EP0119521B1 - Procédé en continu pour la fabrication de fibres et fils en polyacrylonitrile - Google Patents

Procédé en continu pour la fabrication de fibres et fils en polyacrylonitrile Download PDF

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Publication number
EP0119521B1
EP0119521B1 EP84102121A EP84102121A EP0119521B1 EP 0119521 B1 EP0119521 B1 EP 0119521B1 EP 84102121 A EP84102121 A EP 84102121A EP 84102121 A EP84102121 A EP 84102121A EP 0119521 B1 EP0119521 B1 EP 0119521B1
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EP
European Patent Office
Prior art keywords
tow
spinning
crimping
washing
sliver
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Expired
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EP84102121A
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German (de)
English (en)
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EP0119521A3 (en
EP0119521A2 (fr
EP0119521B2 (fr
Inventor
Michael Dr. Bueb
Dieter Dipl.-Ing. Paulini
Edgar Dr. Muschelknautz
Wolfram Dr. Wagner
Herbert Dr. Gröschel
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Bayer AG
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Bayer AG
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Publication of EP0119521A2 publication Critical patent/EP0119521A2/fr
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/18—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of unsaturated nitriles, e.g. polyacrylonitrile, polyvinylidene cyanide
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
    • D02G1/12—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics using stuffer boxes
    • D02G1/122—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics using stuffer boxes introducing the filaments in the stuffer box by means of a fluid jet

