CN113680128B - 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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- CN113680128B CN113680128B CN202110850039.2A CN202110850039A CN113680128B CN 113680128 B CN113680128 B CN 113680128B CN 202110850039 A CN202110850039 A CN 202110850039A CN 113680128 B CN113680128 B CN 113680128B
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- 238000005406 washing Methods 0.000 title claims abstract description 79
- 229920005989 resin Polymers 0.000 title claims abstract description 77
- 239000011347 resin Substances 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 41
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229920000412 polyarylene Polymers 0.000 title claims abstract description 36
- 239000002002 slurry Substances 0.000 claims abstract description 61
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000002904 solvent Substances 0.000 claims abstract description 53
- 239000012065 filter cake Substances 0.000 claims abstract description 43
- 238000002156 mixing Methods 0.000 claims abstract description 37
- 238000001914 filtration Methods 0.000 claims abstract description 34
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 29
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 26
- 238000010926 purge Methods 0.000 claims abstract description 24
- 150000003839 salts Chemical class 0.000 claims abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 21
- 238000006482 condensation reaction Methods 0.000 claims abstract description 13
- 239000011780 sodium chloride Substances 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 230000000694 effects Effects 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 37
- 239000007787 solid Substances 0.000 claims description 30
- 239000012267 brine Substances 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 28
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 28
- 239000000706 filtrate Substances 0.000 claims description 27
- 239000008234 soft water Substances 0.000 claims description 26
- 238000003860 storage Methods 0.000 claims description 26
- 239000007921 spray Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000000746 purification Methods 0.000 claims description 11
- 238000005507 spraying Methods 0.000 claims description 11
- 229920000642 polymer Polymers 0.000 claims description 10
- 238000006068 polycondensation reaction Methods 0.000 claims description 8
- 238000007664 blowing Methods 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 239000012752 auxiliary agent Substances 0.000 claims description 6
- 150000001408 amides Chemical class 0.000 claims description 5
- 239000002736 nonionic surfactant Substances 0.000 claims description 4
- 229920005682 EO-PO block copolymer Polymers 0.000 claims description 3
- 125000004122 cyclic group Chemical group 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000005187 foaming Methods 0.000 claims description 3
- -1 poly (arylene sulfide Chemical compound 0.000 claims description 3
- 238000004537 pulping Methods 0.000 claims description 3
- 239000013557 residual solvent Substances 0.000 claims description 3
- 238000009736 wetting Methods 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 238000010924 continuous production Methods 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 11
- 239000000047 product Substances 0.000 abstract description 9
- 239000007810 chemical reaction solvent Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 9
- 239000004734 Polyphenylene sulfide Substances 0.000 description 8
- 229920000069 polyphenylene sulfide Polymers 0.000 description 8
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N NMP Substances CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 5
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 description 5
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052979 sodium sulfide Inorganic materials 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- GNOIPBMMFNIUFM-UHFFFAOYSA-N hexamethylphosphoric triamide Chemical compound CN(C)P(=O)(N(C)C)N(C)C GNOIPBMMFNIUFM-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000001632 sodium acetate Substances 0.000 description 2
- 235000017281 sodium acetate Nutrition 0.000 description 2
- XURIQWBLYMJSLS-UHFFFAOYSA-N 1,4,7,10-tetrazacyclododecan-2-one Chemical compound O=C1CNCCNCCNCCN1 XURIQWBLYMJSLS-UHFFFAOYSA-N 0.000 description 1
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000011825 aerospace material Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 229920006258 high performance thermoplastic Polymers 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000003880 polar aprotic solvent Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Images
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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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The invention discloses a continuous washing and purifying system and a purifying method for polyarylene sulfide resin, comprising the following steps: (1) Filtering the polyarylene sulfide resin through a first closed belt filter, washing with a hot solvent, purging with high-temperature nitrogen, and stripping to obtain a filter cake containing the polyarylene sulfide resin and sodium chloride; (2) The filter cake is fully dissolved and slurried by a salt dissolving and slurry mixing tank; (3) Filtering the dissolved slurry by a second closed belt filter, washing the dissolved slurry by a solvent, and stripping the dissolved slurry to obtain wet resin; (4) The wet resin obtained by the gas dryer was dried to obtain a purified PPS resin. The continuous closed belt filter is adopted, so that the working procedures of filtering, washing, purging and the like are continuously finished on the continuous filter belt; the reaction solvent, the oligomer and the catalyst are efficiently separated and directly used for condensation reaction; the resin after washing and filtering is continuously dried, and the resin has high working efficiency, good separation effect, high purity of resin products and low cost, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of purification of high polymer products, and particularly relates to a continuous washing purification system and a purification method of polyarylene sulfide resin, which aim to obtain high-quality polyarylene sulfide resin products.
