CN103088446A - Preparation method of polyether sulfone fiber - Google Patents
Preparation method of polyether sulfone fiber Download PDFInfo
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- CN103088446A CN103088446A CN201110340493XA CN201110340493A CN103088446A CN 103088446 A CN103088446 A CN 103088446A CN 201110340493X A CN201110340493X A CN 201110340493XA CN 201110340493 A CN201110340493 A CN 201110340493A CN 103088446 A CN103088446 A CN 103088446A
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Abstract
The invention provides a preparation method of polyether sulfone fibers, and relates to the field of resin spinning. The method comprises the steps of heating and melting the polyether sulfone resin with the water content meeting the spinning requirement by using a single-screw extruder, flowing out in a trickle mode through a spinning assembly, directly entering a drafting and shaping winding machine after cooling and solidification, heating and drafting through a hot roller, and then winding to obtain the final polyether sulfone fiber. The temperature of a feeding section of the single-screw extruder is 300-340 ℃; the temperature of the compression section and the melting section is 310-380 ℃; the temperature of the metering section is 320-390 ℃; the temperature between two drafting hot rollers of the drafting and shaping winder is increased by 10-40 ℃; the temperature of the upper hot roller is lower than that of the lower hot roller, the temperature of the upper hot roller is 90-130 ℃, and the temperature of the lower hot roller is 110-150 ℃. The method of the invention simplifies the process, shortens the time, makes the method closer to the actual production and is suitable for popularization.
Description
Technical field
The present invention relates to a kind of preparation method of fibrous material, say further, relate to a kind of preparation method of polyether sulfone fiber.
Background technology
Polyethersulfone resin is a kind of thermal plastic high polymer of excellent combination property, is one of special engineering plastics few in number that is applied at present, and characteristics are performances outstanding under high temperature.Recurring group See Figure in molecule:
Polyether sulfone is to be found by Union Carbide Corporation in nineteen sixty-five the earliest, polyethersulfone resin is developed in 1972 by Britain ICI company, but due to its prices of raw and semifnished materials and processing charges costliness, general as special engineering plastics, performance under normal temperature is similar to Merlon, is widely used in a lot of fields at present.
The excellent in performance of polyethersulfone resin comprises:
Heat resistance: in the thermoplastic resin of all melt-processable, the serviceability temperature of polyether sulfone is the highest.225 ℃ of vitrification points, 203 ℃ of heat distortion temperatures, long-term serviceability temperature 180-200 ℃; Can anti-150-160 ℃ hot water or steam; Modulus can remain unchanged under-100 ℃-150 ℃.
Flame resistance is good: have self-extinguishment, even burning is not fuming yet, limited oxygen index (LOI) can reach more than 30%, and airborne initial heat decomposition temperature reaches 454 ℃.Need not add any fire retardant namely to have flame-retarding characteristic, avoid the mechanicalness loss of energies such as intensity.Anti-combustion grade UL94-VO.
Creep resistant is good: the strain under 150 ℃ and 20MPa pressure only has 2.55%.
Good stability of the dimension: size distortion is less than 0.1% in the steam of boiling water and 150 ℃.
Chemical proofing is good: in pH is the scope of 2-13, inorganic acid, alkali and electrolyte are had very strong tolerance, the cleaning agents such as anti-gasoline, machine oil, lubricated wet goods oils and fluorine Lyons, but also surfactant-tolerant and hydrocarbon ils.Can keep stable in most non-polar solven, but dissolve in carrene and methyl pyrrolidone isopolarity solvent.
