CN102677194B - Polyphenylene sulfide spinning technology - Google Patents
Polyphenylene sulfide spinning technology Download PDFInfo
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- CN102677194B CN102677194B CN201110066321.8A CN201110066321A CN102677194B CN 102677194 B CN102677194 B CN 102677194B CN 201110066321 A CN201110066321 A CN 201110066321A CN 102677194 B CN102677194 B CN 102677194B
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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 manufacture 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 high temperature, and has fire-retardant, insulation, radiation hardness and good mechanical performance.For expanding the scope of application of this material, the researchers of various countries are finding the new method making it fibration and use always.
A kind of melt spinning of linear high molecular weight polyphenylene sulfide fiber grade resins, stretching heat setting method is disclosed in Chinese patent CN1603477; Chinese patent CN1876906 discloses the long stapled manufacture method of polyphenylene sulfide; Several polyphenylene sulfide is described by melt-melting the method for the polyphenylene sulfide fibre that spinning obtains in US Patent No. 5405695 and US4500706.The shortcoming of these methods is that the mechanical strength of product fiber is still not high enough, although the heating region of melting-spinning extruder is divided into three regions by US5405695, only may produce long fiber, and its mechanical strength indicator conditions is undistinct.
In Chinese Patent Application No. code CN200510022439.5, describe a kind of polyphenylene sulfide melt spinning method, the method does not still depart from the pattern of melt spinnings all at present.
Object of the present invention starts a kind of spinning process of brand-new polyphenylene sulfide fibre, its objective is the disqualification rate reducing polyphenylene sulfide fibre, improve and put spinning speed, the preliminary treatment of few polyphenylene sulfide and drying are waited processing step, also reduce simultaneously and vacuumize as double screw extruder the unnecessary equipment and process operation removing volatile materials, reduce production cost, improve each performance indications such as fibre strength.
Summary of the invention
Tech. polyphenyl thioether spinning, produce polyphenylene sulfide fiber, employing technique is: fiber-grade polyphenyl thioether resin melts---screw extruder melting---and melt metering pump---forced filtration, spinning pack---strand coagulating bath crystallisation by cooling---six bathe washing admittedly---and finished fiber produced by---drawing-off---winding doff, adopts following process conditions to comprise:
1, the melting of polyphenylene sulfide comprises: be that to be fused to temperature be among 260-280 DEG C of sulfolane solvent for the polyphenylene sulfide of 4.8-5.2 by weight average molecular weight, and being mixed with containing polyphenylene sulfide is the sulfolane liquation of 80-90%wt;
2, by 1) what obtain is the 275-280 DEG C of further melting of double screw extruder containing the direct input temp of sulfolane liquation conveying worm of polyphenylene sulfide, melt metering pump is inputted by its head gear pump, the variable-frequency motor rotational frequency of melt metering pump is 20-50Hz, after crossing head forced filtration, sprayed by spinning pack.The temperature of spinning pack remains on 275-280 DEG C.
3, by 2) fiber containing sulfolane and polyphenylene sulfide that sprays directly inputs that below spinnerets, be assembled with a strand coagulating bath crystallisation by cooling region be 0-300mm, the bath of crystallisation by cooling zone freezing is the deionized water solution containing 20-30%wt NMP, and its temperature is 60-80 DEG C; Strand out washs through the coagulating bath of 3-6 level afterwards from crystal region, the deionized water solution of coagulating bath containing 6-8%wt NMP of first order washing zone, the deionized water solution of coagulating bath containing 3-5%wt NMP of second level washing zone, the deionized water solution of coagulating bath containing 0.1-1%wt NMP of third level washing zone, the first-three grades sprinkle water washing regions are 100% deionized water solution; Wherein the temperature of three grades of coagulating bath wash solutions is 80-90 DEG C, and the temperature of three grades of sprinkle wash solutions is 85-95 DEG C.Input strand drying device, it is 30-60s that dry drawing temperature controls 120-160 DEG C 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 draft ratio of strand is 3-6 times.
