CN116478403A - Polysulfone resin production process and polysulfone resin production system - Google Patents
Polysulfone resin production process and polysulfone resin production system Download PDFInfo
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- CN116478403A CN116478403A CN202310365337.1A CN202310365337A CN116478403A CN 116478403 A CN116478403 A CN 116478403A CN 202310365337 A CN202310365337 A CN 202310365337A CN 116478403 A CN116478403 A CN 116478403A
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- pure water
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- 229920002492 poly(sulfone) Polymers 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 32
- 239000011347 resin Substances 0.000 title claims abstract description 29
- 229920005989 resin Polymers 0.000 title claims abstract description 29
- 238000003825 pressing Methods 0.000 claims abstract description 102
- 239000000463 material Substances 0.000 claims abstract description 69
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 60
- 238000000926 separation method Methods 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000007670 refining Methods 0.000 claims abstract description 28
- 239000012043 crude product Substances 0.000 claims abstract description 26
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000000047 product Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 16
- 238000009875 water degumming Methods 0.000 claims abstract description 16
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 15
- 230000007246 mechanism Effects 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000000605 extraction Methods 0.000 claims abstract description 11
- 238000003809 water extraction Methods 0.000 claims abstract description 11
- 239000012065 filter cake Substances 0.000 claims abstract description 10
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 230000018044 dehydration Effects 0.000 claims abstract description 3
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 10
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 8
- 238000001125 extrusion Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- GPAPPPVRLPGFEQ-UHFFFAOYSA-N 4,4'-dichlorodiphenyl sulfone Chemical compound C1=CC(Cl)=CC=C1S(=O)(=O)C1=CC=C(Cl)C=C1 GPAPPPVRLPGFEQ-UHFFFAOYSA-N 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 5
- 238000012512 characterization method Methods 0.000 claims description 4
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 claims description 3
- -1 biphenol Chemical compound 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000010010 raising Methods 0.000 claims description 2
- 239000013014 purified material Substances 0.000 claims 1
- 238000013461 design Methods 0.000 description 17
- 230000001360 synchronised effect Effects 0.000 description 17
- 230000005540 biological transmission Effects 0.000 description 13
- 238000001914 filtration Methods 0.000 description 12
- 238000011084 recovery Methods 0.000 description 12
- 239000000523 sample Substances 0.000 description 11
- 238000011085 pressure filtration Methods 0.000 description 10
- 230000008859 change Effects 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000001514 detection method Methods 0.000 description 7
- 238000007599 discharging Methods 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 230000006837 decompression Effects 0.000 description 3
- 230000001976 improved effect Effects 0.000 description 3
- 230000006698 induction Effects 0.000 description 3
- 230000001939 inductive effect Effects 0.000 description 3
- 239000000543 intermediate Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 230000008093 supporting effect Effects 0.000 description 3
- 229930185605 Bisphenol Natural products 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000005755 formation reaction Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- IBRQUKZZBXZOBA-UHFFFAOYSA-N 1-chloro-3-(3-chlorophenyl)sulfonylbenzene Chemical compound ClC1=CC=CC(S(=O)(=O)C=2C=C(Cl)C=CC=2)=C1 IBRQUKZZBXZOBA-UHFFFAOYSA-N 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 229920000491 Polyphenylsulfone Polymers 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000010534 nucleophilic substitution reaction Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- 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
- B01D33/15—Filters with filtering elements which move during the filtering operation with rotary plane filtering surfaces
-
- 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
- B01D33/35—Filters with filtering elements which move during the filtering operation with multiple filtering elements characterised by their mutual disposition
-
- 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
- B01D33/64—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element for drying by compression
-
- 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
- B01D33/70—Filters with filtering elements which move during the filtering operation having feed or discharge devices
- B01D33/72—Filters with filtering elements which move during the filtering operation having feed or discharge devices for feeding
-
- 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
- B01D33/80—Accessories
- B01D33/804—Accessories integrally combined with devices for controlling the filtration
-
- 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
- C08G75/20—Polysulfones
- C08G75/23—Polyethersulfones
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Filtration Of Liquid (AREA)
Abstract
The invention discloses a polysulfone resin production process, which comprises the following steps: s1, crude product polymerization, namely putting raw and auxiliary materials into a synthesis kettle to perform crude product polymerization reaction; s2, cooling and crushing: cooling the polymerized crude product in a receiving tank; crushing the material cooled to room temperature, and delivering the crushed material to a product refining process; s3, refining acetone: sending the crushed polymerized crude product into an acetone refining kettle for sulfolane extraction operation; extracting sulfolane; s4, refining pure water: the crude product material after sulfolane removal is subjected to synthesis to form a filter cake through a filter pressing separation mechanism, and then the filter cake is transferred into a pure water refining kettle for pure water extraction; centrifugal dehydration is carried out after pure water refining is completed, and the pure water is sent to a drying process; s5, drying and granulating: heating and drying the refined polysulfone product, and extruding and granulating the polysulfone product in a screw extruder after the water content is lower than three thousandths; finally, the polysulfone finished product is obtained.