At present the main available extrusion moulding of polyethersulfone resin is made the section bars such as sheet material, bar, tubing, film, and makes milipore filter or reverse osmosis membrane with solwution method, also can be made into coating with polytetrafluoroethylene (PTFE), or is processed into superfine powder and carries out powder spray.Aspect sanitary standard, approved by U.S. FDA, also meet the requirement of No. the 434th, Japanese health ministry and No. 178 bulletins.What the present finding of fiber-like product was more is the Polyethersulfone Hollow Fiber Plasma filter membrane, and main method is that polyether sulfone and solvent additive etc. is added in container, and dissolving at a certain temperature obtains stable solution, then through wet spinning, the steps such as supersolidification bath obtain milipore filter at last.Also mentioned the method that obtains polyether sulfone fiber with electrostatic spinning in U.S. Patent application US2009/0047515A1, be about on the polymer solution band several thousand to volt high-pressure electrostatics up to ten thousand, charged polymer liquid drops under the effect of electric field force accelerated.When electric field force was enough large, the polymer drop overcame surface tension and forms the injection thread.Thread is solvent evaporation or curing in course of injection, finally drops on the method that forms fiber on receiving system.Utilize melt spinning to carry out the research of polyether sulfone fiber preparation in prior art less, only having in the people's such as Zhang Tianjiao the Chinese patent CN1763278A of Beijing Institute of Clothing Tech uses double screw extruder with the polyether sulfone heating and melting, flow out through the form of high temperature resistant filament spinning component with the melt thread, after cooling curing by the up-coiler winding shaping, balance is after a period of time, then obtains final polyether sulfone fiber through the parallel drafting machine drawing-off.Also have the people such as Yu Jianming of Tianjin Textile Industry College did on the homemade plunger melt spinning machine in laboratory melt spinning experiment (Yu Jianming, Zhou Xiaofeng etc. the polyether sulfone fiber development. Tianjin Textile Industry College journal .1996 (15) 2:14-17).Japan has one piece of patent JP3185025A to mention the melt spinning method of polyether sulfone fiber in addition, but does not mention the concrete grammar of spinning and drawing-off etc.Its melt spinning be partly with polyethersulfone resin in melting more than 300 ℃, pull out with the speed more than 50m/ minute the spinnerets of the spinneret orifice of 0.1～2.0mm from a plurality of apertures are arranged, make fibrous.
More than utilize the limitation of the research that melt spinning is prepared polyether sulfone fiber to be: adopt double screw extruder or homemade plunger type equipment, rather than modal single screw extrusion machine in spinning, equipment is complicated, and cost increases; Melt extrude and reel obtain fiber after, carry out again drawing-off after balance a period of time, and do not adopt the higher one-step method of efficient, namely directly through the hot-rolling drawing-off, coiling obtains the FDY one-step method of finished silk to the polyether sulfone silk at last after cooling curing.
The complete method of utilizing at present melt spinning to carry out the preparation of polyether sulfone fiber is moisture content to be reached the polyethersulfone resin double screw extruder heating and melting of spinning requirement, flow out through the form of resistant to elevated temperatures filament spinning component with thread, after cooling curing, the fiber that forms is batched, balance is after a period of time, then obtains final polyether sulfone fiber through the parallel drafting machine drawing-off.
Summary of the invention
For above problems of the prior art, the present invention is intended to also make polyether sulfone fiber with the FDY one-step method through the melt spinning drawing-off with the common single screw extrusion machine of spinning.
Therefore, the purpose of this invention is to provide a kind of preparation method of polyether sulfone fiber, it is simple, easy and simple to handle, more economical that the method has equipment, is easy to the advantages such as popularization.
Method provided by the invention is moisture content to be reached the polyethersulfone resin single screw extrusion machine heating and melting of spinning requirement, flow out through the form of filament spinning component with thread, after cooling curing, directly enter the drafting forming up-coiler, heat drawing-off by hot-rolling, then batch and obtain final polyether sulfone fiber.
The preparation method of polyether sulfone fiber of the present invention specifically comprises the following steps:
(1) dry polyethersulfone resin makes it moisture content and meets the spinning standard, and namely general water content requirement gets final product at 50-200ppm;
(2) above polyethersulfone resin is melt extruded with single screw extrusion machine, and be squeezed into filament spinning component and carry out melt spinning.