The present invention adopts liquation spinning technique, decrease current all melt spinnings need poly-p-phenylene sulfide ether resin to carry out purifying and spin case and heating and thermal insulation medium and thermostat, improve the spinning speed of polyphenylene sulfide fibre, the strand of the polyphenylene sulfide fibre of weaving out is like this well-balanced, can not produce the advantages such as any molten drop.Adopt method of the present invention, the property made and the mechanical strength of obtained polyphenylene sulfide fibre silk are all improved, and fracture strength is greater than 4CN/dt, and 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 is all the same, the all melts pipeline of polyphenylene sulfide liquation all must be incubated simultaneously, and its temperature remains in the scope of under polyphenylene sulfide fusing point 5-10 DEG C; Measuring pump variable-frequency motor frequency by feeding number and fiber line density limit, its frequency is generally under the scope of 2-30 hertz; General spin pack pressure remains on spinning pack between 1-28 Mpa and uses front pretreatment temperature that its temperature also will be made to remain in the scope of under polyphenylene sulfide fusing point 5-10 DEG C; Strand crystallisation by cooling curing area suitably will regulate according to when ground temperature on the one hand, also regulate according to the line density of fiber or degree of draft on the other hand, up-coiler variable-frequency motor frequency is subject on the one hand to how many restrictions of feeding machine feeding, consider that producd fibers line density limits, up-coiler variable-frequency motor frequency general control is in the scope of 5-200 hertz, between one-level up-coiler and secondary up-coiler, there is certain hertz difference, namely winder winding is around speed difference simultaneously.
The present invention first will through filtering, extraction, washing, the polyphenylene sulfide of dry synthesis adds in 260-280 DEG C of sulfolane solvent, be mixed with the sulfolane liquation containing 80-90%wt polyphenylene sulfide, then be 275-280 DEG C of double screw extruder melting again by liquation input temp, be the melt metering pump of the variable-frequency motor of 20-50Hz again through head gear pump incoming frequency by liquation, spinning pack is inputted through measuring pump, after filter element in spinning pack filters, from the polyphenylene sulfide liquation fiber of spinnerets ejection containing sulfolane solvent that temperature is 275-280 DEG C, liquation fiber is after being provided with 0-300mm temperature and being 60-80 DEG C of coagulating bath crystallisation by cooling region below spinnerets, be conveyed into the coagulating bath sink that temperature is 80-90 DEG C the three grades deionized water solutions containing different N MP concentration, being conveyed into temperature is again that the deionized water sprinkle washing zone of 85-95 DEG C three grades 100% is washed further, then drying and drawing-off that three-stage drying drafting system carries out fiber is inputed to, finally input winder winding and be coiled into polyphenylene sulfide finished fiber.So just obtain polyphenylene sulfide fibre.
accompanying drawing explanation:
Fig. 1 is technological process block-diagram of the present invention.
Accompanying drawing of the present invention illustrates summary:
Polyphenylene sulfide is fused in the sulfolane solvent of 260-280 DEG C with certain percentage by weight, then the further melting of double screw extruder is inputted, extruded by its head gear pump and be conveyed into measuring pump, by the metering input spinning pack of measuring pump, then spray by spinnerets the coagulating bath solution entered containing 20-30%NMP solvent and form strand, strand is after three grades of low concentration NMP coagulating bath is washed further, again after three grades of deionized water sprinkle washings, inputting three grades of temperature is that the drying device of 160-180 DEG C carries out dry drawing-off, finally obtained polyphenylene sulfide finished fiber.
