CN114917687B - Polyphenylene sulfide slurry washing tower - Google Patents
Polyphenylene sulfide slurry washing tower Download PDFInfo
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- CN114917687B CN114917687B CN202210668083.6A CN202210668083A CN114917687B CN 114917687 B CN114917687 B CN 114917687B CN 202210668083 A CN202210668083 A CN 202210668083A CN 114917687 B CN114917687 B CN 114917687B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D43/00—Separating particles from liquids, or liquids from solids, otherwise than by sedimentation or filtration
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- 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
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- 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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- Polymers & Plastics (AREA)
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- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The invention discloses a polyphenylene sulfide slurry washing tower, which comprises a tower body, a tower top stirrer and a small scraper separator, wherein the tower top stirrer is arranged at the top of the tower body; a steam heater is arranged at the central position inside the tower body, the steam heater is positioned below one of the tower plates, and the edge of the steam heater is fixed on the inner wall of the tower body; an air bubbler is arranged below the inner part of the tower body, the air bubbler is positioned at the bottom of the tower plate at the lowest part, and the edge of the air bubbler is fixed on the inner wall of the tower body; the upper portion side of tower body is provided with the feed inlet, and the top of tower body is provided with the gas vent, and the bottom of tower body is provided with the liquid outlet. The invention adopts the structure to improve the product quality of the polyphenylene sulfide, save water resources, reduce cost and solve the defects existing in the prior production equipment.
Description
Technical Field
The invention relates to the technical field of polyphenylene sulfide slurry and salt separation, in particular to a polyphenylene sulfide slurry washing tower.
Background
Polyphenylene sulfide is a special engineering plastic with excellent mechanical properties, has excellent heat resistance, electrical properties and rigidity, and is widely applied to various material fields, such as automobiles and electronic and electric parts. At present, a method for producing polyphenylene sulfide generally adopts dihalogen substituted aromatic compounds and alkali metal sulfides to carry out condensation polymerization reaction in a polar organic solvent, such as p-dichlorobenzene and sodium sulfide are polymerized in an N-methyl-2-pyrrolidone solvent at high temperature and high pressure to prepare slurry containing polyphenylene sulfide resin, and the slurry is filtered and recovered to obtain the polyphenylene sulfide resin. However, in the above-mentioned process for producing polyphenylene sulfide resin, p-dichlorobenzene is polymerized with sodium sulfide to produce sodium chloride as a by-product in addition to the polyphenylene sulfide resin, and the produced sodium chloride is insoluble in the N-methyl-2-pyrrolidone solvent, and at the same time, a small amount of polyphenylene sulfide oligomer, that is, a low molecular weight substance such as polyphenylene sulfide trimer, polyphenylene sulfide tetramer, etc., is produced during the polymerization.
The main components of the slurry prepared by the process are high molecular weight polyphenylene sulfide (PPS) resin, byproduct sodium chloride, a solvent for synthesis, an auxiliary agent and a small amount of polyphenylene sulfide oligomer, and the conventional method for reducing impurities in the polyphenylene sulfide slurry is to wash and purify the polyphenylene sulfide resin in a kettle by using water. When the polyphenylene sulfide slurry is filtered to recover the polyphenylene sulfide, sodium chloride and the polyphenylene sulfide oligomer are combined with the polyphenylene sulfide resin, a large amount of water is needed when the resin is washed and purified, the efficiency of washing equipment determines the water consumption, and the washing water needs to be treated to be discharged or the solvent in the washing water is recovered, so that extra equipment and operation cost are needed. In addition, the polyphenylene sulfide oligomer is insoluble in solvents and water, and when the purified resin is washed in a tank, the polyphenylene sulfide oligomer and the organic solvent remain in the resin, degrading the quality of the resin product.