When generally, polyethersulfone resin melt extrudes with single screw extrusion machine, the problem of difficult feed can appear.Because polyethersulfone resin is complete amorphous polymer, and common single screw rod designs for semi-crystalline polymer.Common single screw rod is divided into feed zone, compression section, melt zone, metering section, feed zone is designed to the temperature lower than the material fusing point, the temperature of compression section is equivalent to the material fusing point, and melt zone and metering section are completed the mushy stage conversion higher than the material fusing point so that material concentrates on melt zone.As identical technique is used for complete unbodied polyethersulfone resin, because amorphous material does not have definite fusing point, only has an extremely wide in range flow temperature, material is in the compression section, and even feed zone, namely begin adhesion agglomerating, charging smoothly is called the link resistance material with this phenomenon in the industry.So, more than method of the present invention respectively distinguishes with single screw rod the flow temperature that temperature all is set in polyether sulfone.Specific requirement is: 300～340 ℃ of feed zones, preferred 305～325 ℃; Compression section and melt zone 310-380 ℃, preferred 320-350 ℃; Metering section 320-390 ℃, preferred 330-360 ℃.Polyethersulfone resin gets final product smooth melting with this understanding, and is squeezed into filament spinning component.
Described filament spinning component is usually filament spinning component used, general heatproof 350-420 ℃.Spinning temperature is also the common spinning temperature of polyether sulfone fiber spinning, is generally 340～400 ℃.
(3) spun silk in above-mentioned filament spinning component is directly introduced the drafting forming up-coiler incessantly, heat drawing-off by hot-rolling, then batch and obtain the polyether sulfone fiber finished product.Need not common equilibrium step, can save equilibration time, and save the required energy of the peaceful weighlock maintenance constant temperature and humidity of occupation of land between balance, enhance productivity and benefit.
The production of general general fibre (as terylene, polyamide fibre etc.), can adopt the high one-step method of efficient, be in filament spinning component spun silk through cooling curing (as under the lateral blowing condition through the spinning shaft cooling curing) directly introduce the drawing-off of drafting forming up-coiler hot-rolling after oiling, reeling at last obtains the FDY one-step method of finished silk.But its technique is only applicable to the fiber that this class has the hypocrystalline structure usually.The temperature of drawing-off hot-rolling used needs below the fusing point of polymer, more than glass transition temperature, to guarantee that fiber had both had certain deformability in drawing-off, can keep certain tensile strength again.
But as complete unbodied polyether sulfone, only have glass transition temperature and there is no a fusing point, namely can sharply descend in case surpass the tensile strength of its glass transition temperature fiber, thus the fibrous fracture of making, drawing-off smoothly.Therefore, the melt spinning of polyether sulfone fiber is to need to pass through balance usually, can not complete in a step.Investigate by theory analysis and practice, the inventor all is arranged on the temperature of two drawing-off hot-rollings of drafting forming up-coiler between the glass transition temperature and secondary transition temperature of polyether sulfone, and there are 10～40 ℃ between two rollers, the temperature of preferred 15～25 ℃ increases progressively, and the temperature of upper hot-rolling is lower than lower heat roller temperature.The temperature of upper hot-rolling is 90～130 ℃, and preferred 100～115 ℃, the temperature of lower hot-rolling is 110～150 ℃, preferred 120～140 ℃.Velocity ratio between drafting forming up-coiler two rollers (being drafting multiple) can reach 1.8-2.5.Coiling speed can reach 800-2000m/min.Spin actual, tow is walked from top to bottom, and top roll is slow, and lower roll is fast, and last batching by a friction roller controlled, and the speed of friction roller is near lower roll, slightly soon or slightly slowly to adjust tension force, coiling speed refers to the speed of friction roller.
The polyether sulfone fiber performance indications of final finished can reach: filament number 1.5-15dtex, fracture strength 1.5-3.2cN/dtex, extension at break 6-20%.Meet follow-up weaving requirement fully.