Background
Polyarylene sulfide is a novel high-performance thermoplastic resin, has excellent electrical insulation, chemical corrosion resistance, heat resistance and flame retardance, has been widely applied to the fields of automobiles, electronic appliances, machinery, rail transit, aerospace, military industry and the like, is called as "the sixth engineering plastic of the world", is one of the eighth aerospace materials, is a strategic new material which is greatly supported and developed in China, and the synthetic method thereof is valued by various countries.
The existing method for synthesizing polyarylene sulfide mainly comprises a sodium sulfide method, namely, condensation reaction is carried out under alkaline condition by taking dihalobenzene, sodium sulfide/sodium hydrosulfide as raw materials and lithium chloride as a catalyst and NMP as a catalyst; 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 is finished must be washed and purified. In the conventional polyarylene sulfide resin production process, 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. Thus, there is a need for more efficient methods for obtaining pure polyarylene sulfide resins, which are critical for the production of polyarylene sulfide resins.
Disclosure of Invention
The invention provides a continuous washing purification system and a purification method of polyarylene sulfide resin, which are characterized in that reasonable process conditions are controlled by adopting a continuous closed belt filter, and the working procedures of filtering, washing, purging and the like are continuously finished on a continuous filter belt; high-efficiency separation of reaction solvent, oligomer and catalyst, and direct use in condensation reaction; washing the filtered resin, and continuously drying in a drying process; the method has the advantages of high working efficiency, good separation effect, high purity of resin products, low cost and suitability for industrial production.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a continuous scrubbing purification system for polyarylene sulfide resin, comprising:
the first airtight belt filter is obliquely 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;
the feeding port of the salt dissolving and slurry mixing tank is connected with the discharging port of the first airtight belt filter, and a stirring assembly is arranged in the salt dissolving and slurry mixing tank;
the feed inlet of the second closed belt filter is connected with the discharge outlet of the salt dissolving and pulping tank, and is obliquely upwards arranged from the feed inlet to the discharge outlet, and the second closed belt filter sequentially comprises a filtering section, a solvent washing section and a stripping section from bottom to top;
and the feed inlet of the gas dryer is connected with the discharge outlet of the second airtight 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 the 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 spray washing assembly is arranged above the solvent washing section of the first closed belt filter; a high-pressure nitrogen blowing component is arranged above the nitrogen blowing section of the first closed belt filter; the first airtight belt filter is provided with a positioning scraper matched with the filter belt at the stripping section.
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 filtrate temporary storage tanks respectively.
As a further description of the above technical solution: and the feed inlet of the second airtight belt filter is connected with the discharge outlet of the salt-dissolving 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 spray washing assembly is arranged above the solvent washing section of the second closed belt filter; the second airtight belt filter is provided with a positioning scraper matched with the filter belt at the stripping section.
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 a gas flow dryer.
As a further description of the above technical solution: the outlet end of the gas dryer is connected with a cyclone separator, an induced draft fan is arranged at the air inlet of the cyclone separator, and a gas filtering heater is arranged at the air inlet of the gas dryer.