In summary, how to find a device capable of effectively removing byproducts in polyphenylene sulfide resin in conventional cleaning and purifying of polyphenylene sulfide resin production becomes a technical problem to be solved currently. The washing tower is novel polyphenylene sulfide slurry purifying treatment equipment, is produced by improving the conventional fixed tray washing tower and the conventional stirring kettle, is widely applied to the aspects of industrial PVC purification, resin separation and the like, and has good effect. The washing tower is particularly suitable for separating slurry and purifying mixed gas containing a large amount of dust in the production of polyphenylene sulfide resin, at present, the desalted water is used for washing sodium chloride in the polyphenylene sulfide salt removal widely applied in industry, and as the PH of the desalted water is close to 7, the components cannot react, the polyphenylene sulfide is not damaged, the desalted water is low in cost and easy to obtain, and the original desalted water station is relied on, so that the method is more in line with economic benefit.
Disclosure of Invention
The invention aims to provide a polyphenylene sulfide slurry washing tower, which improves the product quality of polyphenylene sulfide, saves water resources, reduces cost and solves the defects existing in the existing production equipment.
In order to achieve the above purpose, the invention provides a polyphenylene sulfide slurry washing tower, which comprises a tower body, a tower top stirrer and a small scraper separator, wherein the tower top stirrer is arranged at the top of the tower body, the small scraper separator is connected with the tower body, a plurality of tower plates are arranged in the tower body from bottom to top, a vertical scraping plate is arranged at the upper part of each tower plate, and each vertical scraping plate is connected with a stirring shaft of the tower top stirrer;
a steam heater is arranged at the central position inside the tower body, the steam heater is positioned below one of the tower plates, and the edge of the steam heater is fixed on the inner wall of the tower body;
an air bubbler is arranged below the inner part of the tower body, and is positioned at the bottom of the tower plate at the lowest part, and the edge of the air bubbler is fixed on the inner wall of the tower body;
the upper portion side of tower body is provided with the feed inlet, the top of tower body is provided with the gas vent, the bottom of tower body is provided with the liquid outlet.
Preferably, a bottom stirrer is arranged on the side edge of the bottom of the tower body, the bottom stirrer is positioned below the air bubbler, and the bottom stirrer and a tangent line of the side wall of the tower body form an angle of 45 degrees.
Preferably, a sampling analysis port is arranged on the side edge of the bottom of the tower body, and the sampling analysis port is positioned below the tower bottom stirrer.
Preferably, the lower end of the top flange of the tower body is provided with an overflow port, the overflow port is connected with the inlet of the small scraper separator, and the outlet of the small scraper separator is connected with the pipe orifice in the middle of the tower body.
Preferably, a stirrer is arranged inside the small scraper separator.
Preferably, a manhole, a pressure gauge port, a liquid level gauge port and a steam inlet are formed in the top of the tower body.
Preferably, a sixth of sector-shaped notch is arranged on the column plate, and the column plate is made of solid steel plates.
Preferably, the feed inlet and the cylinder tangent line of the tower body form an angle of 45 degrees.
Preferably, the vertical scraping plate is a wedge-shaped solid steel plate, and the wedge-shaped thick end of each layer is fixed on a stirring shaft of the tower top stirrer by bolts.
Preferably, the steam heater and the air bubbler are both configured as a coil side open-cell immersion structure.
Therefore, the polyphenylene sulfide slurry washing tower adopting the structure has the following beneficial effects:
(1) The desalted water can be used for efficiently washing the polyphenylene sulfide slurry, so that the polyphenylene sulfide is thoroughly separated from salt and oligomer, the product quality of the polyphenylene sulfide is greatly improved, water resources are saved, and the cost is reduced;
(2) The original structure principles of a washing kettle, a disc dryer and a washing tower commonly used in coal chemical industry in the polyphenylene sulfide industry are integrated and innovated, a feed inlet is changed into a 45-degree oblique angle feed and extends into a first tower plate at the top of the tower, so that the problem of blockage of a feed pipe orifice is avoided, and a stirrer is adopted to redistribute solid materials at the top of the tower, so that the materials are prevented from being accumulated;
(3) The column plates adopt sector notch column plates, so that the materials and the solvent have enough contact area, and the distribution of the materials is more reasonable;
(4) The steam heater and the bubbler are arranged, the temperature is increased, the turbulence is increased, and the contact area of the material and the solvent is improved to the maximum extent.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a schematic diagram of a slurry scrubber for polyphenylene sulfide according to an embodiment of the present invention;
FIG. 2 is an enlarged view at A of an embodiment of a polyphenylene sulfide slurry scrubber of the present invention;
FIG. 3 is a schematic diagram of a tray layout of an embodiment of a polyphenylene sulfide slurry scrubber of the present invention;
FIG. 4 is a schematic view of a vertical scraper plate structure of an embodiment of a polyphenylene sulfide slurry scrubber according to the present invention;
FIG. 5 is a schematic diagram showing the structure of an overhead stirrer of an embodiment of a polyphenylene sulfide slurry scrubber of the present invention.
