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CN101161873A - Polyphenylene sulfide filament one-step method complete plant and production method - Google Patents

Polyphenylene sulfide filament one-step method complete plant and production method Download PDF

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Publication number
CN101161873A
CN101161873A CNA200710124609XA CN200710124609A CN101161873A CN 101161873 A CN101161873 A CN 101161873A CN A200710124609X A CNA200710124609X A CN A200710124609XA CN 200710124609 A CN200710124609 A CN 200710124609A CN 101161873 A CN101161873 A CN 101161873A
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China
Prior art keywords
polyphenylene sulfide
production method
polyphenyl thioether
zone
filament
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CNA200710124609XA
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Chinese (zh)
Inventor
侯庆华
杨新华
邓佶
连宏光
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SHENZHEN ZHONGCHENG FIBER ENGINEERING TECHNOLOGY Co Ltd
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SHENZHEN ZHONGCHENG FIBER ENGINEERING TECHNOLOGY Co Ltd
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Priority to CNA200710124609XA priority Critical patent/CN101161873A/en
Publication of CN101161873A publication Critical patent/CN101161873A/en
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Abstract

The present invention specifies a polyphenylene sulfide filament one-step method complete plant and a method for producing the same. The invention provides a method for producing the polyphenylene sulfide filament to eliminate the shortcomings and disadvantages of the two-step method in the prior art. The invention mainly chooses linear polyphenylene sulfide slices, adopts the polyphenylene sulfide one-step method technique and plant and has melt spinning on the polyphenylene sulfide slices between 280 DEG C and 340 DEG C; after the fusant ejects out, , polyphenylene sulfide filament is produced by winding in a winding speed between 1500 m/min and 4500 m/min through a solidification process in a slow cooling zone, a non-wind zone and a cooling zone and a continuous multiway drafting shaping. The method of the invention is stable in production process, high in manufacturing rate, easy in management, high in efficiency, low in cost and good in product quality.