A continuous washing and purifying method of polyarylene sulfide resin comprises the following steps:
(1) After the poly (arylene sulfide) resin is subjected to the synthesis polycondensation reaction, uniformly distributing polymer slurry with 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; along with the movement of the filter belt, the filter belt sequentially passes through a filter section, a solvent washing section, a nitrogen purging section and a stripping section; the high Wen Lvye separated in the filtering section is dissolved with a catalyst, an auxiliary agent and an active oligomer, and is directly circulated to the condensation reaction process for cyclic application; continuously spraying, washing and filtering a filter cake on a filter belt in a solvent washing section by using a hot solvent (120-180 ℃) to remove the solvent and the auxiliary agent remained on the filter cake; part of filtrate of the solvent washing section is recycled to the condensation reaction process, and part of the filtrate is recycled; in the nitrogen purging section, utilizing high-purity nitrogen to purge the filter cake, and removing the residual solvent in the filter cake; in the stripping section, a positioning scraper is utilized to strip, filter and wash filter cake solids, 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 size mixing tank according to a certain proportion, and fully stirring and dissolving sodium chloride in the filter cake solid at the temperature of 30-80 ℃ under stirring; the low-foaming amide surfactant or the ethylene oxide-propylene oxide block copolymer nonionic surfactant is added into the process soft water or the 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/m 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass of the water phase is 4-7 times of the solid mass of the filter cake; temperature in salt-dissolving size mixing tankThe temperature is 30-80 ℃, and the material retention time is 30 minutes;
(3) Maintaining continuous and uniform stirring, temperature and liquid level in the salt-dissolving size mixing tank in the step (2); continuously collecting slurry by using a slurry pump at the bottom of the salt dissolving slurry mixing tank, and delivering the slurry to a second closed belt filter to uniformly distribute the slurry on a continuously running filter belt; sequentially passing through a filtering section, a process soft water spray washing section and a stripping section along with the forward movement of the filter belt; continuously feeding the filtrate obtained in the filtering section, namely strong brine into a strong brine storage tank, and delivering the strong brine to refine and recycle sodium chloride; the filtrate in the soft water spray washing section is dilute brine containing a small amount of sodium chloride, and the dilute brine is recycled to the salt-dissolving size mixing tank in the step (2); the stripped purified filter cake is refined polyarylene sulfide resin, and is continuously sent to a resin drying procedure for drying;
(4) And (3) continuously entering 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. The resin drying temperature is controlled between 130 and 150 ℃ and the residence time is 15 to 40 minutes during the fluidized bed drying; when adopting air flow drying, the drying temperature is 150-180 ℃ and the residence time is 3-10 minutes.
The invention has the following beneficial effects:
1. the washing solvent adopted by the invention can remove most of mixed oligomers and salts in the resin after the condensation reaction is finished, and solves the problems of low purity and poor color of the product after the traditional resin washing is finished.
2. The method realizes 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 percent, and the content of the oligomer is less than or equal to 3 percent.
Drawings
FIG. 1 is a schematic diagram of a continuous washing purification system for polyarylene sulfide resin according to the present invention.
