CN101280465A - Production method of polyphenyl thioether filament - Google Patents
Production method of polyphenyl thioether filament Download PDFInfo
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- CN101280465A CN101280465A CNA2008100111579A CN200810011157A CN101280465A CN 101280465 A CN101280465 A CN 101280465A CN A2008100111579 A CNA2008100111579 A CN A2008100111579A CN 200810011157 A CN200810011157 A CN 200810011157A CN 101280465 A CN101280465 A CN 101280465A
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Abstract
Disclosed is a polyphenylene sulphide PPS filament production method. After the precrystallization the PPS resin slice is sent to a filled-drying tower, the drying is proceeded with the use of the dehumidifying high purity nitrogen. The drying temperature is controlled at 165 DEG C, and the drying time is 6 hours. After the drying, the PPS resin slice relies on the dead weight to enter a screw extruder for the meltdown. The controlling temperature of each zone of the screw extruder is 260/310/318/325/322 DEG C, and then after the meltdown through the screw extruder the PPS resin slice enters a spinning manifold to spin. The filament spraying pressure is 220kg/cm2. After heated through a heater, the as-spun fiber sprayed through a spraying plate is in cooling molding through a lateral blow in which the temperature is controlled at 22 DEG C. The cooled fibers are in winding shaping through a winding head with the winding speed of 1000m/min. After the fiber winding, a parallel drafting machine is adopted for the processing of the drafting setting with the drafting speed of 500m/min, the drafting temperature of 105 DEG C and the setting temperature of 140 DEG C. Therefore, the fiber produced through the method of the invention has the advantages of high fracture strength, low fracture growth, high thermal stability, chemical resistance and so on.
Description
Technical field
The present invention relates to a kind of production method of synthetic fiber filament, specifically is the production method of polyphenyl thioether filament.
Background technology
Polyphenylene sulfide fibre also claims the PPS fiber, and the PPS fiber is a kind of high-performance fiber, and it has outstanding heat resistance chemical resistance, anti-flammability, excellent mechanical property and electrical property.Again because its price is relatively low in many high-performance fibers.Therefore it is once the attention that many industries occur being subjected to immediately, and the PPS fiber also is widely used in many fields such as high temperature fume dust removal, strong corrosive medium filtration, radiation proof Work Clothes and light industry, papermaking, food just because of this.China began to carry out the research and development and the application of PPS resin and PPS staple fibre in 1994, nineteen ninety-five discloses resin manufacture process patent (ZL95111471.9), PPS staple fibre process patent (CN20040096068.0) was disclosed in 2004, introduce the information of Dutch Diolen industry FCFC's exploitation and spinning PPS multifilament in June, 2006 on the international chemical fibre magazine first, in June, 2005, U.S. FIT company declared, the said firm is suitability for industrialized production PPS staple fibre, monofilament, multifilament, product such as melt spraying non-woven fabrics and film, and application and dust arrester, the blowdown control system, papermaking, food and airplane structural parts etc.Hence one can see that, surplus nearest ten year in domestic and international many companies and research unit all making great efforts to research and develop PPS fiber and preparation method and Application Areas thereof.And it is very extensive to have obtained on certain achievement, particularly fire resistant filter material and the corrosion-resistant filtering material application market, is quite paid attention to.
Belong to that the industrial production process of PPS long filament is domestic also to have some units to research and develop in recent years, at present domestic do not have production line that a company can form stable suitability for industrialized production PPS long filament and complete technology preparation method as yet, more do not have a family can produce the applicable PPS long filament of function admirable by industrial production device.Before the present invention, once had in " long stapled manufacture method of polyphenylene sulfide and equipment " patent disclosure in December, 2006 disclosed (200610012937.6), yet this patent has just been introduced the method and apparatus that well-known dissolving spinning prepares long filament.Do not put to the proof out various performance indications and same external PPS long filament performance comparison with the preparation PPS long filament of this patented technology; In the preparation yarn process of its introduction, do not point out to prepare peculiar place on the technology of PPS long filament and long filaments such as preparation PET, PA and the equipment yet.
Summary of the invention
The production method that the purpose of this invention is to provide a kind of polyphenyl thioether filament.
The technical scheme that adopts is:
A kind of production method of polyphenyl thioether filament comprises following process steps:
1, select materials:
The fibre resin of preparation PPS fiber requires the PPS resin to possess:
(1), must be the linear polyphenylthioether fluoropolymer resin;
(2), PPS repetitive ratio should be greater than 90%;
(3), the dissolving index is 45-300g/min;
(4), the polydispersity index of polymer in the 1.39-1.94 scope, MFR is 50-100g/min.