Detailed Description
The technical scheme of the invention is further described below through the attached drawings and the embodiments.
Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The terms "first," "second," and the like, as used herein, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof, but does not exclude other elements or items. The terms "connected" or "connected," and the like, are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", etc. are used merely to indicate relative positional relationships, which may also be changed when the absolute position of the object to be described is changed.
Examples
Fig. 1 is a schematic structural view of an embodiment of a polyphenylene sulfide slurry scrubber according to the present invention, fig. 2 is an enlarged view of a portion a of an embodiment of a polyphenylene sulfide slurry scrubber according to the present invention, fig. 3 is a layout of a tray of an embodiment of a polyphenylene sulfide slurry scrubber according to the present invention, fig. 4 is a schematic structural view of a vertical scraper of an embodiment of a polyphenylene sulfide slurry scrubber according to the present invention, and fig. 5 is a schematic structural view of an overhead stirrer of an embodiment of a polyphenylene sulfide slurry scrubber according to the present invention. As shown in the figure, the invention provides a polyphenylene sulfide slurry washing tower, which comprises a tower body 1, an overhead stirrer 2 and a small scraper separator 3, wherein the overhead stirrer 2 and the small scraper separator 3 are arranged at the top of the tower body 1, the small scraper separator 3 is connected with the tower body 1, a plurality of tower plates 4 are arranged in the tower body 1 from bottom to top, a vertical scraping plate 5 is arranged at the upper part of each tower plate 4, the vertical scraping plates are detachable stainless steel plates and are fixed on a stirring shaft of the overhead stirrer through bolts, a gap of 10mm is reserved between each vertical scraping plate 5 and a bottom tower plate, each vertical scraping plate is connected with the stirring shaft of the overhead stirrer 2, a sixth of sector-shaped notch 18 is arranged on each tower plate 4, the tower plates 4 are made of solid steel plates, each layer of sector-shaped notch is not overlapped with the sector-shaped notch of the next layer, and all the vertical scraping plates uniformly rotate.
A steam heater 6 is arranged at the central position inside the tower body 1, the steam heater 6 is positioned below one of the tower plates 4, and the edge of the steam heater 6 is fixed on the inner wall of the tower body 1; the inside below of tower body 1 is provided with air bubbler 7, and air bubbler 7 is located the bottom of tray 4 of below, and the edge is fixed on the inner wall of tower body 1, and air bubbler and steam heater be for DN25 stainless steel pipe crooked semicircle back welding, every return bend interval 15mm, and it is a plurality of to trompil in the bottom of every return bend, and the hole interval is 25mm, and steam heater 6 and air bubbler 7 all set up to coil pipe side trompil immersion type structure. The upper side of the tower body 1 is provided with a feed inlet 8, and the feed inlet 8 forms a 45-degree angle with a cylinder tangent line of the tower body 1. The top of the tower body 1 is provided with an exhaust port 9, and the bottom of the tower body 1 is provided with a liquid outlet 10. The lower end of the top flange of the tower body 1 is provided with an overflow port 13, the overflow port 13 is connected with the inlet of the small scraper separator 3, and the outlet of the small scraper separator 3 is connected with the middle pipe orifice of the tower body 1. The small scraper separator 3 is internally provided with a stirrer. The washing tower can wash the mixed crude product of the polyphenylene sulfide slurry and the salt by adopting water, plays a role in separating and purifying the pure polyphenylene sulfide slurry by removing the salt, solves the difficult problem of separation in industry, and has the advantages that the overflow port at the upper part of the tower is provided with a small scraper separator, the low-molecular polyphenylene sulfide slurry is independently treated and recycled from the overflow port, and the liquid is returned into the tower for recycling.
