CN102677194A - Polyphenylene sulfide spinning technology - Google Patents
Polyphenylene sulfide spinning technology Download PDFInfo
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- CN102677194A CN102677194A CN2011100663218A CN201110066321A CN102677194A CN 102677194 A CN102677194 A CN 102677194A CN 2011100663218 A CN2011100663218 A CN 2011100663218A CN 201110066321 A CN201110066321 A CN 201110066321A CN 102677194 A CN102677194 A CN 102677194A
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- polyphenylene sulfide
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- temperature
- fiber
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- 239000004734 Polyphenylene sulfide Substances 0.000 title claims abstract description 59
- 229920000069 polyphenylene sulfide Polymers 0.000 title claims abstract description 59
- 238000009987 spinning Methods 0.000 title claims abstract description 45
- 238000005516 engineering process Methods 0.000 title claims abstract description 12
- 239000000835 fiber Substances 0.000 claims abstract description 46
- 230000001112 coagulating effect Effects 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000005406 washing Methods 0.000 claims abstract description 32
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000002425 crystallisation Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 229920005989 resin Polymers 0.000 claims abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- 230000004927 fusion Effects 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims description 30
- 229910021641 deionized water Inorganic materials 0.000 claims description 30
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims description 21
- 229920006389 polyphenyl polymer Polymers 0.000 claims description 15
- 150000003568 thioethers Chemical class 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 12
- 238000007710 freezing Methods 0.000 claims description 5
- 230000008014 freezing Effects 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 2
- 238000002074 melt spinning Methods 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 239000007921 spray Substances 0.000 abstract description 2
- 238000004804 winding Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract 1
- 208000012886 Vertigo Diseases 0.000 description 26
- 230000008676 import Effects 0.000 description 9
- 239000000155 melt Substances 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- XWUCFAJNVTZRLE-UHFFFAOYSA-N 7-thiabicyclo[2.2.1]hepta-1,3,5-triene Chemical compound C1=C(S2)C=CC2=C1 XWUCFAJNVTZRLE-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Images
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- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention discloses a polyphenylene sulfide spinning technology, which is used for producing polyphenylene sulfide resin fibers. Finished fibers are produced through the polyphenylene sulfide spinning technology which comprises the steps of: fiber-grade polyphenylene sulfide resin melting; fusion through a screw extruder; metering through a fusant metering pump; forced filtration; spinning through a spinning assembly; filament coagulating bath, cooling and crystallization; three-level coagulating bath and washing; three-level water spray washing; three-level drying and drafting; and winding and doffing. The spinning speed is 1500-1800m/min. The draft ratio is 3-6. The produced polyphenylene sulfide fibers have excellent manufacturability and more excellent mechanical performance. The polyphenylene sulfide spinning technology has the advantages that the process of purifying polyphenylene sulfide resin, the spinning box, the heating and heat preserving media and the constant-temperature device required by all existing melt spinning methods are reduced, the spinning speed of the polyphenylene sulfide fibers is improved, the woven filaments of the polyphenylene sulfide fibers are well-balanced and any molten drop is not produced.
Description
Technical field
The invention belongs to special fibre and make field, the especially melt-spinning technology of polyphenylene sulfide fibre grade resins.
Background technology
High-performance polyphenylene sulfide has the heat endurance under excellent chemical proofing and the high temperature, and has fire-retardant, insulation, radiation hardness and favorable mechanical performance.For enlarging the scope of application of this material, the researchers of various countries make it the new method that fibration is used in searching always.
A kind of melt spinning, stretching heat setting method of linear high molecular weight polyphenylene sulfide fiber grade resins are disclosed in Chinese patent CN1603477; Chinese patent CN1876906 discloses the long stapled manufacturing approach of polyphenylene sulfide; Introduced the method for several kinds of polyphenylene sulfides among U.S. Pat 5405695 and the US4500706 through the polyphenylene sulfide fibre that melt-melts spinning and obtain.The shortcoming of these methods is that the mechanical strength of product fiber is still not high enough, though US5405695 is divided into three zones with the heating region of fusion-spinning extruder, only possibly produce long fiber, and its mechanical strength index condition is undistinct.
