EP1608803B1 - Procede et dispositif pour produire des fils de cellulose post-etires - Google Patents

Procede et dispositif pour produire des fils de cellulose post-etires Download PDF

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Publication number
EP1608803B1
EP1608803B1 EP04710007A EP04710007A EP1608803B1 EP 1608803 B1 EP1608803 B1 EP 1608803B1 EP 04710007 A EP04710007 A EP 04710007A EP 04710007 A EP04710007 A EP 04710007A EP 1608803 B1 EP1608803 B1 EP 1608803B1
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EP
European Patent Office
Prior art keywords
spun threads
stretching
post
stretched
following step
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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EP04710007A
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German (de)
English (en)
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EP1608803A1 (fr
Inventor
Stefan Zikeli
Klaus Weidinger
Lutz Glaser
Werner Schumann
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LL Plant Engineering AG
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ZiAG Plant Engineering GmbH
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Classifications

    • 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
    • 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
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • 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
    • 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
    • D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/38—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising unsaturated nitriles as the major constituent
    • 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
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
    • D02J1/22—Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J13/00—Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber

Definitions

  • the invention relates to a method for the production of lyocell threads from a spinning solution containing water, cellulose and tertiary amine oxide and the spun threads produced by this method.
  • the invention relates to an apparatus for producing filaments of a spinning solution containing cellulose, water and tertiary amine oxide, with a spinneret through which the spinning solution is extrudable into filaments during operation, with a precipitating bath with a precipitant precipitating a cellulose, through which the filaments in the Operation with a first drawing means, by means of which the filaments are stretchable in operation, with a second drawing means, through which the stretched filaments drawn by the first drawing means are nachverstreckbar during operation, and with a arranged in the region of the second drawing means heating device by the Operation the spun yarns are heatable during Nachverstreckung.
  • the spinning solution is first extruded into filaments, then the filaments are drawn and passed through a precipitation bath, after which the cellulose of the filaments coagulates.
  • fibers and “filaments” are used synonymously
  • a tertiary amine oxide such as N-methyl-morpholine-N-oxide and water
  • lyocell process refers to the patents US-A-4 142 913 .
  • the filaments can be fed to further processing steps.
  • the filaments can be washed, dried and treated with additives or impregnated.
  • the filaments can be cut.
  • the advantage of the Lyocell process lies in the good environmental compatibility and in the excellent mechanical properties of the spun threads or fibers.
  • Various advances in the process developed by McCorsley have greatly improved profitability.
  • the lyocell fiber differs in terms of their structure and their textile properties of the other cellulose fibers and their production, as for example in the DE-A-100 16 307 .
  • WO-A-01/58960 DE-A-197 53 806 .
  • DE-A-197 21 609 DE-A-195 11 151 and DE-A-43 12 219 are described.
  • a particular problem of the Lyocell process compared to the processes described therein lies in the high surface tack of the freshly extruded filaments: As soon as the filaments touch the air gap, they stick together, resulting in either unsatisfactory fiber quality or even disruption of the spinning process and re-spinning leads. McCorsley himself uses this, as in the DE-A-284 41 63 described, the filaments in the air gap on a roller with Kayllbad clips. However, this arrangement is impractical at high spinning speeds. A series of further developments of the McCorsley process therefore deals with measures to reduce the surface tackiness of the spun yarns in the air gap and to improve the operational reliability, also called spin security, of the production process.
  • Lyocell fibers differ significantly from the fibers, as in the DE-A-197 53 806 .
  • DE-A-100 16 307 and the DE-A-43 12 219 are described.
  • JP-A-03-076822 a process for producing fire-resistant fibers is described. After coagulation of the undrawn fibers, the filaments are drawn for a first time, then oiled and dried, then re-stretched under steam and then dried again.
  • the invention is therefore based on the object to improve the known methods and apparatus for producing lyocell fibers in that the mechanical properties, such as the loop strength and the tensile strength of the lyocell fibers can be selectively influenced by an easy-to-control process.