Description

Polyphenyl thioether filament one-step method complete set of equipments and production method
Technical field
The invention belongs to the technical field of special chemical fiber, particularly polyphenyl thioether filament one-step method complete set of equipments and production method.
Background technology
Polyphenylene sulfide (English name Polyphenylene Sulfide, abbreviation PPS) fiber is at first succeeded in developing by U.S.'s Philips (Philip) oil company.The said firm developed the PPS resin of fibre-grade in 1979 in PPS resin suitability for industrialized production in 1973, the industrialization of nineteen eighty-three PPS staple fibre.Because polyphenylene sulfide fibre has good serviceability, Japanese Japan is spun, east is beautiful, Supreme Being people and Bayer A.G also develop and produce polyphenylene sulfide fibre in succession.
Polyphenylene sulfide can be made into long filament and staple fibre, because textile processibility energy and good chemical resistance, heat endurance, heat-resisting quantity and anti-flammability are preferably arranged, in environmental protection, flue and fields such as chemical industry high temperature filtration and Aero-Space, have widely and use, as steam power plant, coal-burning boiler, waste incineration, cement plant high-temperature flue filter bag; Corrosion-resistant filter cloth in the chemical industry; Dry zone in paper industry and the electrical industry, Nomex; The special cable cladding; Flame-retardant textile in the aerospace industry etc.
Polyphenylene sulfide is a thermoplastic, its melt temperature is about 285 ℃, the Japan Patent spy opens clear 57-143518, the spy opens two-step process and the equipment that flat 1-229809 all discloses the drawing-off of polyphenylene sulfide fibre fusion low speed spinning low speed, after being the low speed spinning silk winding, on draft apparatus, carry out the drafting forming production polyphenyl thioether filament of reeling again again, defectives such as this kind method energy consumption is big, processing cost is high, efficient is low, and the polyphenyl thioether filament quality homogeneity of producing is poor, and lousiness is many.
Summary of the invention
The objective of the invention is to problems such as big at the prior art energy consumption, that processing cost is high, efficient is low and the product quality homogeneity is poor, lousiness is many, the complete set of equipments and the production method that provide a kind of stable production process, manageability, row yielding height, cost are low, efficient is high and the one-step method of good product quality is produced polyphenyl thioether filament.
Polyphenyl thioether filament one-step method complete set of equipments of the present invention comprises spinning technique device and drawing-off coiler device.Wherein the spinning technique device is made up of screw extruder, filter, measuring pump and transmission device, spinning manifold, filament spinning component and spinnerets, slow cooling district, zone of silence, cooling zone and path etc.; The drawing-off coiler device is then by oiling roller, godet roller, five groups of drawing roller, pre-Network device, master network devices with reel first-class the composition.
The present invention includes the step of following order:
(1). melt spinning: high-temperature fusion is carried out in the section of the linear polyphenylene sulfide behind the pre-crystallizing and drying in screw extruder.
(2). slow cooling-calm-cooling: melt is after the spinnerets ejection, through slow cooling district-zone of silence-cooling zone solidified forming.
(3). the multiple tracks drawing-off is reeled: the fiber of solidified forming enters the typing of multiple tracks continuous drafting after oiling.
The polyphenylene sulfide slice that the present invention adopts is a kind of polymer of linear structure,
Figure S200710124609XD00011
Construction unit content 〉=70%mol/mol, best 〉=90%mol/mol.Its melt index (MFR) should be 20~600g/10min, is preferably 30~300g/10min.MFR is excessive, the fiberizing difficulty, and MFR is low excessively, melt extrudes difficulty, is difficult to processing.
The present invention is in the melt spinning process, and melt temperature is 280~340 ℃, and spinneret orifice diameter is selected 0.1~1.0mm for use.Because polyphenylene sulfide belongs to the high-elasticity thermoplastic material, spinneret orifice draw ratio L/D is 3.0~10.0 comparatively suitable, and preferably the aperture is at 0.3~0.6mm, and L/D is 3.0~8.0.
The present invention is in slow cooling-calm-cooling procedure, and at first by a slow cooling district, mainly be made up of heater by this zone after spinneret orifice is extruded for polyphenylene sulfide fibre, and its mode of heating of this heater mainly is electrical heating and biphenyl heating; Its profile for operation ease, but can be made into the form of folding for the insulation cartridge type.Its position is 1~30cm place below spinnerets, is preferably in 5~10cm place, and the length of this buffer unit is 10~50cm, is preferably in 20~40cm, and the temperature in slow cooling district is controlled at 190~300 ℃, preferably is controlled at 200~280 ℃.
Polyphenylene sulfide fibre continues by a cooling zone after by slow cooling district and zone of silence, and wind-warm syndrome is controlled at 15~30 ℃, preferably is controlled at 20~25 ℃.Cooling media is an air.