In one Chinese patent application number CN200510022439.5, introduced a kind of polyphenylene sulfide melt spinning method, this method does not still have to break away from the pattern of at present all melt spinnings.
The object of the invention is started a kind of spinning process of brand-new polyphenylene sulfide fibre; Its objective is the disqualification rate that reduces polyphenylene sulfide fibre; Improve and put spinning speed,, also reduced as double screw extruder vacuumizing unnecessary equipment and the technique process that removes volatile materials simultaneously processing steps such as the preliminary treatment of lacking polyphenylene sulfide and dryings; Reduce production cost, improved each performance indications such as fibre strength.
Summary of the invention
Polyphenyl thioether spinning technology; Produce the polyphenylene sulfide fiber; Adopting process is: the fusion of fiber-grade polyphenyl thioether resin---the screw extruder fusion---and melt metering pump---forced filtration, spinning pack---strand coagulating bath crystallisation by cooling---six solid baths are washed---and---drawing-off---coiling doff is produced finished fiber, adopts in the following process conditions to comprise:
1, the fusion of polyphenylene sulfide comprises: with weight average molecular weight be the polyphenylene sulfide of 4.8-5.2 to be fused to temperature be among the 260-280 ℃ of sulfolane solvent, be mixed with to contain the sulfolane liquation that polyphenylene sulfide is 80-90%wt;
2, with 1) the sulfolane liquation that contains polyphenylene sulfide that obtains uses the direct input temp of conveying worm to be the 275-280 ℃ of further melting of double screw extruder; By its head gear pump input melt metering pump; The variable-frequency motor rotational frequency of melt metering pump is 20-50Hz; After crossing the head forced filtration, spray by spinning pack.The temperature of spinning pack remains on 275-280 ℃.
3, with 2) fiber that contains sulfolane and polyphenylene sulfide of ejection directly input below spinnerets, to be assembled with strand coagulating bath crystallisation by cooling zone be 0-300mm; It is the deionized water solution that contains 20-30%wt NMP that the crystallisation by cooling zone freezing is bathed, and its temperature is 60-80 ℃; After coming out from crystal region, washs strand through the coagulating bath of 3-6 level; The coagulating bath in first order washing zone contains the deionized water solution of 6-8%wt NMP; The coagulating bath in washing zone, the second level contains the deionized water solution of 3-5%wt NMP; The coagulating bath in third level washing zone contains the deionized water solution of 0.1-1%wt NMP, and the first-three grade of sprinkle water washing zone is 100% deionized water solution; Wherein the temperature of three grades of coagulating bath wash solutions is 80-90 ℃, and the temperature of three grades of sprinkle wash solutions is 85-95 ℃.Input strand drying device, it is 30-60s that dry drawing temperature is controlled at 120-160 ℃ of drying time.Strand is after super-dry, and input up-coiler doff manufactures polyphenylene sulfide fibre.Polyphenyl thioether spinning speed of the present invention is 1500-1800m/min.The drawing-off multiplying power of strand is 3-6 times.
The present invention adopts the liquation spinning technique; Having reduced present all melt spinnings needs the poly-p-phenylene sulfide ether resin to carry out purifying and spins case and heat tracing medium and thermostat; Improved the spinning speed of polyphenylene sulfide fibre; The strand of the polyphenylene sulfide fibre that comes out of weaving is well-balanced like this, can not produce advantages such as any molten drop.Adopt method of the present invention, the property made and the mechanical strength of the polyphenylene sulfide fibre silk that makes all are improved, and fracture strength is greater than 4CN/dt, and the limit in mean oxygen index (OI) reaches 43%.