The present invention selects single screw extrusion machine to be because single screw extrusion machine is conventional spinning equipment, and is compared with the double screw extruder low price, easy and simple to handle; Selecting the FDY one-step method to be because the FDY one-step method saves time more, is also the important method in conventional resin spinning.Therefore, the preparation method of polyether sulfone fiber provided by the invention has simplified the preparation technology of present polyether sulfone fiber, has shortened the time, makes it more press close to produce real 11 borders, is suitable for promoting, for its suitability for industrialized production is laid a good foundation.
The specific embodiment
Further describe the present invention below in conjunction with embodiment.Scope of the present invention is not subjected to the restriction of these embodiment, and scope of the present invention proposes in claims.
Embodiment 1
With polyether sulfone section through vacuumize to moisture＜200ppm, adopt single screw extrusion machine to melt extrude.The temperature of respectively distinguishing of screw rod is: 305 ℃ of feed zones, 317 ℃ of compression sections, 322 ℃ of melt zones, 332 ℃ of metering sections.By (spinning temperature is 345 ℃) after the filament spinning component wire vent, under the lateral blowing condition through the spinning shaft cooling curing, silk after oiling is directly introduced the drafting forming up-coiler, carry out drafting forming at the up and down hot-rolling, wherein going up heat roller temperature is 96 ℃, speed 445m/min, lower heat roller temperature is 135 ℃, speed 848m/min, drafting multiple are 1.9 times, the coiling speed 830m/min of up-coiler.
The polyether sulfone fiber that finally obtains, filament number 7.2dtex, fracture strength 2.2CN/dtex, extension at break 17%.
Embodiment 2
With polyether sulfone section through vacuumize to moisture＜200ppm, adopt single screw extrusion machine to melt extrude.The temperature of respectively distinguishing of screw rod is: 320 ℃ of feed zones, 330 ℃ of compression sections, 332 ℃ of melt zones, 343 ℃ of metering sections.By (spinning temperature is 345 ℃) after the filament spinning component wire vent, under the lateral blowing condition through the spinning shaft cooling curing, silk after oiling is directly introduced the drafting forming up-coiler, carry out drafting forming at the up and down hot-rolling, wherein going up heat roller temperature is 110 ℃, speed 556m/min, lower heat roller temperature is 128 ℃, speed 1334m/min, drafting multiple are 2.4 times, the coiling speed 1300m/min of up-coiler.
The polyether sulfone fiber that finally obtains, filament number 6.5dtex, fracture strength 3.0CN/dtex, extension at break 11%.
Embodiment 3
With polyether sulfone section through vacuumize to moisture＜200ppm, adopt single screw extrusion machine to melt extrude.The temperature of respectively distinguishing of screw rod is: 335 ℃ of feed zones, 360 ℃ of compression sections, 370 ℃ of melt zones, 380 ℃ of metering sections.By (spinning temperature is 345 ℃) after the filament spinning component wire vent, under the lateral blowing condition through the spinning shaft cooling curing, silk after oiling is directly introduced the drafting forming up-coiler, carry out drafting forming at the up and down hot-rolling, wherein going up heat roller temperature is 125 ℃, speed 1055m/min, lower heat roller temperature is 147 ℃, speed 1947m/min, drafting multiple are 1.8 times, the coiling speed 1900m/min of up-coiler.
The polyether sulfone fiber that finally obtains, filament number 12.0dtex, fracture strength 1.6CN/dtex, extension at break 7%.
Comparative example 1
With polyether sulfone section through vacuumize to moisture＜200ppm, adopt single screw extrusion machine to melt extrude.The temperature of respectively distinguishing of screw rod is: 350 ℃ of feed zones, 385 ℃ of compression sections, 390 ℃ of melt zones, 395 ℃ of metering sections.Because extruder temperature is too high, extrude the melt color and luster of (spinning temperature is 345 ℃) by filament spinning component and send out crow, the sign of degraded is arranged, under the lateral blowing condition after spinning shaft, tow waft silk, fracture of wire is serious, can't introduce the drafting forming up-coiler.