Its drafting forming process of polyphenylene sulfide fibre of the present invention is one and is higher than the process of carrying out drawing-off and typing in the polyphenylene sulfide glass temperature environment that it adds thermal medium is electrical heating.Its drawing temperature of application, drawing-off multiplying power according to polyphenyl thioether filament are different.For the degree of orientation and the degree of crystallinity that improves fiber, reduce the dry-hot shrinkage of fiber, its drafting process can be divided into 3 roads or 4 road drawing-offs are carried out, the total draft multiplying power is controlled at 1.5~6.0 times, preferably be controlled at 2.5~5.0 times, 80~260 ℃ of drawing temperatures, drawing temperature preferably are controlled at 90~250 ℃.In carrying out the multiple tracks drafting process, its total draft multiple can be assigned to each road drawing-off and finish.As when adopting 3 road drawing-offs, the 1st road drawing-off multiplying power is 1.1~1.5 times of total draft multiplying power, and the 2nd road drawing-off multiplying power is 1.8~3.5 times of total draft multiplying power, and the 3rd road drawing-off multiplying power is 1.05~1.2 times of total draft multiplying power.If when adopting 4 road drawing-offs, the 1st road drawing-off multiplying power is 1.1~1.4 times of total draft multiplying power, the 2nd road drawing-off multiplying power is 2~3.5 times of total draft multiplying power, and the 3rd road drawing-off multiplying power is 1.05~1.2 times of total draft multiplying power, and the 4th road drawing-off multiplying power is 1.01~1.15 times of total draft multiplying power; Setting temperature is controlled at 150~280 ℃, preferably be controlled at 160~260 ℃, loose rate is 8.0~11.0%, preferably being controlled at its winding speed of 2.0~4.0%. polyphenylene sulfide fibre is 1500~4500m/min, according to line density polyphenylene sulfide slice and fibre single thread, its winding speed is controlled at 2000~4000m/min usually.
Its final filament line density of polyphenylene sulfide fibre of the present invention is at 0.5~10.0dtex, preferably be controlled at 1.0~8.0dtex, usually the line density of usefulness is controlled at 2.0~7.0dtex, every bundle polyphenylene sulfide fibre can be made up of some filaments, perhaps can the doubling of multiple fibre plying form according to using also.
Technique effect of the present invention is: the linear polyphenylene sulfide section of selecting function admirable for use, adopt custom-designed one-step method to spin and lead the combination machine complete set of equipments, through the strict process control process, can produce all more excellent polyphenyl thioether filaments of performance such as fracture strength, extension at break, dry-hot shrinkage, stable production process, manageability, row yielding height, cost is low, efficient is high and the product quality homogeneity is good, no lousiness.
The invention will be further described below in conjunction with drawings and Examples.
Description of drawings
Accompanying drawing is a polyphenyl thioether filament single step spining complete set of equipments schematic diagram
1-screw extruder 2-filter 3-melt pipe 4-measuring pump 5-spinnerets
10-path, 6-spinning manifold 7-slow cooling district 8-zone of silence 9-cooling zone
Second group of drawing roller of first group of drawing roller 14-of 11-oiling roller 12-godet roller 13-
The 5th group of drawing roller 18-master network of the 4th group of drawing roller 17-of the 3rd group of drawing roller 16-of 15-device
The 19-winding head
The present invention selects the polyphenylene sulfide slice of moisture content≤30PPM after super-dry of function admirable, is injected into screw extruder Melting in 1,280~340 ℃ of melt temperatures filter out impurity through filter 2, and melt passes through melt pipe 3 through measuring pump 4 Enter ejection in the spinneret 5 in the spinning manifold 6 after the metering, the spun filament of ejection is through slow cooling district 7, zone of silence 8, cooling zone 9 and path 10. The slow cooling district is positioned at 1~30cm place, spinneret below, and slow cooling district temperature is controlled at 190~300 ℃, the cooling zone wind-warm syndrome Be controlled at 15~30 ℃. The spinneret orifice diameter of spinneret is at 0.1~1.0mm, and spinneret orifice L/D ratio (L/D) is 3.0~10.0. Fiber behind the cooling curing oils through oiling roller 11 and enters draw roll 13,14,15,16,17 by godet 12 and carry out multiple tracks Many times of drafting forming, fiber enters in the winding head 19 behind master network device 18 networks and reels then. Drafting multiple is 1.5~6.0 Doubly, drawing temperature is 80~260 ℃, and setting temperature is 150~280 ℃, and winding speed is 1500~4500m/min. That makes is poly-Diphenyl sulfide long filament ultimate fibre line density is 0.5~10.0dtex.
The specific embodiment
Embodiment 1
Adopt MFR to be the section of 170g/10min linear polyphenylene sulfide, melt extrude at screw rod for fear of polyphenylene sulfide slice and to produce putty in the process, cause pressure oscillation, oxidative degradation and situation such as crosslinked, before melt spinning, carry out dry polyphenylene sulfide slice in known vacuum drum or pre-crystallizing and drying equipment, moisture content is 23PPM.Extruder temperature is 280~325 ℃ during spinning, 320 ℃ of spin manifold temperatures, and The hole diameter of spinneret 0.3mm, draw ratio (L/D) is 6, and the spinnerets hole count is 60 holes, and the slow cooling offset is from 10cm place, spinnerets below, 240 ℃ of slow cooling district temperature; 25 ℃ of cooling zone wind-warm syndrome; Oil by 1.5% rate of oiling; Adopt three road drawing-offs to carry out drawing-off, the total draft multiple is 3.8 times, each road drawing roller temperature and multiple, and setting temperature, winding speed and polyphenyl thioether filament physical index ginseng are shown in Table 1.
Embodiment 2 and embodiment 3 spinning conditions adopt four road drafting process all with embodiment 1 when only being drawing-off, draw conditions and physical index ginseng are shown in Table 1.
It is the linear polyphenylene sulfide section of 210g/10min that embodiment 4 and embodiment 5 have adopted MFR, spinning condition, and drawing-off coiling condition and physical index are shown in Table 1.
Table 1 embodiment technological parameter and rerum natura table

