CN103088446B - Preparation method of polyether sulfone fiber - Google Patents
Preparation method of polyether sulfone fiber Download PDFInfo
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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, and be one of special engineering plastics few in number be applied at present, feature is performance outstanding under high temperature.Recurring group See Figure in molecule:
Polyether sulfone is found by Union Carbide Corporation in nineteen sixty-five the earliest, polyethersulfone resin is developed in 1972 by ICI company of Britain, 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.Vitrification point 225 DEG C, heat distortion temperature 203 DEG C, Long-Time Service temperature 180-200 DEG C; Can resistance to 150-160 DEG C hot water or steam; Modulus can remain unchanged at-100 DEG C-150 DEG C.
Flame resistance is good: have self-extinguishment, even if burning is not also fuming, limited oxygen index (LOI) can reach more than 30%, and the initial heat decomposition temperature in air reaches 454 DEG C.Any fire retardant need not be added and namely have flame-retarding characteristic, avoid the mechanicalness loss of energies such as intensity.Resistance to combustion grade UL94-VO.
Creep resistant is good: the strain under 150 DEG C 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 DEG C.
Chemical proofing is good: in the scope that pH is 2-13, have very strong tolerance to inorganic acid, alkali and electrolyte, and the cleaning agents such as resistance to gasoline, machine oil, lubrication wet goods oils and fluorine Lyons, also can surfactant-tolerant and hydrocarbon ils.Can keep stable in most non-polar solven, but dissolve in carrene and methyl pyrrolidone polar solvent.
The main available extrusion moulding of current polyethersulfone resin makes the section bars such as sheet material, bar, tubing, film, and makes milipore filter or reverse osmosis membrane by solwution method, also can be made into coating with polytetrafluoroethylene (PTFE), or is processed into superfine powder and carries out powder spray.In sanitary standard, approved by U.S. FDA, also meet the requirement of No. 434th, Japanese health ministry and No. 178 bulletins.What the current finding of fiber-like product was more is polyether sulfone hollow fiber filter membrane, and main method adds in container by polyether sulfone and solvent additive etc., dissolve at a certain temperature and obtain stable solution, then through wet spinning, the steps such as supersolidification bath finally obtains milipore filter.Also refer to the method obtaining polyether sulfone fiber with electrostatic spinning in U.S. Patent application US2009/0047515A1, by polymer solution band several thousand to volt high-pressure electrostatic up to ten thousand, charged polymer liquid is accelerated under dropping in the effect of electric field force.When electric field force is enough large, polymer drop overcomes surface tension and forms injection thread.Thread is solvent evaporation or solidification in course of injection, finally falls and forms the method for fiber on the reception device.Research prepared by polyether sulfone fiber is less to utilize melt spinning to carry out in prior art, only having in the Chinese patent CN1763278A of the people such as the Zhang Tianjiao of Beijing Institute of Clothing Tech uses double screw extruder by polyether sulfone heating and melting, flow out with the form of melt stream through high temperature resistant filament spinning component, by up-coiler winding shaping after cooling curing, after balance a period of time, then obtain final polyether sulfone fiber through 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. polyether sulfone fiber is developed. Tianjin Textile Industry College journal .1996 (15) 2:14-17).Japan has one section of patent JP3185025A to refer to 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 part is by polyethersulfone resin melting more than 300 DEG C, from there being multiple aperture to pull out with the speed of more than 50m/ minute the spinnerets of the spinneret orifice of 0.1 ~ 2.0mm, makes threadiness.
The limitation of melt spinning to the research that polyether sulfone fiber is prepared more than is utilized to be: to adopt double screw extruder or homemade plunger type equipment, instead of modal single screw extrusion machine in spinning, equipment is complicated, and cost increases; Melt extrude and after reeling and obtaining fiber, after balance a period of time, carry out drawing-off again, and the one-step method not adopting efficiency higher, namely polyether sulfone silk is directly through hot-rolling drawing-off after cooling curing, and finally winding obtains the FDY one-step method of finished silk.
The complete method utilizing melt spinning to carry out the preparation of polyether sulfone fiber is at present polyethersulfone resin double screw extruder heating and melting moisture content being reached spinning requirement, flow out with the form of thread through resistant to elevated temperatures filament spinning component, after cooling curing, the fiber of formation is batched, after balance a period of time, then obtain final polyether sulfone fiber through parallel drafting machine drawing-off.
Summary of the invention
For above problems of the prior art, the present invention is intended to the common single screw extrusion machine of spinning and obtains polyether sulfone fiber by FDY one-step method through melt spinning drawing-off.