The bottom side of tower body 1 is provided with tower bottom stirrer 11, and tower bottom stirrer 11 is located the below of air bubbler 7, and tower bottom stirrer 11 and the lateral wall tangent line of tower body 1 are 45 angle.
The bottom side of tower body 1 is provided with sample analysis mouth 12, and sample analysis mouth 12 is located the below of tower bottom mixer 11.
The top of the tower body 1 is provided with a manhole 14, a pressure gauge port 15, a liquid level gauge port 16 and a steam inlet 17. A thermometer port 19 is provided on the top side wall of the tower body.
The vertical scraping plate 5 is a wedge-shaped solid steel plate, and the wedge-shaped thick end of each layer is fixed on the stirring shaft of the tower top stirrer 2 by bolts.
The mounting groove has been seted up to the inner wall of tower body, the edge joint of column plate is in the inside of mounting groove, vertical flitch setting and column plate upper portion 10mm position, the afterbody passes through bolted connection to the overhead stirrer, the overhead stirrer is connected with all vertical flitch of scraping, do not contact with the column plate, drive vertical flitch of scraping and do clockwise rotary motion, the column plate is from last to fan-shaped breach of every layer down and the fan-shaped breach of last layer clockwise deflection 1/6, make the even scattering of material on the column plate, 100mm department below the column plate of the next layer is the bubbler, bubbler and column inner wall welding are fixed on the pre-weld piece in the tower. The bubbling port (aeration head) faces downwards, a steam heater is arranged at the 200mm position of the top of the vertical scraping plate on the upper part of the middle column plate in the tower body, the steam heater is welded with the inner wall of the tower body and is fixed on a welding piece in the tower body, and an opening is arranged upwards. The tower top heater and the tower bottom heater rotate continuously at variable speed, and the tower is filled with liquid.
When slurry is washed, desalted water is filled in the tower, a tower top stirrer and a tower bottom stirrer are started, steam is introduced into a steam heater, so that the temperature in the tower body is increased to 80 ℃, polyphenylene sulfide slurry uniformly drops on a first layer of tower plate from a feed inlet on the tower body, the slurry is uniformly paved on the tower plate through the tower top stirrer, when solid is sampled out from a lower outlet, air is introduced into an air bubbler, a subsequent separation device of a top overflow port is opened, reflux liquid is returned into the tower, and whether a plurality of washing towers are used in series is determined according to the amount of the slurry and the purity of the outlet polyphenylene sulfide.
Therefore, the polyphenylene sulfide slurry washing tower adopting the structure improves the product quality of polyphenylene sulfide, saves water resources, reduces cost and solves the defects existing in the existing production equipment.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (7)
1. The utility model provides a polyphenylene sulfide thick liquids scrubbing tower which characterized in that:
the device comprises a tower body, a tower top stirrer and a small scraper separator, wherein the tower top stirrer and the small scraper separator are arranged at the top of the tower body, the small scraper separator is connected with the tower body, a plurality of tower plates are arranged in the tower body from bottom to top, a vertical scraping plate is arranged at the upper part of each tower plate, and each vertical scraping plate is connected with a stirring shaft of the tower top stirrer;
a sixth of sector-shaped notch is arranged on the column plate, and the column plate is made of solid steel plates;
a steam heater is arranged at the central position inside the tower body, the steam heater is positioned below one of the tower plates, and the edge of the steam heater is fixed on the inner wall of the tower body;
an air bubbler is arranged below the inner part of the tower body, and is positioned at the bottom of the tower plate at the lowest part, and the edge of the air bubbler is fixed on the inner wall of the tower body;
the side edge of the upper part of the tower body is provided with a feed inlet, the top of the tower body is provided with an exhaust port, and the bottom of the tower body is provided with a liquid outlet;
the feed inlet and a cylinder tangent line of the tower body form an angle of 45 degrees;
the bottom side of the tower body is provided with a sampling analysis port, and the sampling analysis port is positioned below the tower bottom stirrer.