Comparative example 2
With polyether sulfone section through vacuumize to moisture＜200ppm, adopt single screw extrusion machine to melt extrude.The temperature of respectively distinguishing of screw rod is: 295 ℃ of feed zones, 300 ℃ of compression sections, 305 ℃ of melt zones, 318 ℃ of metering sections.Because extruder temperature is too low, extrude (spinning temperature is 345 ℃) by filament spinning component, melt pressure increases rapidly, and through the spinning shaft cooling curing, after oiling, the column cap silk is more, can't introduce the drafting forming up-coiler under the lateral blowing condition.
Comparative example 3
With polyether sulfone section through vacuumize to moisture＜200ppm, adopt single screw extrusion machine to melt extrude.The temperature of respectively distinguishing of screw rod is: 320 ℃ of feed zones, 330 ℃ of compression sections, 332 ℃ of melt zones, 338 ℃ of metering sections.After the filament spinning component wire vent, through the spinning shaft cooling curing, the silk after oiling is directly introduced the drafting forming up-coiler under the lateral blowing condition, carry out drafting forming at the up and down hot-rolling, wherein going up heat roller temperature is 145 ℃, speed 500m/min, and lower heat roller temperature is 153 ℃.Due to the up-down rollers excess Temperature, the temperature difference is too small, no matter descends hot-rolling speed how to arrange always fracture of wire occurs, and can't reel, and can not get finished fiber.
Comparative example 4
With polyether sulfone section through vacuumize to moisture＜200ppm, adopt single screw extrusion machine to melt extrude.The temperature of respectively distinguishing of screw rod is: 320 ℃ of feed zones, 330 ℃ of compression sections, 332 ℃ of melt zones, 338 ℃ of metering sections.After the filament spinning component wire vent, under the lateral blowing condition through the spinning shaft cooling curing, silk after oiling is directly introduced the drafting forming up-coiler, carries out drafting forming at the up and down hot-rolling, and wherein going up heat roller temperature is 85 ℃, speed 300m/min, lower heat roller temperature is 135 ℃, and because upper roll temperature is too low, no matter excessive temperature differentials descends hot-rolling speed how to arrange, and fracture of wire always occurs, can't reel, can not get finished fiber.
Comparative example 5
With polyether sulfone section through vacuumize to moisture＜200ppm, adopt single screw extrusion machine to melt extrude.The temperature of respectively distinguishing of screw rod is: 320 ℃ of feed zones, 330 ℃ of compression sections, 332 ℃ of melt zones, 338 ℃ of metering sections.After the filament spinning component wire vent, through the spinning shaft cooling curing, the silk after oiling is directly introduced the drafting forming up-coiler, carries out drafting forming at the up and down hot-rolling under the lateral blowing condition, wherein going up heat roller temperature is 115 ℃, speed 800m/min, lower heat roller temperature is 135 ℃, Speed Setting is 2100m/min, because spinning speed is too fast, the excessive tow of speed ratio produces more lousiness between the hot-rolling of up and down, can't reel, and can not get finished fiber.
Claims (5)
1. the preparation method of a polyether sulfone fiber comprises the following steps:
(1) dry polyethersulfone resin;
(2) above polyethersulfone resin is melt extruded with single screw extrusion machine, and be squeezed into filament spinning component, then through the filament spinning component melt spinning;
Described single screw rod is divided into feed zone, compression section, melt zone, metering section, and wherein the feed zone temperature is 300～340 ℃; 310-380 ℃ of compression section and melt zone temperature; 320-390 ℃ of metering section temperature;
(3) spun silk in above-mentioned filament spinning component is directly introduced the drafting forming up-coiler incessantly, heat drawing-off by hot-rolling, then batch and obtain the polyether sulfone fiber finished product;
Wherein the temperature between two drawing-off hot-rollings of drafting forming up-coiler has 10～40 ℃ increasing progressively; The temperature of upper hot-rolling is lower than lower heat roller temperature; Upper heat roller temperature is 90～130 ℃, and the temperature of lower hot-rolling is 110～150 ℃.