Description
Technical Field
The invention relates to the technical field of polysulfone resin production, in particular to a polysulfone resin production process and a polysulfone resin production system.
Background
Polysulfone resin is a special engineering plastic with strong stability, boiling resistance and good dimensional stability, is increasingly adopted in the technical field of industry (medical treatment, electronics, scientific research equipment, water treatment, milk bottles and the like) and is used for replacing the original traditional engineering resin. However, due to the particularity of the polysulfone resin production process, the national production enterprises of the phoenix-like horns are imported by ninety percent of China.
Polysulfone reaction principle: is prepared by taking 4,4' -dichloro diphenyl sulfone, bisphenol intermediates and anhydrous carbonate as raw materials and synthesizing the raw materials in sulfolane solvent. The reaction process adopts nucleophilic substitution method. Is prepared from 4,4' -dichloro diphenyl sulfone and bisphenol intermediate through polycondensation reaction in solvent under the action of alkali carbonate.
The inventor finds that the prior polysulfone resin has low efficiency during production, particularly when a press cake of a synthesized crude product material from which sulfolane is removed is transferred to a pure water refining kettle, the press filtration efficiency of the material is low, and the traditional press filtration mode mostly adopts intermittent press filtration, so that the press filtration is easy to be interrupted, the automation level is low, the manual operation is required, the labor cost is high, and the integral production efficiency is seriously influenced.
Accordingly, the inventor has the problem of providing a polysulfone resin production process and a polysulfone resin production system, which have more practical value, by keeping the experience of design development and actual production in the related industry for many years and researching and improving the existing structure and the defects.
Disclosure of Invention
In order to solve the problems that the prior polysulfone resin in the background art is low in efficiency in production, particularly in the process that a press cake of a sulfolane-removed synthetic crude product material is transferred to a pure water refining kettle, the press filtration efficiency of the material is low, and the conventional press filtration mode mostly adopts intermittent press filtration, so that the press filtration is easy to break, the press filtration process is low in automation level, manual operation is required, the labor cost is high, and the overall production efficiency is seriously affected, the polysulfone resin production process and the polysulfone resin production system are provided.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the polysulfone resin production process is characterized by comprising the following steps:
s1, crude product polymerization, namely putting sulfolane, biphenol, bisphenol A, bisphenol S, carbonate and 4,4' -dichloro diphenyl sulfone serving as raw materials into a synthesis kettle, sealing, heating and raising the temperature, and carrying out crude product polymerization reaction;
s2, cooling and crushing: cooling the polymerized crude product in a receiving tank; crushing the material cooled to room temperature, and delivering the crushed material to a product refining process;
s3, refining acetone: feeding the crushed polymerized crude product into an acetone refining kettle, injecting the extract into the acetone refining kettle, heating by steam with stirring, maintaining at 40 ℃ for 60min, and extracting acetone to complete primary extraction; repeating the steps for 8-12 times normally, and extracting sulfolane completely;
s4, refining pure water: the method comprises the steps of forming a filter cake from sulfolane-removed synthesized crude product materials through a filter pressing separation mechanism, transferring the filter cake into a pure water refining kettle, injecting extract pure water, heating by jacket steam, stirring, maintaining at 90-95 ℃ for 60min, and then extracting water to complete primary pure water extraction; repeating the pure water extraction operation for 8-10 times, removing the mixed inorganic salt in the product, and taking the conductivity in the water as a characterization index; centrifugally dewatering the material subjected to pure water refining by a centrifugal machine, controlling the water content of the dewatered material to be 40%, and conveying the dewatered material to a drying process;
s5, drying and granulating: drying the refined polysulfone product by using a dryer under a negative pressure state by adopting steam heating, and extruding and granulating by using a screw extruder after the water content is lower than three thousandths; finally obtaining polysulfone finished product
Preferably, after the materials in the step S2 are put into a synthesis kettle and sealed, nitrogen replacement is started while heating, and the system is maintained for 60min after heating to 80 ℃; then rapidly heating to 160 ℃ and keeping the temperature of the system above 160 ℃.
Preferably, the sulfolane extraction method in the step S3 includes the following steps: the extract is injected into an acetone refining kettle, heated by steam with stirring, kept at 40 ℃ for 60min, and then acetone is extracted to finish one-time extraction.
Preferably, the pure water extraction method in step S4 includes the steps of: injecting pure water into the extraction liquid, heating the jacket by steam, stirring, maintaining at 90-95 ℃ for 60min, and then pumping out water to finish the primary pure water extraction.
Preferably, the index of the clean removal of the mixed inorganic salt in the product in the step S4 is to take the conductivity in water as a characterization index.