Reference numerals: 1-a distributing device; 2-a solvent spray wash assembly; 3-a high pressure nitrogen blowing assembly; 4-setting an outer scraper; 5-a salt dissolving size mixing tank; 6-a gas dryer; 7-a gas filtration heater; 8-cyclone separator; 9-induced draft fan; 10-a filtrate buffer tank; 11-a filter belt; 12-high temperature slurry pump.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In industry, anhydrous sodium sulfide, crystalline sodium sulfide or sodium hydrosulfide and sodium hydrosulfide aqueous solution are used as sulfur source compounds, paradichlorobenzene, parachlorobiphenyl and the like are used as chlorine-containing monomers, and the polyarylene sulfide resin is obtained by high-temperature polycondensation reaction in the presence of lithium chloride or sodium acetate in a polar aprotic solvent NMP or HMPTA. The resin contains a large amount of impurities such as oligomers, inorganic salts, pigments and the like, which seriously affect the processing performance, application performance and electrical performance of the resin, deteriorate 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 washing purification system for polyarylene sulfide resin, comprising:
the first airtight belt filter is obliquely 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;
the feeding port of the salt dissolving and slurry mixing tank is connected with the discharging port of the first airtight belt filter, and a stirring assembly is arranged in the salt dissolving and slurry mixing tank;
the feed inlet of the second closed belt filter is connected with the discharge outlet of the salt dissolving and pulping tank, and is obliquely upwards arranged from the feed inlet to the discharge outlet, and the second closed belt filter sequentially comprises a filtering section, a solvent washing section and a stripping section from bottom to top;
and the feed inlet of the gas dryer is connected with the discharge outlet of the second airtight 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 spray washing assembly 2 is arranged above a solvent washing section of the first closed belt filter; the first closed belt filter is provided with a high-pressure nitrogen blowing component 3 above the nitrogen blowing section; the first closed belt filter is provided with a positioning scraper 4 matched with the filter belt at the stripping section.
In this embodiment, the first closed belt filter is provided with liquid outlet pipes in the filtering section, the solvent washing section and the nitrogen purging section, and the three liquid outlet pipes are respectively connected with a filtrate temporary storage tank 10.
In this embodiment, the feed inlet of the second closed belt filter is connected to the discharge outlet of the salt-dissolving slurry mixing tank through a pipeline and the high-temperature slurry pump 12.
In the embodiment, the second closed belt filter comprises a filter belt obliquely arranged from bottom to top, and a process soft water spray washing assembly is arranged above the solvent washing section of the second closed belt filter; the second airtight belt filter is provided with a positioning scraper matched with the filter belt at the stripping section.
In this embodiment, the first closed belt filter is provided with liquid outlet pipes in the filtering section and the solvent washing section, and the two liquid outlet pipes are respectively connected with a filtrate temporary storage tank.
In this embodiment, the gas dryer 6 comprises an ebullated bed or a gas flow dryer.
In this embodiment, the outlet end of the gas dryer 6 is connected with a cyclone separator 8, an air inlet of the cyclone separator 8 is provided with an induced draft fan 9, and an air inlet of the gas dryer 8 is provided with a gas filtering heater 7.
A continuous washing and purifying method of polyarylene sulfide resin comprises the following steps:
(1) After the poly (arylene sulfide) resin is synthesized and subjected to polycondensation, uniformly distributing polymer slurry with 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; along with the movement of the filter belt, the filter belt sequentially passes through a filter section, a solvent washing section, a nitrogen purging section and a stripping section; the high Wen Lvye separated in the filtering section is dissolved with a catalyst, an auxiliary agent and an active oligomer, and is directly circulated to the condensation reaction process for cyclic application; continuously spraying, washing and filtering a filter cake on a filter belt in a solvent washing section by using a hot solvent (120-180 ℃) to remove the solvent and the auxiliary agent remained on the filter cake; part of filtrate of the solvent washing section is recycled to the condensation reaction process, and part of the filtrate is recycled; in the nitrogen purging section, utilizing high-purity nitrogen to purge the filter cake, and removing the residual solvent in the filter cake; in the stripping section, a positioning scraper 4 is utilized to strip, filter and wash filter cake solids, 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 size mixing tank according to a certain proportion, and fully stirring and dissolving sodium chloride in the filter cake solid at the temperature of 30-80 ℃ under stirring; the low-foaming amide surfactant or the ethylene oxide-propylene oxide block copolymer nonionic surfactant is added into the process soft water or the 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/m 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass of the water phase is 4-7 times of the solid mass of the filter cake; the temperature in the salt dissolving size mixing tank is 30-80 ℃, and the material retention time is 30 minutes;
(3) Maintaining continuous and uniform stirring, temperature and liquid level in the salt-dissolving size mixing tank in the step (2); continuously collecting slurry by using a slurry pump at the bottom of the salt dissolving slurry mixing tank, and delivering the slurry to a second closed belt filter to uniformly distribute the slurry on a continuously running filter belt; sequentially passing through a filtering section, a process soft water spray washing section and a stripping section along with the forward movement of the filter belt; continuously feeding the filtrate obtained in the filtering section, namely strong brine into a strong brine storage tank, and delivering the strong brine to refine and recycle sodium chloride; the filtrate in the soft water spray washing section is dilute brine containing a small amount of sodium chloride, and the dilute brine is recycled to the salt-dissolving size mixing tank in the step (2); the stripped purified filter cake is refined polyarylene sulfide resin, and is continuously sent to a resin drying procedure for drying;
(4) And (3) continuously entering 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. The resin drying temperature is controlled between 130 and 150 ℃ and the residence time is 15 to 40 minutes during the fluidized bed drying; when adopting air flow drying, the drying temperature is 150-180 ℃ and the residence time is 3-10 minutes.