Therefore, the object of this invention is to provide a kind of preparation method of polyether sulfone fiber, it is simple that the method has equipment, easy and simple to handle, more economical, is easy to the advantages such as popularization.
Method provided by the invention is polyethersulfone resin single screw extrusion machine heating and melting moisture content being reached spinning requirement, flow out with the form of thread through filament spinning component, after cooling curing, directly enter drafting forming up-coiler, undertaken adding hot gas spring 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 spinning standard, and namely general water content requirement is at 50-200ppm;
(2) above polyethersulfone resin single screw extrusion machine is melt extruded, and be squeezed into filament spinning component and carry out melt spinning.
Generally, there will be the problem of difficult feed when polyethersulfone resin single screw extrusion machine melt extrudes.Because polyethersulfone resin is complete amorphous polymer, and common singe screw designs for semi-crystalline polymer.Common singe screw is divided into feed zone, compression section, melt zone, metering section, feed zone is designed to the temperature lower than material fusing point, the temperature of compression section is equivalent to material fusing point, and melt zone and metering section, higher than material fusing point, concentrate on melt zone to make material and complete mushy stage conversion.As identical technique is used for complete unbodied polyethersulfone resin, due to the fusing point that amorphous material is not determined, only has the flow temperature that extremely wide in range, then material is in compression section, even feed zone, namely starts adhesion agglomerating, cannot charging smoothly, in the industry this phenomenon is called link resistance material.So each for singe screw district temperature is all set in more than the flow temperature of polyether sulfone by method of the present invention.Specific requirement is: feed zone 300 ~ 340 DEG C, preferably 305 ~ 325 DEG C; Compression section and melt zone 310-380 DEG C, preferred 320-350 DEG C; Metering section 320-390 DEG C, preferred 330-360 DEG C.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 DEG C.Spinning temperature is also the usual spinning temperature of polyether sulfone fiber spinning, is generally 340 ~ 400 DEG C.
(3) silk spun in above-mentioned filament spinning component is directly introduced drafting forming up-coiler incessantly, undertaken adding hot gas spring by hot-rolling, then batch and obtain polyether sulfone fiber finished product.Without the need to common equilibrium step, can equilibration time be saved, and between saving balance, take up an area the energy needed for peaceful weighlock maintenance constant temperature and humidity, enhance productivity and benefit.
The production of general general fibre (as terylene, polyamide fibre etc.), the one-step method that efficiency is high can be adopted, namely in filament spinning component spun silk through cooling curing (as under lateral blowing condition through spinning shaft cooling curing) after oiling, directly introduce the drawing-off of drafting forming up-coiler hot-rolling, finally winding obtains the FDY one-step method of finished silk.But its technique is only applicable to this kind of fiber with semicrystalline structure usually.The temperature of drawing-off hot-rolling used below the fusing point of polymer, more than glass transition temperature, to ensure that fiber had both had certain deformability in drawing-off, need can keep certain tensile strength again.
But as complete unbodied polyether sulfone, only have glass transition temperature and there is no fusing point, once namely the tensile strength exceeding its glass transition temperature fiber can sharply decline, thus making fibrous fracture, cannot drawing-off smoothly.Therefore, the melt spinning of usual polyether sulfone fiber needs, by balance, can not a step to complete.Investigated by theory analysis and practice, the temperature of two of drafting forming up-coiler drawing-off hot-rollings is all arranged between the glass transition temperature of polyether sulfone and secondary transition temperature by the present inventor, and have 10 ~ 40 DEG C between two rollers, the preferably temperature increment of 15 ~ 25 DEG C, the temperature of upper hot-rolling is lower than lower heat roller temperature.The temperature of upper hot-rolling is 90 ~ 130 DEG C, preferably 100 ~ 115 DEG C, and the temperature of lower hot-rolling is 110 ~ 150 DEG C, preferably 120 ~ 140 DEG C.Velocity ratio (i.e. drafting multiple) between drafting forming up-coiler two roller 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 is controlled by a friction roller, and the speed of friction roller is close to lower roll, and slightly fast or slightly slow in 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 completely.
The present invention selects single screw extrusion machine to be because single screw extrusion machine is conventional spinning equipment, compared with double screw extruder low price, easy and simple to handle; Selecting FDY one-step method to be because FDY one-step method saves time more, is also the important method in usual resins spinning.Therefore, the preparation method of polyether sulfone fiber provided by the invention, simplifies the preparation technology of current polyether sulfone fiber, shortens 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.