Claims (7)

1. polyphenyl thioether filament one-step method complete set of equipments and production method is characterized in that apparatus for melt spinning and drawing-off winding apparatus form whole process and the complete set of equipments of system integration and the production method that can produce polyphenyl thioether filament continuously.
2. polyphenyl thioether filament one-step method complete set of equipments and production method is characterized in that comprising the steps:
(1) melt spinning: high-temperature fusion is carried out in the section of the linear polyphenylene sulfide behind the pre-crystallizing and drying in screw extruder.
(2) slow cooling-calm-cooling: melt is after the spinnerets ejection, through slow cooling district-zone of silence-cooling zone solidified forming.
(3) the multiple tracks drawing-off is reeled: the fiber of solidified forming enters the typing of multiple tracks continuous drafting after oiling.
3. according to the production method of claim 1,2 described polyphenyl thioether filaments, it is characterized in that in the linear polyphenylene sulfide section Construction unit content 〉=90% (mol/mol), melt index MFR are 20~600g/10min.
4. according to the production method of claim 1,2 described polyphenyl thioether filaments, it is characterized in that the melt temperature of linear polyphenylene sulfide section in screw extruder is 280~340 ℃, The hole diameter of spinneret is 0.1~1.0mm, and draw ratio L/D is 3.0~10.0.
5. according to the production method of claim 1,2 described polyphenyl thioether filaments, it is characterized in that 10cm place, spinnerets below is provided with the slow cooling district, slow cooling district temperature is controlled at 190~300 ℃, and the cooling zone wind-warm syndrome is controlled at 15~30 ℃.
6. according to the production method of claim 1,2 described polyphenyl thioether filaments, it is characterized in that being provided with zone of silence between slow cooling district and the cooling zone, zone of silence length is 10~50cm.
7. according to the production method of claim 1,2 described polyphenyl thioether filaments, it is characterized in that having adopted 3 roads or 4 road continuous draftings, the total draft multiple is 1.5~6.0 times, drawing temperature is 80~260 ℃, setting temperature is 150~280 ℃, winding speed is 1500~4500m/min, and making the filamentary line density of polyphenyl thioether filament is 0.5~10dtex.
CNA200710124609XA 2007-11-19 2007-11-19 Polyphenylene sulfide filament one-step method complete plant and production method Pending CN101161873A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101942703A (en) * 2010-07-20 2011-01-12 江苏瑞泰科技有限公司 Spinning spinneret for polyphenylene sulfide fiber high-capacity spinning
CN102677198A (en) * 2011-03-18 2012-09-19 四川得阳工程塑料开发有限公司 Polyphenylene sulfide (PPS) nascent fiber drafting and setting technology
CN102677194A (en) * 2011-03-18 2012-09-19 四川得阳工程塑料开发有限公司 Polyphenylene sulfide spinning technology
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
CN103060935A (en) * 2013-01-10 2013-04-24 常熟鑫宇织造有限公司 Production method of PPS (polyphenylene sulfite) and PET (polyethylene glycol terephthalate) blended and melted spun yarns
CN105696102A (en) * 2016-02-22 2016-06-22 苏州金泉新材料股份有限公司 Method for preparing polyphenylene sulfide short fibers by direct melt extrusion of polyphenylene sulfide powder

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101942703A (en) * 2010-07-20 2011-01-12 江苏瑞泰科技有限公司 Spinning spinneret for polyphenylene sulfide fiber high-capacity spinning
CN102677198A (en) * 2011-03-18 2012-09-19 四川得阳工程塑料开发有限公司 Polyphenylene sulfide (PPS) nascent fiber drafting and setting technology
CN102677194A (en) * 2011-03-18 2012-09-19 四川得阳工程塑料开发有限公司 Polyphenylene sulfide spinning technology
CN102677198B (en) * 2011-03-18 2015-01-21 四川得阳工程塑料开发有限公司 Polyphenylene sulfide (PPS) nascent fiber drafting and setting technology
CN102677194B (en) * 2011-03-18 2015-04-01 四川得阳工程塑料开发有限公司 Polyphenylene sulfide spinning technology
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
CN103060935A (en) * 2013-01-10 2013-04-24 常熟鑫宇织造有限公司 Production method of PPS (polyphenylene sulfite) and PET (polyethylene glycol terephthalate) blended and melted spun yarns
CN105696102A (en) * 2016-02-22 2016-06-22 苏州金泉新材料股份有限公司 Method for preparing polyphenylene sulfide short fibers by direct melt extrusion of polyphenylene sulfide powder

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Open date: 20080416