Example 1
A continuous washing and purifying technology of polyarylene sulfide resin comprises the following steps:
adding sodium sulfide, sodium hydrosulfide or sodium hydrosulfide aqueous solution into a condensation reaction kettle, carrying out high-temperature polycondensation reaction at 150-280 ℃ to obtain polyarylene sulfide resin slurry, wherein the dihalogenated aromatic hydrocarbon, sodium hydroxide, solvent NMP or HMPTA, lithium chloride or sodium acetate;
(1) After the polycondensation reaction of the polyphenylene sulfide resin is finished, when the temperature is reduced to 150 ℃, the slurry of the polyarylene sulfide resin is conveyed to a first closed belt filter which continuously runs by utilizing a high-temperature slurry pump and cloth, solid-liquid separation is firstly carried out on the first closed belt filter, liquid obtained by separation enters a high Wen Lvye storage tank (namely a filtrate temporary storage tank 1), solid resin is continuously conveyed to a solvent washing section of a belt, 20wt% of hot solvent at 120 ℃ 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) Continuously conveying the filter cake obtained by purging in the step (1) to a salt-dissolving size mixing tank by using a positioning scraper, adding soft water with 5 times of mass into a feed inlet, adding 0.002wt% of amide surfactant into the soft water, keeping the liquid level in the size mixing tank constant, and keeping the temperature at about 85-90 ℃ and the material residence time at 30min.
(3) And (3) extracting slurry subjected to water washing and size mixing in the step (2) through a tank bottom, continuously conveying the slurry to a closed belt filter, firstly, carrying out solid-liquid separation, enabling liquid to enter a strong brine storage tank to recover industrial byproduct salt, continuously conveying the solid to a process soft water spraying section, adopting 20wt% soft water to spray the solid at a high speed, enabling filtrate of the spraying section to enter the weak brine storage tank to serve as a solvent for water washing and size mixing of the next batch for recycling, and continuously conveying a filter cake to a stripping section.
(4) And (3) conveying the filter cake obtained in the step (3) to a fluidized bed dryer through a scraper, wherein the temperature in the dryer is kept between 140 and 150 ℃ and the retention time is 15 to 20 minutes. Thus, a purified polyphenylene sulfide resin product was obtained, and the molecular weight of the polymer was measured to be 41000 to 45000, and the ash content was 1.09%.
Example 2
A continuous washing and purifying technology of 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 ℃, the resin slurry is conveyed to a continuously running belt filter by utilizing a high-temperature slurry pump and cloth, solid-liquid separation is firstly carried out on the belt filter, the separated liquid enters a high Wen Lvye storage tank, the solid resin is continuously conveyed to a solvent washing section of a belt, the solid is continuously sprayed, washed and filtered by using 18wt% of hot solvent at 150 ℃, 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 using high-purity nitrogen with constant flow.