Detailed description of the invention
The present invention is further described below in conjunction with embodiment.Scope of the present invention is not by the restriction of these embodiments, and scope of the present invention proposes in detail in the claims.
Embodiment 1
By polyether sulfone section through vacuumize extremely moisture < 200ppm, single screw extrusion machine is adopted to melt extrude.Each district temperature of screw rod is: feed zone 305 DEG C, 317 DEG C, compression section, melt zone 322 DEG C, metering section 332 DEG C.By (spinning temperature is 345 DEG C) after filament spinning component wire vent, through spinning shaft cooling curing under lateral blowing condition, drafting forming up-coiler directly introduced by silk after oiling, carry out drafting forming at upper and lower hot-rolling, wherein going up heat roller temperature is 96 DEG C, speed 445m/min, lower heat roller temperature is 135 DEG C, speed 848m/min, drafting multiple is 1.9 times, the coiling speed 830m/min of up-coiler.
The polyether sulfone fiber finally obtained, filament number 7.2dtex, fracture strength 2.2CN/dtex, extension at break 17%.
Embodiment 2
By polyether sulfone section through vacuumize extremely moisture < 200ppm, single screw extrusion machine is adopted to melt extrude.Each district temperature of screw rod is: feed zone 320 DEG C, 330 DEG C, compression section, melt zone 332 DEG C, metering section 343 DEG C.By (spinning temperature is 345 DEG C) after filament spinning component wire vent, through spinning shaft cooling curing under lateral blowing condition, drafting forming up-coiler directly introduced by silk after oiling, carry out drafting forming at upper and lower hot-rolling, wherein going up heat roller temperature is 110 DEG C, speed 556m/min, lower heat roller temperature is 128 DEG C, speed 1334m/min, drafting multiple is 2.4 times, the coiling speed 1300m/min of up-coiler.
The polyether sulfone fiber finally obtained, filament number 6.5dtex, fracture strength 3.0CN/dtex, extension at break 11%.
Embodiment 3
By polyether sulfone section through vacuumize extremely moisture < 200ppm, single screw extrusion machine is adopted to melt extrude.Each district temperature of screw rod is: feed zone 335 DEG C, 360 DEG C, compression section, melt zone 370 DEG C, metering section 380 DEG C.By (spinning temperature is 345 DEG C) after filament spinning component wire vent, through spinning shaft cooling curing under lateral blowing condition, drafting forming up-coiler directly introduced by silk after oiling, carry out drafting forming at upper and lower hot-rolling, wherein going up heat roller temperature is 125 DEG C, speed 1055m/min, lower heat roller temperature is 147 DEG C, speed 1947m/min, drafting multiple is 1.8 times, the coiling speed 1900m/min of up-coiler.
The polyether sulfone fiber finally obtained, filament number 12.0dtex, fracture strength 1.6CN/dtex, extension at break 7%.
Comparative example 1
By polyether sulfone section through vacuumize extremely moisture < 200ppm, single screw extrusion machine is adopted to melt extrude.Each district temperature of screw rod is: feed zone 350 DEG C, 385 DEG C, compression section, melt zone 390 DEG C, metering section 395 DEG C.Because extruder temperature is too high, the melt color and luster being extruded (spinning temperature is 345 DEG C) by filament spinning component sends out crow, has the sign of degraded, and under lateral blowing condition after spinning shaft, tow wafts silk, fracture of wire seriously, cannot introduce drafting forming up-coiler.
Comparative example 2
By polyether sulfone section through vacuumize extremely moisture < 200ppm, single screw extrusion machine is adopted to melt extrude.Each district temperature of screw rod is: feed zone 295 DEG C, 300 DEG C, compression section, melt zone 305 DEG C, metering section 318 DEG C.Because extruder temperature is too low, extruded (spinning temperature is 345 DEG C) by filament spinning component, melt pressure increases rapidly, and through spinning shaft cooling curing under lateral blowing condition, after oiling, column cap silk is more, cannot introduce drafting forming up-coiler.
Comparative example 3
By polyether sulfone section through vacuumize extremely moisture < 200ppm, single screw extrusion machine is adopted to melt extrude.Each district temperature of screw rod is: feed zone 320 DEG C, 330 DEG C, compression section, melt zone 332 DEG C, metering section 338 DEG C.After filament spinning component wire vent, through spinning shaft cooling curing under lateral blowing condition, drafting forming up-coiler directly introduced by the silk after oiling, drafting forming is carried out at upper and lower hot-rolling, wherein going up heat roller temperature is 145 DEG C, speed 500m/min, and lower heat roller temperature is 153 DEG C.Because up-down rollers temperature is too high, the temperature difference is too small, no matter descends hot-rolling speed how to arrange and always fracture of wire occurs, cannot reel, can not get finished fiber.