  • this object is achieved in that the filaments are stretched by the first drawing means in an air gap before entering the precipitation bath.
  • the post-stretching or stretching of the filaments which have already been drawn once in the air gap and then coagulated, can considerably improve the mechanical properties, in particular the wet modulus, compared with the conventional lyocell fibers. Due to the heat treatment during the post-drawing, the wet module is lowered a little after the first attempts and the fiber becomes somewhat more elastic again.
  • lyocell fibers having a wet modulus of at least 250 cN / tex and a wet rubbing rate per 25 fibers of at least 18 can be obtained by the process of the present invention.
  • Even wet modules of at least 300 cN / tex or 350 cN / tex can be achieved with the process according to the invention.
  • the wet maximum tensile force extension can assume relatively low values, for example at most 12%.
  • the predetermined tensile stress with which the spun threads are stretched or stretched the higher the wet modulus of the finished threads and fibers seems to be.
  • a considerable increase of the wet modulus compared to conventional fibers can be achieved according to an advantageous process control if the predetermined tensile stress with which the post-stretching is carried out amounts to at least 0.8 cN / tex.
  • Higher values for the wet modulus can be achieved if, according to a further embodiment, the predetermined tensile stress during the post-drawing is at least 3.5 cN / tex.
  • the heat treatment can be carried out subsequent to a washing or impregnation process as a drying process, so-called tension drying.
  • the heat treatment may also take place in a steam or dry steam atmosphere.
  • the steam or dry steam may contain impregnating agents which act on the filaments and lead to a chemical aftertreatment.
  • the heat treatment is preferably carried out in an oven in which the drawn and coagulated filaments are post-stretched between two godets with a predetermined tensile stress.
  • a hot inert gas such as hot air, or steam or dry steam may be passed through the surfaces of the godets and the filaments lying thereon.
  • the spun threads can be crimped, since the natural crimp of the spun threads is substantially reduced due to the post-stretching. At the same time a treatment with dry steam is possible simultaneously with the crimping.
  • the filaments can finally be cut.
  • a plant 1 for the production of lyocell fibers on the basis of the schematic representation of Fig. 1 described.
  • the plant 1 of Fig. 1 is used to produce staple fibers from Lyocell.
  • a high-viscosity spinning solution containing water, cellulose and tertiary amine oxide, for example N-methyl-morpholine-N-oxide passed.
  • the line system 2 is modularly constructed from fluid line pieces 2a of predetermined length, which are connected to each other via standard flanges 2b.
  • the fluid line pieces 2a are provided with an internal temperature control device 3, which is mounted in the fluid line pieces 2 instead of the core flow of the spinning solution and is regulated by the temperature of the spinning solution in the pipeline system 2.
  • a temperature-controlled fluid is passed through the inner temperature control device via feed modules 4 arranged between two adjacent fluid line sections, as indicated by the arrows 5.
  • the feed modules 4 essentially have the dimension of the standard flanges and are designed to be connectable with these.
  • the feed modules 4 At predetermined intervals, also replace by the arranged between the fluid line sections 2a Berstmodule 6, the feed modules 4.
  • the bursting modules 6 have essentially the same configuration as the feed modules 4. You are in the Fig. 1 Not shown Berstkörpem provided that break when exceeding a predetermined pressure in the piping system 2, in case of bursting, and allow a pressure discharge to the outside.
  • the bursting event may be especially at a spontaneous exothermic Reaction of the spinning solution due to overaging or overheating occur.
  • the spinning solution which escapes in the event of a burst is collected in collecting containers 7, from where it can be recycled or disposed of.
  • the spinning solution is fed to a spinner 8.
  • the spinner head 8 is provided with a spinneret 9 having a large number of extrusion orifices (not shown), usually several thousand extrusion orifices. Through the extrusion openings, the spinning solution is extruded into filaments 10.
  • the arrangement of the extrusion openings in the spinneret 9 may be circular, circular or rectangular; In the following, reference will be made, by way of example only, to a rectangular arrangement.
  • baffles can be provided, which can also be connected via the standard flanges, simply with the fluid line pieces 2a or with the feed modules 4 or bursting modules 6.
  • a surge tank 11 a may be arranged, which compensates for pressure fluctuations and volume flow fluctuations of the spinning solution in the pipe 2 via a change in its internal volume and ensures a uniform extrusion pressure at the extrusion openings of the spinner head 8.
  • a mechanical filter device 11b with a backwashable filter element may be provided in the pipeline system 2.
  • the filter element has a fineness between 5 microns and 25 microns.
  • the extrusion openings adjoin an air gap 12 which the freshly extruded spun threads 10 pass through and in which the spun threads are hidden by a tensile stress.