Definitions

  • the invention relates to a continuous process for the production of polyacrylonitrile threads and fibers, in which the spun material is produced by the dry spinning method.
  • Polyacrylonitrile threads are produced by the polymer in a suitable solvent, for. B. dimethylformamide dissolves and presses the spinnable solution through a spinneret. If the threads are solidified in a mostly aqueous liquid ("precipitant") by coagulation, this is referred to as the wet spinning process. If the threads are solidified by evaporation of the solvent in a hot air spinning shaft, this is referred to as the dry spinning process.
  • Post-treatment means the typical process steps of washing (solvent extraction), stretching, crimping, preparation, steaming, drying and cutting.
  • the spinning belt is placed in a spinning can after leaving the spinning machine and fed from many such spinning cans to an aftertreatment line.
  • Such an interruption between the spinning and post-treatment process has major disadvantages, for example high manufacturing costs, larger amounts of waste, emissions of solvents from the spinning cans, fluctuations in product quality.
  • a process for continuous wet treatment in particular washing thread coulters at speeds up to 150 m / min, has become known from DE-A-1 760 004, with washing liquor being briefly passed through the thread coulters transversely to the running direction of the thread coulters at the beginning of the wet treatment and then being removed
  • the washable substances in the fibers remain in a treatment liquid for a longer period of time. Between the individual liquid treatments is dewatered by squeezing.
  • the thread coulters are transported on rollers.
  • the devices required for this process are complex and do not allow speeds of over 150 m / min.
  • the object of the present invention was therefore to provide a continuous process for the production of polyacrylonitrile threads and fibers, in which the spun material is produced by the dry spinning method and is fed to the aftertreatment without interruption. It was a prerequisite that the spinning take-off speed at the spinning shaft at about 150 m / min, and a certain sliver weight in the aftertreatment stage of about 10 g / m were not undercut so as not to question the economics of the process.
  • the cut fibers can be conveyed continuously from the cutting device in a pneumatic conveying line to the baling press and pressed therein into completely packed fiber bales.
  • the washing process is preferably carried out in such a way that washing liquid is sprayed onto the folded spinning belt in each step, which for the most part seeps through the spinning belt and through the belt transport device within the step and is then collected below the transport device in a template and repeated several times under showering is attributed to the tape at the same level.
  • a suitable washing machine is described in DE-A-2 950 014.
  • the stretching can be carried out in one or more stages with a total stretching ratio of 1: 2 to 1: 5.
  • the stretching is preferably carried out in tubes charged with steam.
  • the preparation is preferably carried out in the crimping nozzle, the aerodynamic crimping device preferably being an injector operated with superheated steam or hot air.
  • the ruffling nozzle is preferably designed as an annular gap injector nozzle comprising an inlet part, a mixing section, a diffuser and a rod cage.
  • the vibrating trough, on which the crimp is then fixed and the shrinkage is removed, is preferably combined with the crimping nozzle to form a device part such that the crimping vapor escaping from the rod cage of the crimping nozzle can be used for damping in the damping step.
  • the dryer is preferably divided into several chambers, which can be brought to different temperatures, mostly decreasing temperatures in the direction of the thread.
  • the last chamber is fed with room temperature air as a cooling zone.
  • the vibrating troughs are preferably operated with an unbalance drive or electromagnetic excitation.
  • the vibrating trough of the washing stage preferably has bottoms made of perforated sheets, sieve fabrics or slotted sheets with 10 to 50% free cross-sectional area.
  • Fig. 1 is a schematic representation of the overall process and a possibility of its apparatus configuration
  • Fig. 2 is a schematic representation of the preferred curling nozzle.
  • fiber tapes are produced in the spinning shafts of a dry spinning machine (1) using the dry spinning process.
  • solvent e.g. dimethylformamide
  • the slivers are combined into a spinning belt (2) with a belt weight of 10-100 g / m and drawn off from the take-off unit (3) at a spinning speed of 150-400 m / min. After dry spinning, the fibers still contain approx. 5 - 20% solvent (e.g. dimethylformamide).
  • solvent e.g. dimethylformamide
  • the solvent extraction is carried out in a washing machine (6), in which the folded spinning belt is washed in a countercurrent process in 10-30 stages with hot water at 60-95 ° C.
  • Coupling the continuous aftertreatment system to a running spinning machine can be difficult because it has to be done very quickly and requires special technology.
  • the spinning belt is first drawn off via the take-off unit (3) and placed in a loss spinning can.
  • the spinning belt is suddenly conveyed pneumatically with the aid of a compressed air-operated injector through an feed pipe (4) to the delivery unit (5) of the washing machine (6) and inserted into the delivery unit.