2. The polyphenylene sulfide slurry scrubber of claim 1, wherein: the bottom side of the tower body is provided with a tower bottom stirrer, the tower bottom stirrer is positioned below the air bubbler, and the tower bottom stirrer and a tangent line of the side wall of the tower body form an angle of 45 degrees.
3. The polyphenylene sulfide slurry scrubber of claim 1, wherein: the top flange lower extreme of the tower body is provided with the overflow mouth, the overflow mouth with little scraper blade separator's inlet connection, little scraper blade separator's export with the middle part mouth of pipe of the tower body is connected.
4. A polyphenylene sulfide slurry scrubber according to claim 3, wherein: the small scraper separator is internally provided with a stirrer.
5. The polyphenylene sulfide slurry scrubber of claim 1, wherein: the top of the tower body is provided with a manhole, a pressure gauge port, a liquid level gauge port and a steam inlet.
6. The polyphenylene sulfide slurry scrubber of claim 1, wherein: the vertical scraping plate is a wedge-shaped solid steel plate, and the wedge-shaped thick end of each layer is fixed on a stirring shaft of the tower top stirrer through bolts.
7. The polyphenylene sulfide slurry scrubber of claim 1, wherein: the steam heater and the air bubbler are both arranged in a coil pipe side open-pore immersion type structure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210668083.6A CN114917687B (en) | 2022-06-14 | 2022-06-14 | Polyphenylene sulfide slurry washing tower |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210668083.6A CN114917687B (en) | 2022-06-14 | 2022-06-14 | Polyphenylene sulfide slurry washing tower |
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| Publication Number | Publication Date |
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| CN114917687A CN114917687A (en) | 2022-08-19 |
| CN114917687B true CN114917687B (en) | 2023-05-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202210668083.6A Active CN114917687B (en) | 2022-06-14 | 2022-06-14 | Polyphenylene sulfide slurry washing tower |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033619A (en) * | 1987-12-17 | 1989-07-05 | 三井石油化学工业株式会社 | The method of the dispersion medium of exchange terephthalic acid slurry |
| CN201000259Y (en) * | 2007-01-26 | 2008-01-02 | 张志霄 | Drying mechanism for axis type stirring sludge multilevel indirect steam back |
| CN101837260A (en) * | 2009-03-18 | 2010-09-22 | 上海亦晨信息科技发展有限公司 | Tower-type premixing device with cross tower plates and method thereof |
| CN102892490A (en) * | 2010-05-21 | 2013-01-23 | 株式会社吴羽 | Vertical countercurrent solid-liquid contact method, method for washing solid particles, method for producing polyarylene sulfide, and device therefor |
| CN109705347A (en) * | 2019-01-10 | 2019-05-03 | 宜宾学院 | A kind of process of the separation of oligomeric from polyphenylene sulfide synthesis slurry |
| WO2021073301A1 (en) * | 2019-10-15 | 2021-04-22 | 浙江新和成特种材料有限公司 | Continuous washing process for polyphenylene sulfide slurry |
-
2022
- 2022-06-14 CN CN202210668083.6A patent/CN114917687B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033619A (en) * | 1987-12-17 | 1989-07-05 | 三井石油化学工业株式会社 | The method of the dispersion medium of exchange terephthalic acid slurry |
| CN201000259Y (en) * | 2007-01-26 | 2008-01-02 | 张志霄 | Drying mechanism for axis type stirring sludge multilevel indirect steam back |
| CN101837260A (en) * | 2009-03-18 | 2010-09-22 | 上海亦晨信息科技发展有限公司 | Tower-type premixing device with cross tower plates and method thereof |
| CN102892490A (en) * | 2010-05-21 | 2013-01-23 | 株式会社吴羽 | Vertical countercurrent solid-liquid contact method, method for washing solid particles, method for producing polyarylene sulfide, and device therefor |
| CN109705347A (en) * | 2019-01-10 | 2019-05-03 | 宜宾学院 | A kind of process of the separation of oligomeric from polyphenylene sulfide synthesis slurry |
| WO2021073301A1 (en) * | 2019-10-15 | 2021-04-22 | 浙江新和成特种材料有限公司 | Continuous washing process for polyphenylene sulfide slurry |
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