Preferably, the water content of the material after centrifugal dehydration in the step S4 is controlled to be 40%.
The polysulfone resin production system comprises a synthesis kettle, a receiving tank, a crusher, a crude product collecting tank, an acetone refining kettle, a filter pressing separation mechanism, a pure water refining kettle, a dryer and an extrusion granulator, wherein the synthesis kettle, the receiving tank, the crusher, the crude product collecting tank, the acetone refining kettle, the filter pressing separation mechanism, the pure water refining kettle, the dryer and the extrusion granulator are sequentially connected end to end.
Compared with the prior art, the invention has the beneficial effects that:
1. the rotatable design of the separating plate enables each filter pressing cylinder to sequentially move to the lower part of the feeding pipe in a rotating mode, so that automatic feeding during filter pressing in the filter pressing cylinder is realized, and continuous feeding of the feeding pipe is realized; the material can directly enter the lower part of the filter plate in the filter pressing cylinder through the feed inlet on the filter pressing plate, the filter pressing plate can move up and down, automatic filter pressing can be realized through the downward movement of the filter pressing plate, meanwhile, the filter plate can be rotationally opened and closed, solid-liquid separation can be carried out when the filter pressing plate is downward for filter pressing, and meanwhile, after the filter pressing is finished, the automatic separation of a filter cake after the filter pressing can be realized through the rotation of the filter plate; the automatic operation effectively improves the filter pressing efficiency, thereby improving the production efficiency;
2. the design of the reciprocating screw thread can realize the periodical automatic up-and-down movement of the filter pressing plate through the continuous rotation of the filter pressing shaft and the characteristic of the reciprocating screw thread; the design of the synchronous gear and the synchronous rack enables the synchronous gear to continuously rotate under the engagement of the synchronous rack through the rotation of the separating plate, so that the continuous rotation of the filter pressing shaft is realized; the combination of the reciprocating threads, the synchronous gear and the synchronous rack can realize continuous rotation of the separating plate, so that the filter pressing cylinder can be periodically and automatically replaced, the filter pressing efficiency of the filter pressing cylinder is ensured, and meanwhile, the separating plate can rotate and simultaneously, the filter pressing plate can automatically filter and separate materials;
3. the design of the filter press plate, the feed inlet, the torsion spring and the feed plate can ensure that the torsion spring drives the feed plate to seal the feed inlet when no feed is carried out, and the feed plate is extruded and rotated to be opened due to the pressure of materials when the feed is carried out, so that the automatic feed of the materials is realized, and the feed plate can be driven to seal the feed inlet under the elastic action of the torsion spring after the feed is finished, and meanwhile, the sealing performance of the filter press plate during filter pressing is ensured;
4. the design of the detection rod and the induction probe can automatically sense the humidity of the material after press filtration through the induction probe, so that the solid-liquid separation efficiency is judged through the induction probe, and the time for rotating and opening the filter plate is controlled;
5. the design of spring bolt, locating plate and constant head tank, locked groove can make the filter after rotatory closure, stretches out through the spring bolt and block with the locked groove, can realize the fixed of filter, when the contact is fixed, only need with the spring bolt shrink, can realize the dismantlement of filter fixed to rotatory opening.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic illustration of the process flow of the present invention.
Fig. 2 is a schematic perspective view of a separator according to the present invention.
Fig. 3 is a schematic perspective view of the separator plate, filter press cartridge and collection box of the present invention.
Fig. 4 is a schematic perspective view of a filter cartridge and a filter pressing shaft according to the present invention.
Fig. 5 is a schematic perspective view of a filter press plate and a filter press shaft according to the present invention.
Fig. 6 is a schematic diagram of the internal structure of the pressure filter cartridge according to the present invention.
Fig. 7 is an enlarged view of fig. 6 at a in accordance with the present invention.
Fig. 8 is a schematic top perspective view of the collection chamber, discharge orifice and adjustment hydraulic rod of the present invention.
FIG. 9 is a schematic cross-sectional view of the recovery tank and the extension plate of the present invention.
In the figure: 1. a synthesis kettle; 2. a receiving groove; 3. a crusher; 4. a crude product collecting tank; 5. an acetone refining kettle; 6. a filter pressing separation mechanism; 60. a separation box; 61. a feed pipe; 62. a liquid discharge pipe; 63. a driving motor; 631. a rotation shaft; 64. a collection box; 65. a separation plate; 651. a separation tank; 66. a filter pressing shaft; 661. a synchronous rack; 662. a synchronizing gear; 663. a fixing plate; 664. a reciprocating thread; 665. a feed plate; 666. a filter pressing plate; 667. sealing the hose; 668. a support groove; 669. a support rod; 67. pressing the filter cylinder; 671. a filter plate; 68. a collection chamber; 681. a collection plate; 682. adjusting a hydraulic rod; 683. an adjusting plate; 684. a discharge hole; 685. separating the annular plate; 686. an extension plate; 687. a recovery tank; 69. a detection rod; 691. an inductive probe; 692. a transmission member; 693. a protruding block; 694. a connecting piece; 695. a positioning groove; 696. a positioning plate; 697. a locking groove; 698. a bolt; 699. a return spring; 690. an adjustment tank; 7. and (3) a pure water refining kettle.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. 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.