  • the spinning belt is then placed in a changeable depositing device in the form of a tube in a serpentine shape on the transport surface of the washing machine.
  • An annular nozzle operated with washing water sits in the depositing device in order to apply water to the fiber sliver, to safely pull the fiber sliver away from the delivery mechanism (5) and to achieve a compact, compressed shape of the fiber sliver on the transport surface of the washing apparatus.
  • the folded spinning belt is transported on a perforated plate with lateral boundary walls at 1 - 4 m / min, the perforated plate being part of a vibrating trough trough.
  • the ratio of the delivery speed of the sliver into the washing machine to the conveying speed of the sliver cake in the washing machine results in a folding factor of approx. 50 - 150.
  • the spraying of the sliver cake within each stage must be carried out so gently that any floating of the fibers and any formation of tangles and Matting is avoided. This is made possible by shower boxes placed as close as possible above the sliver cake, from the bores of which the water flows only under the action of gravity and hits the sliver cake at a speed of less than 1 m / s.
  • the necessary fresh water consumption is 0.7 - 2 kg water per 1 kg fiber.
  • the residence time of the sliver in the washing machine is 2 - 6 min. Before leaving the washing machine, the sliver is pulled smooth again and then mechanically dewatered (7) to a water content of 30 - 50%.
  • the solvent content in the sliver after leaving the scrubber is approx. 1 - 2%.
  • the speed of entry into the drawing must be controlled so that the dissolving point of the sliver cake in the washing machine is always at the same point.
  • the measurement of the resolution point can be done with the help of light barriers or an inductive measuring probe.
  • the sliver is drawn in hot steam in two stages or stretching fields. Between the drive rollers (8) and (9) wrapped in the sliver, the sliver is stretched in the first stage in a ratio of 1: 1.1 to 1: 2 and at the same time heated by passing it through a 1 - 3 m long steam pipe or a steam duct (11) is guided, in which water vapor from 100 - 130 ° C is fed.
  • the main drawing takes place between the drive rollers (9) and (10) in a ratio of 1: 2 to 1: 6 in a 3 to 7 m long steam pipe or steam duct (12), into which steam of 100 to 130 ° C is fed.
  • the outlet speed on the drive rollers (10) is between 500 and 2000 m / min, depending on the spinning speed and the stretch ratio set.
  • low-solvent polyacrylic fiber tape can be stretched at high speeds if the stretching in the manner according to the invention is carried out in two stages in water vapor of at least 100 ° C.
  • stretching is carried out in a steam pipe, in which an excess pressure of 0.1-2 bar is generated with the aid of pressure locks at the inlet and outlet, so that stretching can take place at saturated steam temperatures of up to 130.degree.
  • the threading of the fiber sliver into the steam pipe is carried out pneumatically with the aid of integrated injectors. The drawn sliver is then crimped at the same speed in a steam nozzle crimper (13).
  • Such an aerodynamic crimping device basically consists of an injector operated with superheated steam or hot air (5 - 16 bar and 50 - 210 ° C), through the effect of which the fiber sliver is continuously sucked into the nozzle and the fiber sliver is compressed or crimped in the nozzle becomes.
  • the sliver speed is reduced by a factor of 10-20, so that the compressed and crimped sliver leaves the crimping device at a speed of 50-200 m / min.
  • an aerodynamic crimping nozzle Compared to a mechanical compression crimping machine, an aerodynamic crimping nozzle produces a compression force that is 3 to 9 times smaller. It has surprisingly been found, however, that even a small compression force is completely sufficient to achieve a sufficiently intense crimp if the sliver is crimped in the presence of water vapor at 150-200 ° C.
  • the band cross-sectional area can be according to the relationship are determined, where M is the tape mass in [kg], L the tape length in [m] and p the density of the fibers in jkg / m 3 j. An essentially three-dimensional crimp is obtained.
  • slivers have to be wetted with a preparation in order to achieve the desired static and sliding friction properties of the fibers and to avoid electrostatic charges.
  • a in the method according to the invention such preparation can be applied continuously to the sliver. It has surprisingly been found that the continuous metering of an aqueous preparation can take place directly in the curling nozzle (13) because the preparation is distributed evenly over all fibers by the effect of the steam flow.
  • the preparation is an approximately 5 to 20% by weight oil-in-water emulsion which is applied in an amount of 0.2 to 0.6% by weight oil, based on fiber solids.
  • suitable oils are known to the person skilled in the art.
  • the crimped and folded sliver cake is then transported on a vibrating trough without tension under the action of water vapor at 100-120 ° C. with a dwell time of 0.1 to 2 minutes through a steaming device (14).
  • the fiber sliver After washing, stretching, crimping, preparing and steaming, the fiber sliver still has a water content of 30 - 60%. This water must be removed by a thermal drying process.