(2) Continuously conveying the filter cake obtained by purging in the step (1) to a salt dissolving and slurry mixing tank by using a positioning scraper, adding 6 times of dilute brine by mass into a feed inlet, adding 0.003wt% of ethylene oxide-propylene oxide segmented 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 residence time for 30min.
(3) And (3) extracting slurry subjected to water washing and size mixing in the step (2) through a tank bottom, continuously conveying the slurry to a closed belt filter, firstly, carrying out solid-liquid separation, enabling 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 soft water with the weight percent, enabling filtrate of the spraying section to enter the weak brine storage tank to serve as a solvent for water washing and size mixing of the next batch, recycling, and continuously conveying a filter cake to a stripping section.
(4) The filter cake obtained in the step (3) is the refined polyphenylene sulfide wet resin, and is sent to an air flow dryer through a scraper, the drying temperature is 160-170 ℃, and the residence time is 5-10 minutes. Thus, a refined polyphenylene sulfide resin product is obtained, and the molecular weight of the polymer is 39000-43000 and the ash content is 1.11 per mill.
Example 3
A continuous washing and purifying technology of 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 ℃, the resin slurry is conveyed to a continuously running belt filter by utilizing a high-temperature slurry pump and cloth, solid-liquid separation is firstly carried out on the belt filter, the separated liquid enters a high Wen Lvye storage tank, the solid resin is continuously conveyed to a solvent washing section of a belt, the solid is continuously sprayed, washed and filtered by using 15wt% of hot solvent at 180 ℃, 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 using high-purity nitrogen with constant flow.
(2) Continuously conveying the filter cake obtained by purging in the step (1) to a salt-dissolving size mixing tank by using a positioning scraper, simultaneously adding 7 times of soft water by mass into a feed inlet, adding 0.004wt% of amide surfactant into the soft water, keeping the liquid level in the size mixing tank constant, and keeping the temperature at about 85-90 ℃ and the material residence time at 30min.
(3) The slurry after washing and size mixing in the step (2) is extracted from the tank bottom and is continuously sent to a closed belt filter, firstly, through solid-liquid separation, liquid enters a strong brine storage tank (namely a filtrate temporary storage tank 4) to recycle industrial byproduct salt, the solid is continuously transported to a process soft water spraying section, 15wt% soft water is adopted to spray the solid at a high speed, filtrate of the spraying section enters a weak brine storage tank (namely a filtrate temporary storage tank 5) to be recycled as a solvent for washing and size mixing of the next batch, and a filter cake is continuously transported to a stripping section.
(4) And (3) conveying the filter cake obtained in the step (3) to a fluidized bed dryer through a scraper, wherein the temperature in the dryer is kept between 130 and 140 ℃ and the retention time is 25 to 30 minutes. Thus, a purified polyphenylene sulfide resin product was obtained, and the molecular weight of the polymer was found to be 43000 to 47000, and the ash content was found to be 1.05%.
Finally, it should be noted that: the foregoing description is only illustrative of the preferred embodiments of the present invention, and 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 described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements or changes may be made without departing from the spirit and principles of the present invention.