2, before spinning, the PPS resin slicer of choosing is placed on continous mode and gives crystallization on crystallizing bed, give crystallization temperature and be controlled to be 110-150 ℃, gave crystallization time 1.5-4 hour.Give crystallization treatment by what the PPS resin carried out, not only remove the water of PPS resin adsorption, and make the resin crystallization that wherein is in non-crystalline state, improve resin softening point.
3, the PPS resin slicer that above-mentioned process is given crystallization treatment enters the fill-type drying tower, utilizes the dehumidification high pure nitrogen to carry out drying, and baking temperature is 160-200 ℃, and be 6-14 hour drying time, and dry back PPS resin is moisture≤80ppm.
Adopt the dehumidification nitrogen drying, it is adhered to one another to prevent that the PPS resin from producing in dry run, and can fully in time get rid of the moisture of discharging in the dry run, the existence of oxygen in the deaeration simultaneously.Avoid taking place in the dry run pyrohydrolysis and high-temperature oxydation reaction.
4, dried PPS resin slicer leans on and reenters screw rod extruding carrying out fusion certainly, and adds the high pure nitrogen protection at the screw extruder feeding mouth, to prevent PPS resin slicer high-temperature oxydation.Screw extruder divides five sections to add thermal control, first section heating-up temperature is 230-260 ℃, and second section heating-up temperature is 280-310 ℃, and the 3rd section heating-up temperature is 290-320 ℃, the 4th section heating-up temperature is 290-325 ℃, and the 5th section heating-up temperature is 300-340 ℃.
5, in entering spinning manifold on the melting weaving production line, the PPS of screw extruder fusion resin slicer carries out spinning, spinning temperature is controlled at 280-340 ℃, by a plurality of spinneret orifice ejections on the spinnerets, spray silk Pressure control is at 120-220kg/cm after the measuring pump metering for the PPS resin slicer of fusion
2, heating through post-heater through the as-spun fibre of spray line plate ejection, heating and temperature control is after 250-300 ℃, again through the lateral blowing cooling forming.The lateral blowing wind-warm syndrome is controlled at 18-24 ℃.
6, cooled PPS fiber is through the winding head coiling and molding, winding speed 800-2500m/min.To the PPS silk of above-mentioned winding with high-intensity parallel drafting machine drafting forming, to improve the physical and mechanical property of PPS long filament.Adopt the hot drawing-off technology of secondary, wherein first order draw ratio is 1.1-1.5 times, and second level draw ratio is 3.5-5.0 times, first order drawing-off heating-up temperature is 90-130 ℃, drawing-off heating-up temperature in the second level is 160-200 ℃, all adopts the hot plate heating, and the total draft multiple is 6-8 times.Setting temperature is controlled at 95-220 ℃, and draft speed is controlled at 300-900m/min, filament number 1.5-6dtex.
Advantage: the fiber of producing with method of the present invention has the fracture strength height, advantages such as extension at break is low, heat endurance is high, chemical resistance.
The specific embodiment
Embodiment one
A kind of production method of polyphenyl thioether filament comprises following processing step:
1, select the linear polyphenylene sulfide section for use, the polydispersity index of polymer is 1.85, and the dissolving index is 95g/min, and fluoropolymer resin gives crystallization on crystallizing bed before spinning, and crystallization temperature is controlled at 130 ℃, and crystallization time is 1.5 hours.
2, the polyphenylene sulfide section that will give after the crystallization is fed into the fill-type drying tower, utilizes the dehumidification high pure nitrogen to carry out drying, and baking temperature is controlled at 165 ℃, and drying time, dried polyphenylene sulfide section was moisture about 60ppm at 6 hours.
3, dry back polyphenylene sulfide section is by carrying out fusion from reentering screw extruder, and screw extruder is Φ 65mm, 1: 25 Ba Mage screw rod of draw ratio, and each district's control temperature of screw extruder is 260/310/318/325/322.
4, enter spinning manifold through the section of the polyphenylene sulfide of screw extruder fusion and carry out spinning, by the spinneret orifice ejection, The hole diameter of spinneret is 0.3mm through spinning pump metering back in the polyphenylene sulfide section of fusion, and a spray pressure is 220kg/cm
2After the as-spun fibre of spinnerets ejection heats through post-heater, carry out cooling forming with lateral blowing, the post-heater temperature is controlled at 260 ℃, and the lateral blowing wind-warm syndrome is controlled at 22 ℃, cooled fiber is through the winding head coiling and molding, winding speed 1000m/min, processing adopts the parallel drafting machine to carry out drafting forming behind the undrawn yarn, and draft speed is 500m/min, 105 ℃ of drawing temperatures, 140 ℃ of setting temperatures.The polyphenylene sulfide fibre physical index of producing is as follows: total fiber number: 125dtex, and specific elongation: 22%, elongation cv%:6.82%, powerful relatively: 2.87cN/dtex.