Example 1
Referring to fig. 1-3, a polysulfone resin production system comprises a synthesis kettle 1, a receiving tank 2, a crusher 3, a crude product collecting tank 4, an acetone refining kettle 5, a filter pressing separation mechanism 6, a pure water refining kettle 7, a dryer and an extrusion granulator, wherein the synthesis kettle 1, the receiving tank 2, the crusher 3, the crude product collecting tank 4, the acetone refining kettle 5, the filter pressing separation mechanism 6, the pure water refining kettle 7, the dryer and the extrusion granulator are connected in sequence from end to end; the filter-pressing separating mechanism 6 comprises a separating box 60, the separating box 60 is barrel-shaped, a rotatable separating plate 65 is arranged in the separating box 60, a plurality of separating grooves 651 which are evenly distributed in an annular mode are arranged on the separating plate 65, a filter pressing cylinder 67 which is fixedly connected is arranged at the bottom of the separating groove 651, filter plates 671 which can be opened and closed in a rotating mode are arranged at the bottom of the filter pressing cylinder 67, filter pressing plates 666 which can move up and down are arranged in the filter pressing cylinder 67, a feed inlet for one-way material entering is formed in the filter pressing plates 666, a feed pipe 61 is arranged on one side of the separating box 60, and the feed pipe 61 is arranged at the upper end of the separating groove 651.
The rotatable design of the separating plate 65 enables each filter press cylinder 67 to sequentially move to the lower part of the feeding pipe 61 in a rotating manner, thereby realizing automatic feeding during filter press in the filter press cylinder 67 and continuous feeding of the feeding pipe 61; the material can directly enter the lower part of the filter plate 666 in the filter pressing cylinder 67 through the feeding hole on the filter pressing plate 666, the filter pressing plate 666 can move up and down, automatic filter pressing can be realized through the downward movement of the filter pressing plate 666, meanwhile, the filter plate 671 can be designed to be rotatable to be opened and closed, solid-liquid separation can be carried out when the filter pressing plate 666 is pressed down, and meanwhile, after the filter pressing is finished, the automatic separation of a filter cake after the filter pressing can be realized through the rotation of the filter plate 671.
As a possible implementation manner, referring to fig. 5, the filter pressing cylinders 67 are provided with rotatable filter pressing shafts 66, the filter pressing shafts 66 are provided with reciprocating threads 664, the filter pressing plates 666 are provided with thread grooves which are in matching connection with the reciprocating threads 664, and the filter pressing cylinders 67 are polygonal prismatic.
The design of the reciprocating screw 664 allows for periodic automatic up and down movement of the filter press plate 666 by the continuous rotation of the filter press shaft 66, coupled with the nature of the reciprocating screw 664.
In this embodiment, referring to fig. 6, the upper and lower ends of the filter pressing plate 666 are respectively provided with a sealing hose 667 which is fixedly connected and telescopic, the sealing hose 667 is sleeved outside the filter pressing shaft 66, and the extending ends of the sealing hose 667 are respectively rotatably and hermetically connected with the filter pressing shaft 66 outside the reciprocating screw thread 664.
The sealing hose 667 is designed to seal the joint of the reciprocating threads 664, so that the integral tightness of the filter press plate 666 during filter press is ensured, and the filter press effect is improved.
As a possible implementation manner, referring to fig. 3-6, a fixed plate 663 fixedly connected and used for limiting the filter pressing shaft 66 is disposed in the separation groove 651, a synchronous gear 662 fixedly connected is disposed at the upper end of the filter pressing shaft 66, a synchronous rack 661 which is annular and meshed with the corresponding synchronous gear 662 is disposed on the inner wall of the separation box 60, the synchronous rack 661 is fixedly connected with the inner wall of the separation box 60, a rotating shaft 631 in rotation connection is disposed in the middle of the separation box 60, the rotating shaft 631 is fixedly connected with the separation plate 65, a driving motor 63 is disposed at the bottom of the separation box 60, and an output end of the driving motor 63 is connected with the rotating shaft 631. The press shaft 66 passes through the fixed plate 663, and the press shaft 66 is rotatably connected with the fixed plate 663 through a bearing.
By the design of the synchronous gear 662 and the synchronous rack 661, the synchronous gear 662 can continuously rotate under the engagement of the synchronous rack 661 by the rotation of the separating plate 65, thereby continuously rotating the filter pressing shaft 66.