detailed description of the invention:
embodiment 1
The polyphenylene sulfide of drying is added in 260 DEG C of sulfolane solvents, be mixed with the sulfolane liquation containing 80%wt polyphenylene sulfide, then be 275 DEG C of double screw extruder meltings again by liquation input temp, be the melt metering pump of the variable-frequency motor of 20Hz again through head gear pump incoming frequency by liquation, spinning pack is inputted through measuring pump, after filter element in spinning pack filters, from the polyphenylene sulfide liquation fiber of spinnerets ejection containing sulfolane solvent that temperature is 275 DEG C, liquation fiber is after being provided with 0mm temperature and being 60 DEG C of coagulating bath crystallisation by cooling regions below spinnerets, the bath of its crystallisation by cooling zone freezing is that the deionized water solution containing 30%wt NMP is defeated, send into the coagulating bath sink that temperature is 80 DEG C the three grades deionized water solutions containing different N MP concentration, the deionized water solution of coagulating bath containing 6%wt NMP of first order washing zone, its temperature is 90 DEG C, the deionized water solution of coagulating bath containing 3%wt NMP of second level washing zone, its temperature is 90 DEG C, the deionized water solution of coagulating bath containing 0.1%wt NMP of third level washing zone, its temperature is 90 DEG C, being conveyed into temperature is again that the deionized water sprinkle washing zone of 95 DEG C three grades 100% is washed further, then inputing to temperature is drying and the drawing-off that 160 DEG C of three-stage drying drafting systems carry out fiber, drying time is that 60s finally inputs winder winding and is coiled into polyphenylene sulfide finished fiber.Polyphenyl thioether spinning speed is 1500m/min.The draft ratio of strand is 3 times.
embodiment 2
The polyphenylene sulfide of drying is added in 280 DEG C of sulfolane solvents, be mixed with the sulfolane liquation containing 90%wt polyphenylene sulfide, then be 280 DEG C of double screw extruder meltings again by liquation input temp, be the melt metering pump of the variable-frequency motor of 50Hz again through head gear pump incoming frequency by liquation, spinning pack is inputted through measuring pump, after filter element in spinning pack filters, from the polyphenylene sulfide liquation fiber of spinnerets ejection containing sulfolane solvent that temperature is 280 DEG C, liquation fiber is after being provided with 300mm temperature and being 80 DEG C of coagulating bath crystallisation by cooling regions below spinnerets, the bath of its crystallisation by cooling zone freezing is that the deionized water solution containing 20%wt NMP is defeated, be conveyed into the coagulating bath sink that temperature is 80 DEG C the three grades deionized water solutions containing different N MP concentration, the deionized water solution of coagulating bath containing 8%wt NMP of first order washing zone, its temperature is 80-90 DEG C, the deionized water solution of coagulating bath containing 5%wt NMP of second level washing zone, its temperature is 80 DEG C, the deionized water solution of coagulating bath containing 1%wt NMP of third level washing zone, its temperature is 80 DEG C, being conveyed into temperature is again that the deionized water sprinkle washing zone of 85 DEG C three grades 100% is washed further, then inputing to temperature is drying and the drawing-off that 180 DEG C of three-stage drying drafting systems carry out fiber, drying time is that 30s finally inputs winder winding and is coiled into polyphenylene sulfide finished fiber.Polyphenyl thioether spinning speed is 1800m/min.The draft ratio of strand is 6 times.
