obtained by sweeping in the step (1) to a dissolved salt slurry mixing tank by using a positioning scraper, simultaneously adding 7 times of soft water by mass into a feed inlet, adding 0.004 wt% of amide surfactant into the soft water, keeping the liquid level in the slurry mixing tank constant, maintaining the temperature at about 85-90 ℃, and keeping the material retention time for 30 min.
(3) And (3) extracting slurry subjected to water washing and size mixing in the step (2) from the tank bottom, continuously conveying the slurry to a closed belt filter, performing solid-liquid separation, allowing liquid to enter a strong brine storage tank (namely, a filtrate temporary storage tank 4) to recover industrial byproduct salt, continuously conveying the solid to a process soft water spraying section, spraying the solid at a high speed by adopting 15 wt% of soft water, allowing filtrate in the spraying section to enter a dilute brine storage tank (namely, a filtrate temporary storage tank 5) to be recycled as a solvent for next batch of water washing and size mixing, and continuously conveying a filter cake to a stripping section.
(4) And (4) sending the filter cake obtained in the step (3), namely refined polyphenylene sulfide wet resin, to a fluidized bed dryer through a scraper, wherein the temperature in the dryer is maintained at 130-140 ℃, and the retention time is 25-30 minutes. Thus, a refined polyphenylene sulfide resin product is obtained, and the molecular weight of the polymer is measured to be 43000-47000, and the ash content is 1.05%.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (10)
1. A continuous scrubbing purification system for polyarylene sulfide resins, comprising:
the first closed belt filter is obliquely and upwards arranged from the feed inlet to the discharge outlet and sequentially comprises a filtering section, a solvent washing section, a nitrogen purging section and a stripping section from bottom to top;
a feed inlet of the dissolved salt slurry mixing tank is connected with a discharge outlet of the first closed belt filter, and a stirring assembly is arranged in the dissolved salt slurry mixing tank;
a feed inlet of the second closed belt filter is connected with a discharge outlet of the dissolved salt slurry mixing tank and is arranged from the feed inlet to the discharge outlet in an inclined upward manner, and the second closed belt filter sequentially comprises a filtering section, a solvent washing section and a stripping section from bottom to top;
and a feed inlet of the gas dryer is connected with a discharge outlet of the second closed belt filter.
2. The polyarylene sulfide resin continuous washing purification system according to claim 1, wherein a feed inlet of the first closed belt filter is provided with a distributor, and the polymer slurry is conveyed into the distributor by a high temperature slurry pump and enters the first closed belt filter from the distributor.
3. The system for continuously washing and purifying polyarylene sulfide resin as recited in claim 1, wherein said first closed belt filter comprises a filter belt inclined from bottom to top, said first closed belt filter being provided with a solvent spray washing assembly above a solvent washing section; a high-pressure nitrogen blowing assembly is arranged above the nitrogen blowing section of the first closed belt filter; and a positioning scraper matched with a filter belt is arranged at the stripping section of the first closed belt filter.
4. The system for continuously washing and purifying polyarylene sulfide resin as claimed in claim 1, wherein the first closed belt filter is provided with liquid outlets at the filtering section, the solvent washing section and the nitrogen purging section, and the three liquid outlets are respectively connected with a filtrate temporary storage tank.
5. The polyarylene sulfide resin continuous washing purification system according to claim 1, wherein the feed inlet of the second closed belt filter is connected with the discharge outlet of the dissolved salt slurrying tank through a pipeline and a high temperature slurry pump.
6. The system for continuously washing and purifying polyarylene sulfide resin as claimed in claim 1, wherein the second closed belt filter comprises a filter belt which is obliquely arranged from bottom to top, and the second closed belt filter is provided with a process soft water spray washing assembly above the solvent washing section; and a positioning scraper matched with a filter belt is arranged at the stripping section of the second closed belt filter.
7. The system for continuously washing and purifying polyarylene sulfide resin as claimed in claim 1, wherein the first closed belt filter is provided with liquid outlet pipes at the filtering section and the solvent washing section respectively, and the two liquid outlet pipes are connected with filtrate temporary storage tanks respectively.
8. The continuous scrubbing purification system for polyarylene sulfide resin as recited in claim 1, wherein the gas dryer comprises an ebullated bed or a flash dryer.
9. The system for continuously washing and purifying polyarylene sulfide resin as claimed in claim 1, wherein a cyclone is connected to an outlet end of the gas dryer, an induced draft fan is arranged at an air inlet of the cyclone, and a gas filtering heater is arranged at an air inlet of the gas dryer.
10. A method for continuously washing and purifying polyarylene sulfide resin is characterized by comprising the following steps:
(1) after the poly (arylene sulfide) resin synthesis polycondensation reaction is finished, uniformly distributing polymer slurry at a certain temperature (150-250 ℃) on a filter belt of a first closed belt filter which continuously runs by using a high-temperature slurry pump and a distributor; with the movement of the filter belt, the filter belt sequentially passes through a filtering section, a solvent washing section, a nitrogen purging section and a stripping section; the high-temperature filtrate separated in the filtering section is dissolved with a catalyst, an auxiliary agent and an active oligomer, and directly circulated to the condensation reaction process for recycling; in a solvent washing section, continuously spraying, washing and filtering a filter cake on a filter belt by using a hot solvent (120-180 ℃), and removing the solvent and the auxiliary agent remained on the filter cake; part of the filtrate of the solvent washing section is recycled to the condensation reaction process, and is recycled, and part of the filtrate is removed from the solvent for recovery; in the nitrogen purging section, purging the filter cake by using high-purity nitrogen to remove the residual solvent in the filter cake; in the stripping section, a positioning scraper is utilized to strip filter cake solids which are filtered and washed, and the main components of the filter cake solids are polyarylene sulfide resin and sodium chloride;
(2) continuously feeding the filter cake solid obtained in the step (1) and process soft water/dilute brine into a salt dissolving and pulp mixing tank according to a certain proportion, and fully stirring and dissolving sodium chloride salt in the filter cake solid under stirring and temperature control of 30-80 ℃; adding a low-foaming amide surfactant or an ethylene oxide-propylene oxide block copolymer nonionic surfactant into process soft water or dilute brine to help wetting and improve the salt-dissolving washing effect;
(3) maintaining the continuous and uniform stirring, temperature and liquid level in the salt dissolving and pulp mixing tank in the step (2); continuously extracting slurry by using a slurry pump at the bottom of the dissolved salt size mixing tank, conveying the slurry to a second closed belt filter, and uniformly distributing the slurry on a continuously running filter belt; the filter belt moves forwards and sequentially passes through a filtering section, a process soft water spraying and washing section and a stripping section; the filtrate obtained in the filtering section, namely the strong brine, continuously enters a strong brine storage tank and is sent to be refined and recycled to obtain sodium chloride; the filtrate in the soft water spraying and washing section is dilute brine containing a small amount of sodium chloride, and is circulated to the dissolved salt pulp mixing tank in the step (2) for recycling; the stripped purified filter cake is refined polyarylene sulfide resin and is continuously sent to a resin drying procedure for drying;
(4) and (4) continuously feeding the wet resin obtained after the water washing in the step (3) into a drying process, and drying by adopting a fluidized bed or an air flow dryer. Controlling the drying temperature of the resin to be 130-150 ℃ during the drying of the fluidized bed, and keeping the resin for 15-40 minutes; when the air flow drying is adopted, the drying temperature is 150-180 ℃, the retention time is 3-10 minutes, and the refined PPS resin is obtained after the drying is finished.
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| CN113680128B (en) | 2023-06-06 |
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