  • the crimped sliver is placed evenly on a belt dryer (15) with the aid of a traversing device and moves through the dryer on the transport base at speeds of 0.1-3 m / min and dwell times of 2-10 min. Drying takes place with the help of warm air at 60 - 180 ° C depending on the desired drying conditions.
  • the sliver Before cutting, the sliver must be cooled to temperatures below 50 ° C so that the crimp is not lost due to the cutting stress. Part of the dryer is therefore designed as a cooling zone (16). There the sliver is exposed to cold air. Before leaving the dryer, the sliver cake is dissolved again by quickly pulling the sliver off at a speed of 500
  • the sliver is then cut into staple fibers of 30 to 150 mm in a cutter (17).
  • the fiber flakes are conveyed in a pneumatic conveying line (18) to the baling press (19) and pressed therein into completely packed fiber bales (20).
  • the speed of the cutting machine (17) must be controlled so that the sliver cake always dissolves in the same place at the end of the dryer.
  • the ruffling nozzle (13) shown in Fig. 2 consists of an inlet part (21), the mixing section (25), the diffuser (26) and the rod cage (27).
  • the spinning belt (28) is sucked in through the mouthpiece (30).
  • a hot gas (29) is fed through the feed line (22) and the annular gap (23), heats and conveys the spinning belt.
  • the two bores (24) are used to feed the preparation.
  • the inlet part of the nozzle is preferably 50 to 100 mm long and has a diameter of 8 to 15 mm.
  • the gap width of the annular gap is in particular 0.2 to 0.6 mm.
  • the inflowing hot gas reaches speeds of 450 to 500 m / sec. at a temperature of 100 to 150 ° C.
  • the angle between entering hot gas and sliver is less than 20 °.
  • the subsequent mixing section has a length of 100 to 200 mm with a diameter of 9 to 16 mm.
  • the sliver is from the gas speed of 150 to 200 m / sec. transported through the nozzle.
  • the sliver opens in the diffuser, which is then braked and crimped in the rod cage.
  • the rod cage has a diameter of 20 to 30 mm and a length of 100 to 200 mm and consists of about 20 to 50 concentrically arranged steel rods of 0.5 to 2 mm thickness, which can be of the same or different lengths.
  • the hot gas escapes laterally through the rods.
  • Polyacrylonitrile with the composition 93.6% by weight of acrylonitrile, 5.7% by weight of methyl acrylate and 0.7% by weight of methallylsulfonate and a K value of 81 was obtained as a 30% by weight solution in dimethylformamide (DMF ) spun using the dry spinning process.
  • the take-off speed at the spinning shaft was 240 m / min.
  • the single fiber titer was 10 dtex and the total undrawn sliver weight of the spinning sliver was 20 g / m. After leaving the spinning machine, the threads still had a DMF content of 17% by weight.
  • the spinning belt was washed in the folded state in a washing machine with 20 washing stages, which has a vibrating trough as a transport base.
  • the dwell time of the spinning belt in the laundry was about 3 minutes
  • the washing water temperature was about 90 ° C.
  • the amount of fresh water used was 1 kg of water / kg of threads.
  • the spinning belt left the washing machine with a DMF content of 1% and a speed of 200 m / min.
  • the spinning belt was drawn in two stages in steam pipes with saturated steam at 100 ° C.
  • the stretch ratio of the first stage was 1: 1.3
  • the stretch ratio of the second stage was 1: 2.85 and the outlet speed was approx. 1000 m / min.
  • the sliver was crimped with a steam nozzle with 9 bar saturated steam.
  • the crimping nozzle corresponded to FIG. 2, the inlet mouthpiece having a diameter of 9 mm, the mixing section a diameter of 12.5 mm and the annular gap having a clear width of 0.39 mm with a total area of the annular gap of 15.2 mm 2 .
  • a 10% by weight oil-in-water was The emulsion was added as a preparation in such an amount that 0.45% by weight of oil, based on fiber solids, was applied.
  • the total length of the crimping nozzle was 500 mm.
  • the rod cage consisted of 30 rods with a diameter of 1 mm.
  • the steam temperature was 121 ° C, the steam speed 480 m / sec.
  • the crimp cake was steamed in a steamer with the steam emerging from the rod cage of the crimping nozzle.
  • the residence time was 15 seconds in a steam atmosphere of approx. 100 ° C.
  • the sliver still had approx. 40% water and a cooking shrinkage of 2%.
  • the crimped and folded sliver was placed on a belt dryer with 4 drying chambers, which at a speed of 0.8 m / min. ran.
  • the air temperature was 150 ° C in the first three drying chambers and 20 ° C in the fourth chamber.
  • the residence time in the dryer was 3 minutes. After leaving the dryer, the sliver had only a water content of 1% and a temperature of 30 ° C.
  • the sliver was drawn off at 620 m / min, cut into staple fibers of 60 mm in length on a rotor blade, and then made into bales in the baler packed up.
  • the polyacrylonitrile staple fibers produced in this way could be processed on the card at a card speed of 120 m / min.
  • the individual fibers had a titer of 3.3 dtex, a tensile strength of 24 cN / tex, an elongation at break of 30%, a residual solvent content of 0.1% and no vacuoles.
  • the crimp was 11.2% and the crimp resistance was 74.6%.
  • the crimped thread is hung at one end and loaded with a weight of 0.001 cN / dtex. Its length is 1 0 .
  • the load is increased to 0.1 cN / dtex. Its length is now 1 1 .
  • the load is reduced again to 0.001 cN / dtex. Its length is now 1 2 .