As a possible implementation manner, referring to fig. 5-6, the feed inlets are symmetrically distributed on two sides of the filter pressing plate 666, and the feed inlets are internally provided with feed plates 665 in rotary connection, the feed plates 665 are in rotary connection with the side walls of the filter pressing plate 666 through hinges, and torsion springs for driving the feed plates 665 to rotate to recover the initial positions are arranged at the connection positions of the feed plates 665 and the filter pressing plate 666.
The design of filter press board 666, feed inlet, torsion spring and feed plate 665 can be when not feeding, and torsion spring can drive feed plate 665 and seal the feed inlet, and when feeding, the pressure of material can overcome torsion spring's elasticity, extrudeed rotatory opening of feed plate 665 to realized the automatic feed of material, and after the feeding is accomplished, torsion spring's elasticity can drive feed plate 665 and seal the feed inlet, has guaranteed the leakproofness of filter pressing board 666 when the filter-pressing simultaneously.
As a possible embodiment, referring to fig. 6, a detection rod 69 is fixedly connected to the bottom of the filter press plate 666, and an inductive probe 691 for detecting humidity is disposed on the detection rod 69.
The design of the detection rod 69 and the sensing probe 691 can automatically sense the humidity of the material after the filter pressing through the sensing probe 691, so that the solid-liquid separation efficiency is judged through the sensing probe 691, and the time for the rotation opening of the filter plate 671 is controlled.
In this embodiment, referring to fig. 6-7, one end of the filter plate 671 is rotatably connected with the bottom of the filter pressing cylinder 67 through a hinge, and the other end of the filter plate 671 is provided with a positioning plate 696 fixedly connected, a positioning groove 695 for clamping and inserting the positioning plate 696 is provided at the bottom of the filter pressing cylinder 67, a through type locking groove 697 is provided on the positioning plate 696, and a telescopic lock tongue 698 for inserting the locking groove 697 to be clamped and fixed is provided on the side wall of the positioning groove 695.
The design of the lock tongue 698, the positioning plate 696, the positioning groove 695 and the locking groove 697 can enable the filter plate 671 to stretch out through the lock tongue 698 to be clamped with the locking groove 697 after being rotationally closed, so that the fixation of the filter plate 671 can be realized, and when the contact fixation is carried out, the release fixation of the filter plate 671 can be realized only by contracting the lock tongue 698, and the filter plate 671 can be rotationally opened.
In this embodiment, referring to fig. 6-7, an adjusting groove 690 is disposed on a side wall of the positioning groove 695, the lock tongue 698 is slidably connected in the adjusting groove 690, a return spring 699 for driving the lock tongue 698 to automatically pop out is disposed in the adjusting groove 690, a fixedly connected and bendable connecting piece 694 is further disposed at an end portion of the lock tongue 698, a protruding block 693 is disposed on an inner wall of the filter pressing cylinder 67, an extending end of the connecting piece 694 movably passes through a side wall of the adjusting groove 690 and is fixedly connected with the protruding block 693, the detecting rod 69 is an electric hydraulic rod with a telescopic length, the detecting rod 69 is located right above the protruding block 693, a fixedly connected and bendable transmission piece 692 is disposed at an end portion of the detecting rod 69, and an extending end of the transmission piece 692 is fixedly connected with the filter plate 671.
The reset spring 699 can realize the automatic pop-up of spring bolt 698, and the design of protruding piece 693, connecting piece 694 and measuring rod 69, can make measuring rod 69 along with the in-process of filter pressing board 666 downstream, measuring rod 69 tip and protruding piece 693 contact, drive protruding piece 693 downstream a section distance, thereby through the transmission of connecting piece 694, drive the separation of spring bolt 698 and locked groove 697, the automatic dismantlement of locating plate 696 has been realized, make the rotor plate automatic opening, moreover, measuring rod 69 telescopic design, can respond to the change of material humidity through inductive probe 691, the flexible length of measuring rod 69 is controlled, if humidity is bigger, can reduce measuring rod 69's length, thereby make filter pressing board 666 to the material filter pressing time longer, thereby make the material can more thoroughly filter pressing, if humidity is little, can extend measuring rod 69 length, so, measuring rod 69 can be faster with protruding piece 693 contact, thereby more in time open 671's separation after making filter pressing, prevent that the material from crossing, the change of material can's the flexible length of measuring rod 69, if the change through the change of material, the change of passing through the transmission piece 666, the filter pressing board 666 can's the transmission is moved down, the filter pressing board 692 can's that can's the filter pressing through the filter plate is moved down, the filter plate is closed, the manual material 692 is moved in time, the manual transmission of the change, and the change through the filter, the filter through the manual transmission of the manual transmission of the process, and the manual transmission of the control.
As a possible embodiment, referring to fig. 8, a discharge hole 684 for discharging the material after press filtration is provided at the bottom of the separation tank 60, and a collection tank 64 for collecting the material is provided below the discharge hole.