2. the preparation method of polyether sulfone fiber according to claim 1 is characterized in that:
Described in described step (2), single screw rod is divided into feed zone, compression section, melt zone, metering section, and wherein the feed zone temperature is 305～325 ℃; 320-350 ℃ of compression section and melt zone temperature; 330-360 ℃ of metering section temperature.
3. the preparation method of polyether sulfone fiber according to claim 1 is characterized in that:
Temperature between two drawing-off hot-rollings of drafting forming up-coiler described in described step (3) has 15～25 ℃ increasing progressively; 100～115 ℃ of the temperature of upper hot-rolling, the temperature of lower hot-rolling are 120～140 ℃.
4. the preparation method of polyether sulfone fiber according to claim 1 is characterized in that:
In described step (1), dry polyethersulfone resin to its moisture content is 50-200ppm.
5. the preparation method of according to claim 1～3 described polyether sulfone fibers of any one is characterized in that:
Velocity ratio between described step (3) two rollers is 1.8～2.5; Coiling speed is 800～2000m/min.
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Cited By (5)
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| CN103361748A (en) * | 2013-07-25 | 2013-10-23 | 绍兴文理学院 | Method for producing high-temperature-resistant PES (polyether sulfone) fibers by melting method |
| CN103572500A (en) * | 2013-11-13 | 2014-02-12 | 泰安鲁普耐特塑料有限公司 | Polyether sulfone fiber compound rope and preparation method thereof |
| CN108004617A (en) * | 2017-12-15 | 2018-05-08 | 常州创赢新材料科技有限公司 | A kind of polyether-ether-ketone/polyether sulfone composite fibre and preparation method thereof |
| CN110382761A (en) * | 2017-03-03 | 2019-10-25 | 住友化学株式会社 | The manufacturing method of non-woven fabrics |
| CN111364119A (en) * | 2020-04-29 | 2020-07-03 | 廖国庆 | Preparation method of polyether sulfone short fiber |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103361748A (en) * | 2013-07-25 | 2013-10-23 | 绍兴文理学院 | Method for producing high-temperature-resistant PES (polyether sulfone) fibers by melting method |
| CN103361748B (en) * | 2013-07-25 | 2015-09-23 | 绍兴文理学院 | Fusion method produces the method for high temperature resistant PES fiber |
| CN103572500A (en) * | 2013-11-13 | 2014-02-12 | 泰安鲁普耐特塑料有限公司 | Polyether sulfone fiber compound rope and preparation method thereof |
| CN110382761A (en) * | 2017-03-03 | 2019-10-25 | 住友化学株式会社 | The manufacturing method of non-woven fabrics |
| US11174573B2 (en) | 2017-03-03 | 2021-11-16 | Sumitomo Chemical Company, Limited | Production method of nonwoven fabric |
| CN110382761B (en) * | 2017-03-03 | 2022-05-10 | 住友化学株式会社 | Method for producing nonwoven fabric |
| CN108004617A (en) * | 2017-12-15 | 2018-05-08 | 常州创赢新材料科技有限公司 | A kind of polyether-ether-ketone/polyether sulfone composite fibre and preparation method thereof |
| CN108004617B (en) * | 2017-12-15 | 2021-03-02 | 常州创赢新材料科技有限公司 | Polyether-ether-ketone/polyether-sulfone composite fiber and preparation method thereof |
| CN111364119A (en) * | 2020-04-29 | 2020-07-03 | 廖国庆 | Preparation method of polyether sulfone short fiber |
| CN111364119B (en) * | 2020-04-29 | 2022-09-23 | 辽宁欧瑞康环境技术有限公司 | Preparation method of polyether sulfone short fiber |
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