embodiment 3
The polyphenylene sulfide of drying is added in 270 DEG C of sulfolane solvents, be mixed with the sulfolane liquation containing 85%wt polyphenylene sulfide, then be 278 DEG C of double screw extruder meltings again by liquation input temp, be the melt metering pump of the variable-frequency motor of 35Hz again through head gear pump incoming frequency by liquation, spinning pack is inputted through measuring pump, after filter element in spinning pack filters, from the polyphenylene sulfide liquation fiber of spinnerets ejection containing sulfolane solvent that temperature is 278 DEG C, liquation fiber is after installing 200mm temperature and being 70 DEG C of coagulating bath crystallisation by cooling regions below spinnerets, be conveyed into the coagulating bath sink that temperature is 85 DEG C the three grades deionized water solutions containing different N MP concentration, the deionized water solution of coagulating bath containing 7%wt NMP of first order washing zone, its temperature is 85 DEG C, the deionized water solution of coagulating bath containing 4%wt NMP of second level washing zone, its temperature is 85 DEG C, the deionized water solution of coagulating bath containing 0.6%wt NMP of third level washing zone, its temperature is 85 DEG C, being conveyed into temperature is again that the deionized water sprinkle washing zone of 90 DEG C three grades 100% is washed further, then inputing to temperature is drying and the drawing-off that 170 DEG C of three-stage drying drafting systems carry out fiber, drying time is that 45s finally inputs winder winding and is coiled into polyphenylene sulfide finished fiber.Polyphenyl thioether spinning speed is 1600m/min.The draft ratio of strand is 4 times.
Claims (4)
1. tech. polyphenyl thioether spinning, produce polyphenylene sulfide fiber, employing technique is: finished fiber produced by fiber-grade polyphenyl thioether resin melting-screw extruder melting-melt metering pump-forced filtration-spinning pack-strand coagulating bath crystallisation by cooling-tri-grade coagulating bath washing-tri-grades of sprinkle washings-3 grades of dry drawing-off-winding doffs, it is characterized in that, adopt following process conditions to comprise:
1) melting of polyphenylene sulfide comprises: be that to be fused to temperature be among 260-280 DEG C of sulfolane solvent for the polyphenylene sulfide of 4.8-5.2 ten thousand by weight average molecular weight, and being mixed with containing polyphenylene sulfide is the sulfolane liquation of 80-90%wt;
2) by 1) what obtain is the 275-280 DEG C of further melting of double screw extruder containing the direct input temp of sulfolane liquation conveying worm of polyphenylene sulfide, melt metering pump is inputted by its head gear pump, after head forced filtration, sprayed by spinning pack, the temperature of spinning pack remains on 275-280 DEG C;
3) by 2) fiber containing sulfolane and polyphenylene sulfide that sprays directly inputs a strand coagulating bath crystallisation by cooling region below spinnerets, this crystal region is 0-300mm, strand out washs through 3 grades of coagulating baths afterwards from crystal region, 3 grades of sprinkle water washings, input strand drying device, strand is after super-dry, and input up-coiler doff manufactures polyphenylene sulfide fibre.
2. tech. polyphenyl thioether spinning according to claim 1, it is characterized in that, described polyphenyl thioether spinning speed is 1500-1800m/min, the bath of crystallisation by cooling zone freezing is the deionized water solution containing 20-30%wt NMP, and its crystallisation by cooling zone freezing bath solution temperature is 60-80 DEG C; The coagulating bath of first order washing zone contains the deionized water solution of 6-8%wt NMP, the coagulating bath of second level washing zone contains the deionized water solution of 3-5%wtNMP, the coagulating bath of third level washing zone contains the deionized water solution of 0.1-1%wtNMP, the first-three grades sprinkle water washing regions are 100% deionized water solution, the temperature of three grades of coagulating bath wash solutions is 80-90 DEG C, and the temperature of three grades of sprinkle wash solutions is 85-95 DEG C.
3. the tech. polyphenyl thioether spinning according to claim 1 or 2, it is characterized in that the variable-frequency motor rotational frequency of described melt metering pump is 20-50Hz, dry drawing temperature controls at 120-160 DEG C, and drying time is 30-60s.
4. the tech. polyphenyl thioether spinning according to claim 1 or 2, is characterized in that the draft ratio of strand during the liquation spinning of described fiber-grade polyphenyl thioether resin is 3-6 times.
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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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| CN103088461B (en) * | 2013-01-27 | 2014-08-13 | 陈逊 | Manufacturing process of polyphenylene sulfide macrofiber |
| 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 | Preparation method of high-performance polyphenylene sulfide fiber paper |
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