Embodiment two
A kind of production method of polyphenyl thioether filament, be to select linear polyphenylene sulfide for use, the polydispersity index of polymer is 1.85, the dissolving index is 95g/min, give crystallization on fluoropolymer resin crystallizing bed before spinning, crystallization temperature is controlled at 130 ℃, crystallization time is 1.5 hours, the polyphenylene sulfide section enters the fill-type drying tower after giving crystallization, utilize dehumidification nitrogen to carry out drying, baking temperature is controlled at 165 ℃, drying time was at 8 hours, dried polyphenylene sulfide section is moisture about 50ppm, the polyphenylene sulfide section of dry back is by carrying out fusion from reentering screw extruder, screw extruder is Φ 65mm, 1: 25 Ba Mage screw extruder of draw ratio, each district's control temperature of screw extruder is 320/331/328/325/322, enter spinning manifold through the section of the polyphenylene sulfide of screw extruder fusion and carry out spinning, the polyphenylene sulfide section of fusion is sprayed by spinneret orifice after the spinning pump metering, The hole diameter of spinneret is 0.3mm, behind the as-spun fibre process post-heater of spinnerets ejection, carry out cooling forming with lateral blowing, the post-heater temperature is controlled at 290 ℃, the lateral blowing wind-warm syndrome is controlled at 22 ℃, cooled fiber is through the winding head coiling and molding, winding speed is 1300m/min, and processing adopts the parallel drafting machine to carry out drafting forming behind the undrawn yarn, and draft speed is 500m/min, drawing temperature is 110 ℃, 160 ℃ of setting temperatures.The polyphenylene sulfide fibre physical index of producing is as follows: fiber number: 133.6dtex, and specific elongation: 26.1%, elongation cv%:8.06%, powerful relatively: 3.32cN/dtex.
Claims (3)
1, a kind of production method of polyphenyl thioether filament comprises following process steps:
1), select materials:
The fibre resin of preparation PPS fiber requires the PPS resin to possess:
(1), must be the linear polyphenylthioether fluoropolymer resin;
(2), PPS repetitive ratio should be greater than 90%;
(3), the dissolving index is 45-300g/min;
(4), the polydispersity index of polymer in the 1.39-1.94 scope, MFR is 50-100g/min;
2), before spinning, the PPS resin slicer of choosing is placed on continous mode and gives crystallization on crystallizing bed, give crystallization temperature and be controlled to be 110-150 ℃, gave crystallization time 1.5-4 hour; Give crystallization treatment by what the PPS resin carried out;
3), PPS resin slicer that above-mentioned process is given crystallization treatment enters the fill-type drying tower, utilizes the dehumidification high pure nitrogen to carry out drying, baking temperature is 160-200 ℃, be 6-14 hour drying time, dry back PPS resin is moisture≤80ppm;
4), dried PPS resin slicer is by carrying out fusion from reentering screw rod extruding, and adds the high pure nitrogen protection at the screw extruder feeding mouth, to prevent PPS resin slicer high-temperature oxydation; Screw extruder divides five sections to add thermal control, first section heating-up temperature is 230-260 ℃, and second section heating-up temperature is 280-310 ℃, and the 3rd section heating-up temperature is 290-320 ℃, the 4th section heating-up temperature is 290-325 ℃, and the 5th section heating-up temperature is 300-340 ℃;
5), in entering spinning manifold on the melting weaving production line, the PPS of screw extruder fusion resin slicer carries out spinning, spinning temperature is controlled at 280-340 ℃, by a plurality of spinneret orifice ejections on the spinnerets, spray silk Pressure control is at 120-220kg/cm after the measuring pump metering for the PPS resin slicer of fusion
2, heating through post-heater through the as-spun fibre of spray line plate ejection, heating and temperature control is after 250-300 ℃, again through the lateral blowing cooling forming; The lateral blowing wind-warm syndrome is controlled at 18-24 ℃;
6), cooled PPS fiber is through the winding head coiling and molding, winding speed 800-2500m/min; To the PPS silk of above-mentioned winding with high-intensity parallel drafting machine drafting forming, to improve the physical and mechanical property of PPS long filament; Adopt the hot drawing-off technology of secondary, wherein first order draw ratio is 1.1-1.5 times, and second level draw ratio is 3.5-5.0 times, first order drawing-off heating-up temperature is 90-130 ℃, the heating-up temperature of drawing-off for the second time is 160-200 ℃, all adopts the hot plate heating, and the total draft multiple is 6-8 times; Setting temperature is controlled at 95-220 ℃, and draft speed is controlled at 300-900m/min, filament number 1.5-6dtex.