In the liquation spinning technique flow process of fiber-grade polyphenyl thioether resin of the present invention; The temperature of each heating region of double screw extruder all is the same; Simultaneously all melts pipeline of polyphenylene sulfide liquation all must insulation, and its temperature remains under the polyphenylene sulfide fusing point in 5-10 ℃ the scope; The line density of measuring pump variable-frequency motor frequency receives feeding what and fiber limits, and its frequency is generally under the scope of 2-30 hertz; General spinning pack pressure remains on pretreatment temperature before spinning pack uses between the 1-28 Mpa also will make its temperature remain under the polyphenylene sulfide fusing point in 5-10 ℃ the scope; Strand crystallisation by cooling curing area on the one hand will be according to suitably regulating when ground temperature; Also regulate on the other hand according to the line density or the degree of draft of fiber; Receive how much limiting of feeding machine feeding on the one hand for up-coiler variable-frequency motor frequency, consider the restriction of producd fibers line density, up-coiler variable-frequency motor frequency generally is controlled in the scope of 5-200 hertz; Between one-level up-coiler and secondary up-coiler, there are simultaneously certain hertz difference, i.e. up-coiler winding speed difference.
The present invention at first will pass through in filtration, extraction, washing, 260-280 ℃ of sulfolane solvent of dry synthetic polyphenylene sulfide adding; Be mixed with the sulfolane liquation that contains the 80-90%wt polyphenylene sulfide; Be 275-280 ℃ of double screw extruder melting once more with the liquation input temp then; Be the melt metering pump of the variable-frequency motor of 20-50Hz with liquation through head gear pump incoming frequency again; Import spinning pack through measuring pump; After filtering through filter element in the spinning pack, be the polyphenylene sulfide liquation fiber that 275-280 ℃ spinnerets ejection contains sulfolane solvent, after the liquation fiber is equipped with the 0-300mm temperature and is 60-80 ℃ of coagulating bath crystallisation by cooling zone through the spinnerets below from temperature; Be conveyed into temperature and be three grades of coagulating bath sinks that contain the deionized water solution of different N MP concentration of 80-90 ℃; Be conveyed into temperature again and be 85-95 ℃ three grades 100% further washing of deionized water sprinkle washing zone, input to drying and drawing-off that the three-stage drying drafting system carries out fiber then, import up-coiler at last and be wound into the polyphenylene sulfide finished fiber.So just made polyphenylene sulfide fibre.
Description of drawings:
Fig. 1 is a technological process block-diagram of the present invention.
Description of drawings summary of the present invention:
Polyphenylene sulfide is fused to certain percentage by weight in 260-280 ℃ the sulfolane solvent; Import the further melting of double screw extruder then; Extruded by its head gear pump and to be conveyed into measuring pump, the metering input spinning pack through measuring pump gets into the coagulating bath solution that contains the 20-30%NMP solvent by the spinnerets ejection then and forms strand; After strand further washs through three grades of low concentration NMP coagulating bath; Again through after the washing of three grades of deionized water sprinkles, the drying device of importing three grades of temperature and be 160-180 ℃ carries out dry drawing-off, makes the polyphenylene sulfide finished fiber at last.
The specific embodiment:
Embodiment 1
The polyphenylene sulfide of drying is added in 260 ℃ of sulfolane solvents; Be mixed with the sulfolane liquation that contains the 80%wt polyphenylene sulfide; Being 275 ℃ of double screw extruder meltings once more with the liquation input temp then, is the melt metering pump of the variable-frequency motor of 20Hz with liquation through head gear pump incoming frequency again, imports spinning pack through measuring pump; After filter element filtration in the spinning pack; From temperature is the polyphenylene sulfide liquation fiber that 275 ℃ spinnerets ejection contains sulfolane solvent, and after the liquation fiber was equipped with the 0mm temperature and is 60 ℃ of coagulating bath crystallisation by cooling zones through the spinnerets below, it was that to contain the deionized water solution of 30%wt NMP defeated that its crystallisation by cooling zone freezing is bathed; Send into temperature and be three grades of coagulating bath sinks that contain the deionized water solution of different N MP concentration of 80 ℃; The coagulating bath in first order washing zone contains the deionized water solution of 6%wt NMP, and its temperature is 90 ℃, and the coagulating bath in washing zone, the second level contains the deionized water solution of 3%wt NMP; Its temperature is 90 ℃; The coagulating bath in third level washing zone contains the deionized water solution of 0.1%wt NMP, and its temperature is 90 ℃, is conveyed into temperature again and is 95 ℃ three grades 100% further washing of deionized water sprinkle washing zone; Inputing to temperature then is drying and the drawing-off that 160 ℃ of three-stage drying drafting systems carry out fiber, and be that 60s imports up-coiler at last and is wound into the polyphenylene sulfide finished fiber drying time.Polyphenyl thioether spinning speed is 1500m/min.The drawing-off multiplying power of strand is 3 times.