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Artificial Filaments (AREA)

Claims (6)

1. Procédé de production de fils et de fibres de polyacrylonitrile par filage de la solution de filature dans une cuve de filage à air chaud, lavage, étirage, frisage, préparation, vaporisage, séchage, refroidissement et, le cas échéant, découpage, caractérisé en ce que le ruban filé à sec est enlevé à une vitesse de 150 à 400 m/min et engagé sans interruption du déroulement du procédé dans les autres étapes de post-traitement avec un poids de ruban de 10 a 100 g/m, en sorte que
a) le processus de lavage est effectué en plusieurs étapes selon le principe à contrecourant et une gouttière vibrante est utilisée comme dispositif de transport pour le ruban de filature dans le processus de lavage,
b) l'étirage est effectué avant et/ou après le processus de lavage dans une atmosphère de vapeur à 100 - 120° C,
c) le frisage est effectué dans un dispositif aérodynamique de frisage avec un milieu gazeux chaud sous pression de 5 à 16 bars et à une température de 50 a 210°C,
d) la préparation est appliquée sur le ruban de fibres en continu avant, pendant ou après le frisage,
e) le ruban de fibres est transporté en vue du vaporisage sous la forme pliée sans subir de tension sur une gouttière vibrante en traversant un appareil de vaporisage où il est traité avec de la vapeur d'eau à 100 - 120° C,
f) le ruban de fibres est enfin séché à l'état plié sur un appareil de séchage à l'aide d'air chaud à 60 - 180: C, puis refroidi à l'air froid à des températures inférieures à 50°C et, le cas échéant, amené è un dispositif de découpage.
2. Procédé suivant la revendication 1, caractérisé en ce que l'opération de lavage est effectuée en 10 à 30 étapes avec 0,7 à 2 kg d'eau chaude à 60 - 95°C par kg de fibres de façon telle que, dans chaque étape, on fait tomber en pluie sur le ruban de filature plissé du liquide de lavage qui est absorbé en majeure partie au cours de l'étape par le ruban de filature et par le dispositif de transport du ruban et qui est ensuite recueilli au-dessous du dispositif de transport dans un collecteur et recyclé de nombreuses fois dans la même étape avec arrosage en pluie du ruban et la durée de séjour du ruban de fibres dans l'appareil de lavage est de 2 à 6 minutes.
3. Procédé suivant la revendication 1, caractérisé en ce que l'étirage est effectué en une ou plusieurs étapes avec des rapports totaux d'étirage de 1 : 2 à 1 : 5.
4. Procédé suivant la revendication 1, caractérisé en ce que la préparation est appliquée sur le ruban de fibres dans la filière de frisage.
5. Procédé suivant la revendication 1, caractérisé en ce que le frisage est effectué à la vapeur d'eau et la vapeur qui s'échappe du dispositif de frisage est utilisée pour l'étape de vaporisage e).
6. Procédé suivant les revendications 1 et 5, caractérisé en ce que le quotient de l'aire de section transversale de la filière par l'aire de section transversale du ruban de fibres se situe entre 5 et 50.
EP84102121A 1983-03-11 1984-02-29 Procédé en continu pour la fabrication de fibres et fils en polyacrylonitrile Expired - Lifetime EP0119521B2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3308657A DE3308657A1 (de) 1983-03-11 1983-03-11 Kontinuierliches verfahren zur herstellung von polyacrylnitrilfaeden und -fasern
DE3308657 1983-03-11

Publications (4)

Publication Number Publication Date
EP0119521A2 EP0119521A2 (fr) 1984-09-26
EP0119521A3 EP0119521A3 (en) 1987-06-10
EP0119521B1 true EP0119521B1 (fr) 1989-01-25
EP0119521B2 EP0119521B2 (fr) 1992-10-14

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ID=6193160

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Application Number Title Priority Date Filing Date
EP84102121A Expired - Lifetime EP0119521B2 (fr) 1983-03-11 1984-02-29 Procédé en continu pour la fabrication de fibres et fils en polyacrylonitrile

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US (1) US4622195A (fr)
EP (1) EP0119521B2 (fr)
JP (1) JPS59168117A (fr)
DE (2) DE3308657A1 (fr)

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KR102400546B1 (ko) * 2017-01-26 2022-05-19 코오롱인더스트리 주식회사 고강도 폴리에스테르 원사의 제조 방법 및 그 제조 장치
CN112853516B (zh) * 2021-01-08 2021-12-17 温州国宏新材料科技有限公司 一种塑料编织袋制作成型方法
CN113969429A (zh) * 2021-12-02 2022-01-25 山东越神新材料科技有限公司 一种用干法腈纶工艺制备高性能大丝束碳纤维原丝的方法

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US3932571A (en) * 1972-11-30 1976-01-13 E. I. Du Pont De Nemours And Company Process for dyeing undrawn acrylonitrile polymer filaments
DE3225268A1 (de) * 1982-07-06 1984-01-12 Bayer Ag, 5090 Leverkusen Kontinuierliches trockenspinnverfahren fuer hochschrumpffaehige acrylnitrilfaeden und -fasern
DE3225266A1 (de) * 1982-07-06 1984-01-12 Bayer Ag, 5090 Leverkusen Kontinuierliches trockenspinnverfahren fuer acrylnitrilfaeden und - fasern

Also Published As

Publication number Publication date
JPS59168117A (ja) 1984-09-21
EP0119521A3 (en) 1987-06-10
EP0119521A2 (fr) 1984-09-26
DE3308657A1 (de) 1984-09-20
JPS6256242B2 (fr) 1987-11-25
EP0119521B2 (fr) 1992-10-14
DE3476429D1 (en) 1989-03-02
US4622195A (en) 1986-11-11

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