2, the production method of a kind of polyphenyl thioether filament according to claim 1, the polydispersity index that it is characterized in that described polymer is 1.85, the dissolving index is 95g/min, give crystallization temperature and be controlled at 130 ℃, giving crystallization time is 1.5 hours, and in the fill-type drying tower of polyphenylene sulfide section, baking temperature is 165 ℃, be 6 hours drying time, and dry back moisture is at 60ppm; It is 260/310/318/325/322 that described screw extruder is respectively distinguished temperature; Described The hole diameter of spinneret is 0.3mm, and spray silk pressure is 220kg/cm
2, the lateral blowing temperature is 22 ℃, and back heating and temperature control is at 260 ℃, and described winding speed is 1000m/min, and hauling speed is 500m/min, and the traction temperature is 105 ℃, and setting temperature is 140 ℃.
3, the production method of a kind of polyphenyl thioether filament according to claim 1, the polydispersity index that it is characterized in that described polymer is 1.85, the dissolving index is 95g/min, give crystallization temperature and be controlled at 130 ℃, crystallization time is 1.5 hours, the polyphenylene sulfide section is controlled at 165 ℃ in fill-type drying tower inner drying temperature, drying time was at 8 hours, dried polyphenylene sulfide section is moisture to be 50ppm, each district's control temperature of screw extruder is 320/331/328/325/322, and The hole diameter of spinneret is 0.3mm, and described post-heater temperature is controlled at 290 ℃, the lateral blowing wind-warm syndrome is controlled at 22 ℃, winding speed is 1300m/min, the undrawn yarn drafting forming, and draft speed is 500m/min, drawing temperature is 110 ℃, 160 ℃ of setting temperatures.
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| CNA2008100111579A CN101280465A (en) | 2008-04-23 | 2008-04-23 | Production method of polyphenyl thioether filament |
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| CNA2008100111579A CN101280465A (en) | 2008-04-23 | 2008-04-23 | Production method of polyphenyl thioether filament |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560717A (en) * | 2011-12-19 | 2012-07-11 | 东华大学 | High-strength low-contract polyphenylene sulfide filament and preparation method thereof |
| CN102797052A (en) * | 2012-08-23 | 2012-11-28 | 江苏金达福高分子材料科技有限公司 | Manufacturing method of high-strength polyphenyl thioether filament |
| CN102877141A (en) * | 2012-08-17 | 2013-01-16 | 苏州市兴吴工程塑胶有限公司 | Direct spinning method suitable for chemical fibers |
| CN103242659A (en) * | 2013-05-31 | 2013-08-14 | 常熟市金泉化纤织造有限责任公司 | Method for increasing viscosity of polyphenylene sulfide resin before spinning |
| CN103409835A (en) * | 2013-08-05 | 2013-11-27 | 江苏瑞泰科技有限公司 | Fine denier polyphenylene sulfide short fiber production method |
| CN104532436A (en) * | 2014-12-29 | 2015-04-22 | 太原理工大学 | Multistage stretching heat shaping method of polyphenylene sulfide filament |
| CN115506040A (en) * | 2022-10-11 | 2022-12-23 | 山东明化新材料有限公司 | Spinning method for directly melt-extruding polyphenylene sulfide powder |
-
2008
- 2008-04-23 CN CNA2008100111579A patent/CN101280465A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560717A (en) * | 2011-12-19 | 2012-07-11 | 东华大学 | High-strength low-contract polyphenylene sulfide filament and preparation method thereof |
| CN102560717B (en) * | 2011-12-19 | 2013-10-30 | 东华大学 | High-strength low-contract polyphenylene sulfide filament and preparation method thereof |
| CN102877141A (en) * | 2012-08-17 | 2013-01-16 | 苏州市兴吴工程塑胶有限公司 | Direct spinning method suitable for chemical fibers |
| CN102797052A (en) * | 2012-08-23 | 2012-11-28 | 江苏金达福高分子材料科技有限公司 | Manufacturing method of high-strength polyphenyl thioether filament |
| CN103242659A (en) * | 2013-05-31 | 2013-08-14 | 常熟市金泉化纤织造有限责任公司 | Method for increasing viscosity of polyphenylene sulfide resin before spinning |
| CN103409835A (en) * | 2013-08-05 | 2013-11-27 | 江苏瑞泰科技有限公司 | Fine denier polyphenylene sulfide short fiber production method |
| CN104532436A (en) * | 2014-12-29 | 2015-04-22 | 太原理工大学 | Multistage stretching heat shaping method of polyphenylene sulfide filament |
| CN104532436B (en) * | 2014-12-29 | 2016-09-28 | 太原理工大学 | A kind of multistage stretching heat setting method of polyphenyl thioether filament |
| CN115506040A (en) * | 2022-10-11 | 2022-12-23 | 山东明化新材料有限公司 | Spinning method for directly melt-extruding polyphenylene sulfide powder |
| CN115506040B (en) * | 2022-10-11 | 2024-04-26 | 山东明化新材料有限公司 | Spinning method for directly melting and extruding polyphenylene sulfide powder |
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Open date: 20081008 |