The design of discharge hole 684 and collection box 64 can be after filter 671 is rotatory to be opened, and the material drops to collection box 64 through discharge hole 684 in, has realized the automatic collection of material after the filter-pressing.
In this embodiment, referring to fig. 8-9, a separating ring plate 685 that is fixedly connected and is annular is disposed in the middle of the separating box 60, a collecting cavity 68 for the filtrate is formed between the separating ring plate 685 and the inner wall of the separating box 60, collecting plates 681 for sealing two ends of the collecting cavity 68 are disposed on two sides of the discharging hole 684, the collecting box 64 is arc-shaped, and the arc length of the collecting box 64 is greater than that of the discharging hole 684. Wherein the separating ring plate 685 is sleeved outside the rotating shaft 631.
The collecting chamber 68 can realize unified collection of filtrate, and the collecting plate 681 realizes the sealing property of the whole collecting chamber 68.
In this embodiment, referring to fig. 8-9, two ends of the collecting plate 681 far from one end of the feeding pipe 61 are slidably and sealingly connected with the corresponding separating ring plate 685 and the inner wall of the separating box 60, one side of the discharging hole 684 is provided with an arc-shaped recovery groove 687, an extending plate 686 in sliding and sealing connection is arranged in the recovery groove 687, the end of the extending plate 686 is fixedly connected with the corresponding collecting plate 681, a fixedly connected adjusting plate 683 is arranged in the discharging hole 684, a rotationally connected adjusting hydraulic rod 682 is arranged on the adjusting plate 683, and the extending end of the adjusting hydraulic rod 682 is rotationally connected with the collecting plate 681 outside the extending plate 686. Wherein a drain 62 for filtrate is provided on one side of the collection chamber 68.
As a possible implementation manner, the upper surface of the separation tank 651 is provided with a diversion ring groove which is in an annular inclined shape and is used for diversion and conveying of materials into the filter pressing cylinder 67.
As a possible embodiment, a supporting groove 668 is provided at the bottom of the press shaft 66, and a supporting rod 669 corresponding to the supporting groove 668 is provided at the upper end of the filter plate 671.
When the embodiment is used, the following steps are adopted:
the material is discharged through the acetone refining kettle 5, enters the separation box 60 through the feed pipe 61, falls into the corresponding filter pressing cylinder 67 through the end part of the feed pipe 61, starts the driving motor 63 at the moment, drives the separation plate 65 to rotate in the separation box 60, and when the driving motor 63 drives, the filter pressing plate 666 in the filter pressing cylinder 67 positioned right below the feed pipe 61 is positioned at the highest position in the filter pressing cylinder 67;
when the filter-pressing cylinder 67 is full of materials, the separating plate 65 rotates to move the next empty filter-pressing cylinder 67 to the bottom of the feeding pipe 61, and by controlling the rotation speed of the separating plate 65, when the feeding pipe 61 is kept in a normally open state, the guide ring groove moves from just below the feeding pipe 61 to the process of separating from the feeding pipe 61, and the materials discharged from the feeding pipe 61 can fill the filter-pressing cylinder 67; by the design, the intermittent opening and closing control of the feeding pipe 61 is not needed, so that the filter pressing efficiency of the filter pressing separation mechanism 6 on materials is improved to the maximum extent;
when the filter pressing cylinder 67 filled with materials synchronously rotates along with the separating plate 65, the continuous rotation of the filter pressing shaft 66 in the filter pressing cylinder 67 can be driven by the transmission of the synchronous rack 661 and the synchronous gear 662, and the filter pressing cylinder 67 can synchronously move downwards when rotating by the characteristic of the reciprocating thread 664, so that the materials are subjected to filter pressing, and the filter pressing liquid is discharged by the filter plate 671 and falls into the collecting cavity 68 for uniform collection;
when the sensing probe 691 at the end part of the detection rod 69 detects that the humidity of the material after the pressure filtration is too high, the pressure filtration rod is controlled to shrink a certain distance, and meanwhile, the hydraulic rod 682 is started to be regulated to drive the extension plate 686 to be unfolded from the recovery groove 687, so that the collecting length of the collecting cavity 68 for the pressure filtration cylinder 67 is increased, the filtrate after the pressure filtration of the pressure filtration cylinder 67 can be better collected by the collecting cavity 68, the pressure filtration time of the pressure filtration plate 666 for the material in the pressure filtration cylinder 67 is improved, the material with the too high humidity can be better pressure-filtered, and the end part of the detection rod 69 extrudes the boss 693 and drives the boss 693 to move downwards a certain distance along with the pressure filtration of the material in the pressure filtration cylinder 67 (at the moment, the discharge hole 684 at the outer side of the extension plate 686), and the automatic release of the positioning plate 696 is realized by driving the transmission of the connecting piece 694; at this time, along with the downward movement of the filter pressing plate 666, the automatic separation of the materials of the filter pressing cylinder 67 can be realized, and along with the continuous rotation of the separation plate 65, the filter pressing plate 666 automatically ascends in the filter pressing cylinder 67, and meanwhile, the bottom of the filter pressing cylinder 67 is automatically rotated and closed by the filter plate 671 driven by the transmission piece 692, and after the filter pressing plate 666 is closed, the lock tongue 698 is automatically inserted into the lock groove 697, so that the filter plate 671 is automatically fixed after the filter pressing plate 666 is closed;
along with the continuous rotation of the separation plate 65, the press cylinder 67 after material separation moves to the lower part of the feeding pipe 61 again to charge again, so that the periodical automatic charging, press filtering and discharging processes of the press cylinder 67 are realized;
and when the sensing probe 691 on the detecting rod 69 detects that the humidity is too low, the material is extruded and overdried, the detecting rod 69 can be controlled to automatically extend, so that the detecting rod 69 can be earlier contacted with the protruding block 693 to drive the filter plate 671 to be opened in a faster rotating way, and meanwhile, the hydraulic rod 682 is controlled to be regulated to recycle the extension plate 686, so that the collection length of the collection cavity 68 is reduced.