Embodiment 2
The polyphenylene sulfide of drying is added in 280 ℃ of sulfolane solvents; Be mixed with the sulfolane liquation that contains the 90%wt polyphenylene sulfide; Being 280 ℃ of double screw extruder meltings once more with the liquation input temp then, is the melt metering pump of the variable-frequency motor of 50Hz with liquation through head gear pump incoming frequency again, imports spinning pack through measuring pump; After filter element filtration in the spinning pack; From temperature is the polyphenylene sulfide liquation fiber that 280 ℃ spinnerets ejection contains sulfolane solvent, and after the liquation fiber was equipped with the 300mm temperature and is 80 ℃ of coagulating bath crystallisation by cooling zones through the spinnerets below, it was that to contain the deionized water solution of 20%wt NMP defeated that its crystallisation by cooling zone freezing is bathed; Be conveyed into temperature and be three grades of coagulating bath sinks that contain the deionized water solution of different N MP concentration of 80 ℃; The coagulating bath in first order washing zone contains the deionized water solution of 8%wt NMP, and its temperature is 80-90 ℃, and the coagulating bath in washing zone, the second level contains the deionized water solution of 5%wt NMP; Its temperature is 80 ℃; The coagulating bath in third level washing zone contains the deionized water solution of 1%wt NMP, and its temperature is 80 ℃, is conveyed into temperature again and is 85 ℃ three grades 100% further washing of deionized water sprinkle washing zone; Inputing to temperature then is drying and the drawing-off that 180 ℃ of three-stage drying drafting systems carry out fiber, and be that 30s imports up-coiler at last and is wound into the polyphenylene sulfide finished fiber drying time.Polyphenyl thioether spinning speed is 1800m/min.The drawing-off multiplying power of strand is 6 times.
Embodiment 3
The polyphenylene sulfide of drying is added in 270 ℃ of sulfolane solvents; Being mixed with the sulfolane liquation that contains the 85%wt polyphenylene sulfide, is 278 ℃ of double screw extruder meltings once more with the liquation input temp then, is the melt metering pump of the variable-frequency motor of 35Hz with liquation through head gear pump incoming frequency again; Import spinning pack through measuring pump; After filtering through filter element in the spinning pack, be the polyphenylene sulfide liquation fiber that 278 ℃ spinnerets ejection contains sulfolane solvent from temperature, the liquation fiber is installed after the 200mm temperature is 70 ℃ of coagulating bath crystallisation by cooling zones through the spinnerets below; Be conveyed into temperature and be three grades of coagulating bath sinks that contain the deionized water solution of different N MP concentration of 85 ℃; The coagulating bath in first order washing zone contains the deionized water solution of 7%wt NMP, and its temperature is 85 ℃, and the coagulating bath in washing zone, the second level contains the deionized water solution of 4%wt NMP; Its temperature is 85 ℃; The coagulating bath in third level washing zone contains the deionized water solution of 0.6%wt NMP, and its temperature is 85 ℃, is conveyed into temperature again and is 90 ℃ three grades 100% further washing of deionized water sprinkle washing zone; Inputing to temperature then is drying and the drawing-off that 170 ℃ of three-stage drying drafting systems carry out fiber, and be that 45s imports up-coiler at last and is wound into the polyphenylene sulfide finished fiber drying time.Polyphenyl thioether spinning speed is 1600m/min.The drawing-off multiplying power of strand is 4 times.