Comparative example 4
By polyether sulfone section through vacuumize extremely moisture < 200ppm, single screw extrusion machine is adopted to melt extrude.Each district temperature of screw rod is: feed zone 320 DEG C, 330 DEG C, compression section, melt zone 332 DEG C, metering section 338 DEG C.After filament spinning component wire vent, through spinning shaft cooling curing under lateral blowing condition, drafting forming up-coiler directly introduced by silk after oiling, carries out drafting forming at upper and lower hot-rolling, and wherein going up heat roller temperature is 85 DEG C, speed 300m/min, lower heat roller temperature is 135 DEG C, and because upper roll temperature is too low, no matter excessive temperature differentials descends hot-rolling speed how to arrange always fracture of wire occurs, cannot reel, can not get finished fiber.
Comparative example 5
By polyether sulfone section through vacuumize extremely moisture < 200ppm, single screw extrusion machine is adopted to melt extrude.Each district temperature of screw rod is: feed zone 320 DEG C, 330 DEG C, compression section, melt zone 332 DEG C, metering section 338 DEG C.After filament spinning component wire vent, through spinning shaft cooling curing under lateral blowing condition, drafting forming up-coiler directly introduced by the silk after oiling, and carries out drafting forming at upper and lower hot-rolling, wherein going up heat roller temperature is 115 DEG C, speed 800m/min, lower heat roller temperature is 135 DEG C, and Speed Setting is 2100m/min, because spinning speed is too fast, the excessive tow of speed ratio produces more lousiness between upper and lower hot-rolling, cannot reel, can not get finished fiber.
Claims (5)
1. a preparation method for polyether sulfone fiber, comprises the following steps:
(1) dry polyethersulfone resin;
(2) above polyethersulfone resin single screw extrusion machine is melt extruded, and be squeezed into filament spinning component, then through filament spinning component melt spinning;
Described singe screw is divided into feed zone, compression section, melt zone, metering section, wherein feed zone temperature 300 ~ 340 DEG C; Compression section and melt zone temperature 310-380 DEG C; Metering section temperature 320-390 DEG C;
(3) silk spun in above-mentioned filament spinning component is directly introduced drafting forming up-coiler incessantly, undertaken adding hot gas spring by hot-rolling, then batch and obtain polyether sulfone fiber finished product;
Temperature wherein between drafting forming up-coiler two drawing-off hot-rollings has 10 ~ 40 DEG C increasing progressively; The temperature of upper hot-rolling is lower than lower heat roller temperature; Upper heat roller temperature is 90 ~ 130 DEG C, and the temperature of lower hot-rolling is 110 ~ 150 DEG C; Velocity ratio between described step (3) two roller is greater than 1.8, and is less than or equal to 2.5.
2. the preparation method of polyether sulfone fiber according to claim 1, is characterized in that:
Described in described step (2), singe screw is divided into feed zone, compression section, melt zone, metering section, wherein feed zone temperature 305 ~ 325 DEG C; Compression section and melt zone temperature 320-350 DEG C; Metering section temperature 330-360 DEG C.
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 DEG C increasing progressively; The temperature of upper hot-rolling 100 ~ 115 DEG C, the temperature of lower hot-rolling is 120 ~ 140 DEG C.
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 the polyether sulfone fiber according to any one of claims 1 to 3, is characterized in that:
In described step (3), coiling speed is 800 ~ 2000m/min.
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| 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 |
| JP6813393B2 (en) * | 2017-03-03 | 2021-01-13 | 住友化学株式会社 | Non-woven fabric manufacturing method |
| 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 |
| 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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Effective date of registration: 20220523 Address after: A2 Beikou, Heping Street, Chaoyang District, Beijing 100029 Patentee after: BEIJING INSTITUTE OF FASHION TECHNOLOGY Patentee after: Kaitai special fiber technology Co., Ltd Address before: Room 102, complex building, No. 22, Zhonghe street, Beijing Economic and Technological Development Zone, Daxing District, Beijing 100176 Patentee before: CTA YOUTH HIGH-TECH FIBER Co.,Ltd. Patentee before: BEIJING INSTITUTE OF FASHION TECHNOLOGY Patentee before: CTA HIGH-TECH FIBER Co.,Ltd. |