Claims (1)
1. A continuous process for the wash purification of polyarylene sulfide resins, comprising a continuous wash purification system for polyarylene sulfide resins, the system comprising:
the first airtight belt filter is obliquely 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;
the feeding port of the salt dissolving and slurry mixing tank is connected with the discharging port of the first airtight belt filter, and a stirring assembly is arranged in the salt dissolving and slurry mixing tank;
the feed inlet of the second closed belt filter is connected with the discharge outlet of the salt dissolving and pulping tank, and is obliquely upwards arranged from the feed inlet to the discharge outlet, and the second closed belt filter sequentially comprises a filtering section, a solvent washing section and a stripping section from bottom to top;
the feed inlet of the gas dryer is connected with the discharge outlet of the second airtight belt filter;
the polymer slurry is conveyed into the distributor through a high-temperature slurry pump, and enters the first closed belt filter from the distributor;
the first closed belt filter comprises a filter belt which is obliquely arranged from bottom to top, and a solvent spray washing assembly is arranged above the solvent washing section of the first closed belt filter; a high-pressure nitrogen blowing component is arranged above the nitrogen blowing section of the first closed belt filter; the first closed belt filter is provided with a positioning scraper matched with the filter belt at the stripping section;
the first closed belt filter is provided with liquid outlet pipes respectively at the filtering section, the solvent washing section and the nitrogen purging section, and the three liquid outlet pipes are respectively connected with a filtrate temporary storage tank;
the feed inlet of the second closed belt filter is connected with the discharge outlet of the salt-dissolving slurry mixing tank through a pipeline and a high-temperature slurry pump;
the second closed belt filter comprises a filter belt which is obliquely arranged from bottom to top, and a process soft water spray washing assembly is arranged above the solvent washing section of the second closed belt filter; the second airtight belt filter is provided with a positioning scraper matched with the filter belt at the stripping section;
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; the gas dryer comprises an ebullated bed or a gas stream dryer;
the outlet end of the gas dryer is connected with a cyclone separator, an induced draft fan is arranged at the air inlet of the cyclone separator, and a gas filtering heater is arranged at the air inlet of the gas dryer; characterized in that the method comprises the following steps:
(1) After the poly (arylene sulfide) resin is subjected to the synthesis polycondensation reaction, uniformly distributing polymer slurry with 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; along with the movement of the filter belt, the filter belt sequentially passes through a filter section, a solvent washing section, a nitrogen purging section and a stripping section; the high Wen Lvye separated in the filtering section is dissolved with a catalyst, an auxiliary agent and an active oligomer, and is directly circulated to the condensation reaction process for cyclic application; continuously spraying, washing and filtering a filter cake on a filter belt in a solvent washing section by using a hot solvent (120-180 ℃) to remove the solvent and the auxiliary agent remained on the filter cake; part of filtrate of the solvent washing section is recycled to the condensation reaction process, and part of the filtrate is recycled; in the nitrogen purging section, utilizing high-purity nitrogen to purge the filter cake, and removing the residual solvent in the filter cake; in the stripping section, a positioning scraper is utilized to strip, filter and wash filter cake solids, 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 size mixing tank according to a certain proportion, and fully stirring and dissolving sodium chloride in the filter cake solid at the temperature of 30-80 ℃ under stirring; the low-foaming amide surfactant or the ethylene oxide-propylene oxide block copolymer nonionic surfactant is added into the process soft water or the dilute brine to help wetting and improve the salt-dissolving washing effect;
(3) Maintaining continuous and uniform stirring, temperature and liquid level in the salt-dissolving size mixing tank in the step (2); continuously collecting slurry by using a slurry pump at the bottom of the salt dissolving slurry mixing tank, and delivering the slurry to a second closed belt filter to uniformly distribute the slurry on a continuously running filter belt; sequentially passing through a filtering section, a process soft water spray washing section and a stripping section along with the forward movement of the filter belt; continuously feeding the filtrate obtained in the filtering section, namely strong brine into a strong brine storage tank, and delivering the strong brine to refine and recycle sodium chloride; the filtrate in the soft water spray washing section is dilute brine containing a small amount of sodium chloride, and the dilute brine is recycled to the salt-dissolving size mixing tank in the step (2); the stripped purified filter cake is refined polyarylene sulfide resin, and is continuously sent to a resin drying procedure for drying;
(4) And (3) continuously entering 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. The resin drying temperature is controlled between 130 and 150 ℃ and the residence time is 15 to 40 minutes during the fluidized bed drying; when air flow drying is adopted, the drying temperature is 150-180 ℃, the residence time is 3-10 minutes, and the refined PPS resin is obtained after the drying is finished.
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