Example 2
A polysulfone resin production process comprises the following steps:
crude S1 polymerization, namely sulfolane, biphenol (used for producing PPSU), bisphenol A (used for producing PESU), bisphenol S (used for producing PSU), carbonate and 4,4' -dichloro diphenyl sulfone which are raw auxiliary materials. Putting the mixture into a synthesis kettle 1, sealing the synthesis kettle 1, heating while starting nitrogen substitution, and keeping the system at 80 ℃ for 60min after the nitrogen substitution is finished, and fully melting and dissolving raw and auxiliary materials. At this time, the nitrogen is replaced, the normal pressure state is restored in the kettle, and the state that the low-flow nitrogen continuously flows in is maintained. And opening the emptying branch pipe leading to the water seal, and starting to heat. At this time, bubbles bulge out at the water seal part, and the state and the nitrogen flow rate are maintained.
Rapidly heating to 160 ℃ and keeping the system temperature above 160 ℃. Observing the state of the water seal, and after about half an hour, the frequency of bubbles at the water seal begins to increase. The salt formation reaction starts. With gradual acceleration of salt forming reaction, the temperature of the system slightly rises, and the heating principle of the system is kept at 160 ℃ or above. The bubble frequency continuously begins to decrease until the water seal is reached, which indicates that salt formation tends to be completed and the temperature continues to rise. This process lasted 10 hours. The temperature rising process needs to be carried out every 10 ℃ before 180 ℃ for 30min, and is not stopped after 180 ℃ is reached, so that the temperature rises to 200 ℃ quickly. A torque sensor is arranged on the stirring of the reaction kettle, and a current transducer is arranged on each phase of the incoming line of the motor to characterize the viscosity change of the reaction system. As the polysulfone is gradually polymerized, the viscosity of the polysulfone is correspondingly and gradually increased, and the characteristic phenomenon is that the torque is increased and the current is increased. After the torque and current reached the expected values, the heating was stopped, and a small amount of 0.2% of the monomer dichlorodiphenyl sulfone (calculated on the molar amount of the reaction system) was added and the reaction was continued for 30 minutes. The crude polymerization reaction is completed. The polymerization process is normally around 12 hours. The process is realized by adopting an automatic control system for remote monitoring after the material feeding is finished.
S2, cooling and crushing: the crude polymer product is cooled in a receiving tank 2. Crushing the material cooled to room temperature, and delivering the crushed material to a product refining process;
s3, refining acetone: the crushed polymerized crude product is sent into an acetone refining kettle 5, the extract is injected into the acetone refining kettle 5, the jacket steam is heated, the mixture is stirred, the mixture is kept at 40 ℃ for 60min, and then the acetone is extracted, thus completing one-time extraction. The above steps are normally repeated for 8 to 12 times, and sulfolane is extracted cleanly, specifically, the residual amount of sulfolane contained in acetone reaches the standard. The extract mixed with sulfolane is sent to a recovery device for on-line recovery of the acetone and sulfolane.
S4, refining pure water: the crude product material after sulfolane removal is formed into a filter cake through a filter pressing separation mechanism 6, the filter cake is transferred into a pure water refining kettle 7, extraction liquid pure water is injected, jacket steam is used for heating, stirring is assisted, the temperature is kept between 90 and 95 ℃ for 60 minutes (high temperature is helpful for dissolving salt in the material into water), and then water is pumped out to finish primary pure water extraction. The pure water extraction operation is repeated for 8 to 10 times, so that the mixed inorganic salt in the product can be removed completely, and the conductivity in the water is used as a characterization index. The concentrated part of the saline water is sent to a decompression evaporation device for separating out byproduct inorganic salt, the byproduct inorganic salt is recycled for three times in the middle, and the inorganic salt with lower content is directly sent to sewage treatment.