Claims (4)
1. polyphenyl thioether spinning technology; Produce the polyphenylene sulfide fiber; Adopting process is :-3 grades of dry drawing-off-coiling doffs of-three grades of sprinkle washings of fiber-grade polyphenyl thioether resin fusion-screw extruder fusion-melt metering pump-forced filtration-spinning pack-strand coagulating bath crystallisation by cooling-three grade coagulating bath washing are produced finished fiber; It is characterized in that, adopt in the following process conditions to comprise:
1) fusion of polyphenylene sulfide comprises: with weight average molecular weight be the polyphenylene sulfide of 4.8-5.2 to be fused to temperature be among the 260-280 ℃ of sulfolane solvent, be mixed with to contain the sulfolane liquation that polyphenylene sulfide is 80-90%wt;
2) with 1) the sulfolane liquation that contains polyphenylene sulfide that obtains uses the direct input temp of conveying worm to be the 275-280 ℃ of further melting of double screw extruder; By its head gear pump input melt metering pump; After the head forced filtration; By the spinning pack ejection, the temperature of spinning pack remains on 275-280 ℃;
3) with 2) fiber that contains sulfolane and polyphenylene sulfide of ejection directly input below spinnerets, to be assembled with strand coagulating bath crystallisation by cooling zone be 0-300mm; After coming out from crystal region, washs strand through 3 grades of coagulating baths; 3 grades of sprinkle water washings; Input strand drying device, strand are after super-dry, and input up-coiler doff manufactures polyphenylene sulfide fibre.
2. the polyphenyl thioether spinning technology according to claim 1; It is characterized in that; Described polyphenyl thioether spinning speed is 1500-1800m/min; It is the deionized water solution that contains 20-30%wt NMP that the crystallisation by cooling zone freezing is bathed, and its crystallisation by cooling zone freezing bath solution temperature is 60-80 ℃; The coagulating bath in first order washing zone contains the deionized water solution of 6-8%wt NMP; The coagulating bath in washing zone, the second level contains the deionized water solution of 3-5%wtNMP; The coagulating bath in third level washing zone contains the deionized water solution of 0.1-1%wtNMP; The first-three grade of sprinkle water washing zone is 100% deionized water solution, and the temperature of three grades of coagulating bath wash solutions is 80-90 ℃, and the temperature of three grades of sprinkle wash solutions is 85-95 ℃.
3. according to claim 1 or 2 said polyphenyl thioether spinning technologies, the variable-frequency motor rotational frequency that it is characterized in that said melt metering pump is 20-50Hz, and dry drawing temperature is controlled at 120-160 ℃, and be 30-60s drying time.
4. according to claim 1 or 2 said polyphenyl thioether spinning technologies, when it is characterized in that the liquation spinning of described fiber-grade polyphenyl thioether resin the drawing-off multiplying power of strand be 3-6 doubly.
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| CN201110066321.8A CN102677194B (en) | 2011-03-18 | 2011-03-18 | Polyphenylene sulfide spinning technology |
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| CN201110066321.8A CN102677194B (en) | 2011-03-18 | 2011-03-18 | Polyphenylene sulfide spinning technology |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103088461A (en) * | 2013-01-27 | 2013-05-08 | 陈逊 | Manufacturing process of polyphenylene sulfide macrofiber |
| CN103484964A (en) * | 2013-09-16 | 2014-01-01 | 东华大学 | Method for preparing low-porosity polyacrylonitrile-based carbon fiber precursors |
| CN105544001A (en) * | 2016-03-01 | 2016-05-04 | 苏州金泉新材料股份有限公司 | Method for directly preparing PPS (polyphenylene sulfide) modified short fibers through modification of PPS powder |
| CN114232379A (en) * | 2021-11-29 | 2022-03-25 | 大连工业大学 | A kind of preparation method of high-performance polyphenylene sulfide fiber paper |
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| CN103088461A (en) * | 2013-01-27 | 2013-05-08 | 陈逊 | Manufacturing process of polyphenylene sulfide macrofiber |
| CN103484964A (en) * | 2013-09-16 | 2014-01-01 | 东华大学 | Method for preparing low-porosity polyacrylonitrile-based carbon fiber precursors |
| CN103484964B (en) * | 2013-09-16 | 2015-08-12 | 东华大学 | A kind of preparation method of low-porosity polyacrylonitrile base carbon fiber precursors |
| CN105544001A (en) * | 2016-03-01 | 2016-05-04 | 苏州金泉新材料股份有限公司 | Method for directly preparing PPS (polyphenylene sulfide) modified short fibers through modification of PPS powder |
| CN114232379A (en) * | 2021-11-29 | 2022-03-25 | 大连工业大学 | A kind of preparation method of high-performance polyphenylene sulfide fiber paper |
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