The material after pure water refining is centrifugally dehydrated by a four-foot flat plate centrifuge, the water content of the dehydrated material can be controlled to be about 40 percent, and the dehydrated material is sent to a drying process. And delivering the centrifuged liquid to sewage treatment.
The process is realized by adopting an automatic control system for remote monitoring after the material feeding is finished.
S5, drying and granulating
And (3) drying the refined polysulfone product by adopting a rotary double-cone dryer under a negative pressure state by adopting steam heating, and conveying the polysulfone product to a screw extruder for extrusion granulation after the water content is lower than three thousandths. Finally, the polysulfone finished product is obtained.
S6, recycling and applying: the liquid mixed with sulfolane is first sent to an acetone recovery system, the acetone recovery adopts normal pressure rectification technology, and the concentrated solution after acetone recovery is sent to a decompression rectification device. Sulfolane is extracted by a decompression rectification mode and can be recycled. The acetone recovery rate was 90% and the sulfolane recovery rate was 95%. Concentrating the water containing the high-concentration inorganic salt in a reduced pressure rectification mode, and separating out the inorganic salt; and sending the condensate to sewage treatment.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
In the present invention, unless explicitly specified and limited otherwise, the terms "disposed," "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; the connection may be mechanical connection, direct connection or indirect connection through an intermediate medium, and may be internal connection of two elements or interaction relationship of two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
The control mode of the invention is automatically controlled by the controller, the control circuit of the controller can be realized by simple programming of a person skilled in the art, the supply of power also belongs to common knowledge in the art, and the invention is mainly used for protecting a mechanical device, so the invention does not explain the control mode and circuit connection in detail.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (7)
1. The polysulfone resin production process is characterized by comprising the following steps:
s1, crude product polymerization, namely putting sulfolane, biphenol, bisphenol A, bisphenol S, carbonate and 4,4' -dichloro diphenyl sulfone serving as raw auxiliary materials into a synthesis kettle (1), sealing, heating, and raising the temperature to perform crude product polymerization reaction;
s2, cooling and crushing: cooling the polymerized crude product in a receiving groove (2); crushing the material cooled to room temperature, and delivering the crushed material to a product refining process;
s3, refining acetone: sending the crushed polymerized crude product into an acetone refining kettle (5) for sulfolane extraction operation; repeating the operation for 8-12 times normally, and extracting sulfolane completely;
s4, refining pure water: the crude product material after sulfolane removal is formed into a filter cake through a filter pressing separation mechanism (6), and then the filter cake is transferred into a pure water refining kettle (7) for pure water extraction; repeating the pure water extraction operation for 8-10 times, and removing the mixed inorganic salt in the product; centrifugally dewatering the purified material in a centrifugal machine, and conveying the material to a drying process;
s5, drying and granulating: drying the refined polysulfone product by using a dryer under a negative pressure state by adopting steam heating, and extruding and granulating by using a screw extruder after the water content is lower than three thousandths; finally, the polysulfone finished product is obtained.
2. The polysulfone resin production process according to claim 1, wherein: the materials in the step S2 are put into a synthesis kettle (1) and sealed, nitrogen replacement is started while heating, and the system is maintained for 60min after heating to 80 ℃; then rapidly heating to 160 ℃ and keeping the temperature of the system above 160 ℃.
3. The polysulfone resin production process according to claim 1, wherein: the sulfolane extraction method in the step S3 comprises the following steps: the extract is injected into an acetone refining kettle (5), heated by steam and stirred, kept at 40 ℃ for 60min, and then the acetone is extracted to finish one-time extraction.
4. The polysulfone resin production process according to claim 1, wherein: the pure water extraction method in the step S4 comprises the following steps: injecting pure water into the extraction liquid, heating the jacket by steam, stirring, maintaining at 90-95 ℃ for 60min, and then pumping out water to finish the primary pure water extraction.
5. The polysulfone resin production process according to claim 1, wherein: the index of the clean removal of the mixed inorganic salt in the product in the step S4 is to take the conductivity in water as a characterization index.
6. The polysulfone resin production process according to claim 1, wherein: and in the step S4, the water content of the material subjected to centrifugal dehydration by the four-foot flat plate centrifuge is controlled at 40%.
7. A polysulfone resin production system employing the polysulfone resin production process as defined in any one of claims 1-6, characterized by: the novel filter press comprises a synthesis kettle (1), a receiving tank (2), a crusher (3), a crude product collecting tank (4), an acetone refining kettle (5), a filter pressing separation mechanism (6), a pure water refining kettle (7), a dryer and an extrusion granulator, wherein the synthesis kettle (1), the receiving tank (2), the crusher (3), the crude product collecting tank (4), the acetone refining kettle (5), the filter pressing separation mechanism (6), the pure water refining kettle (7), the dryer and the extrusion granulator are sequentially connected from head to tail.
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