  • a cooling gas flow 13 is directed to the spun yarns 10, which is generated by a blowing device 14.
  • Temperature, humidity and composition of the cooling gas flow 13 can be regulated by an air conditioning device 15 to predetermined or variably predeterminable values.
  • the cooling gas stream 13 acts at a distance from the spinneret 9, on the spun yarns 10 and has a velocity component in the extrusion direction E, so that the spun yarns are mitverstreckt by the cooling gas stream 13. In order to allow a good heat transfer, the cooling gas flow 13 is turbulent.
  • the spun threads 10 After passing through the air gap 12, the spun threads 10 enter a precipitation bath 16.
  • the cooling gas flow 13 is sufficiently spaced from the surface 17 of the precipitation bath, so that it does not impinge on the surface.
  • the spun threads 10 are deflected by a substantially roller-shaped deflecting member 18 to a bundling member 19 above the precipitation bath, so that they again pass through the Klallbadober Structure 17.
  • the deflection can be rigid or fixed, or rotate with the threads.
  • the bundling member 19 is rotatably driven and exerts as the first drawing means via the deflection member 18 a back to the extrusion openings of the spinneret 9 retrospective tensile stress on the spun yarns 10, which stretches the spun yarns 10.
  • the stretching means and the deflecting member 18 may be driven.
  • the tensile stress can also be generated only by the cooling gas stream 13 as the first drawing agent. This has the advantage that the tensile stress is introduced into the spun threads 10 by a friction stress acting on the surface of the spun threads.
  • the filaments 10 are combined to form a bundle of fibers 20. Subsequently, the still wetted with the Klallbadans 16, combined to form the bundle of fibers 20 spun yarns 10 are placed without tension on a conveyor 21 and transported largely tensionless on this. During the transport of the filaments on the conveyor 21, the complete or almost complete coagulation of the cellulose filaments can take place under the lowest possible voltage influence.
  • the conveyor 21 may, as in Fig. 1 is shown to be configured as a vibrating conveyor, which transports the bundle of fibers 20, or optionally a plurality of bundles of fibers 20 at the same time, by vibrations in the conveying direction F.
  • the vibrations of the conveyor 21 are indicated by the double arrow 22.
  • the spun-thread bundle 20 is deposited in an orderly manner on the conveyor.
  • other conveying devices such as a plurality of godets arranged one behind the other, can be used with almost the same or peripheral speed decreasing in the conveying direction.
  • various treatments of the bundle of fibers 20 can be carried out, for example, the bundle of fibers 20 washed once or more times, dried and aviviert, for example by a sprinkler 23 from a treatment medium 24 is sprayed onto the filament bundle 20.
  • the bundle of fibers 20 is received by a godet 25 of the conveyor 21 and fed to a second Nachverstreckungsstoff 26 through which the effetkoagul functioning filaments 10 are nachverstreckt.
  • the second Nachverstreckungsstoff 26 may also be provided immediately after the bundling means 19, ie between the conveyor 21 and the precipitation bath 16, so that only the nachverstreckten filaments are subjected to further treatment steps.
  • the post-stretching means 26 in the entry region of the spun yarn 20 may have a heating device 27 which brings the spun-fiber bundle 20 to a predetermined temperature and at the same time dries the spun-fiber bundle 20 at least superficially.
  • the spun yarns are guided over two godets 28, 29, which are driven so that the spun yarn bundle 20 between them with a predetermined Nachverstreckungs tensile stress Z N is applied.
  • the spunbond bundle charged with this tension is maintained at a predetermined high temperature and can be impregnated during post-stretching, in particular by a hot inert gas, such as air, or by steam, for example dry steam, and swelling agents or other chemical fiber treatment means, such as Arrows 30 is indicated.
  • a hot inert gas such as air
  • steam for example dry steam
  • swelling agents or other chemical fiber treatment means such as Arrows 30 is indicated.
  • the godets 28, 29 may also be heated.
  • the spun-thread bundle 20 has a reduced crimp compared with conventional fibers, so that it is crimped over a stuffer box 31. Subsequently, the fiber bundle 20 is cut by a cutting device 32. If an endless fiber to be generated, of course, can be dispensed with the crimping and / or cutting.
  • the crimped staple fibers can be transported in random orientation in the form of a crimped endless cable 33 on a conveyor 34 for further method steps.
  • a post-stretching means 26 is shown schematically.
  • a post-stretching takes place in the form of a voltage drying.
  • the Nachverstreckungsstoff 26 two godets 28, 29, which are driven so that the thread bundle 20 between them with a predetermined tensile stress Z N of at least 0.8 cN / tex, preferably at least 3.5 cN / tex stretched or stretched.
  • a predetermined tensile stress Z N of at least 0.8 cN / tex, preferably at least 3.5 cN / tex stretched or stretched.
  • the following in the conveying direction F godet 29 with a predetermined, higher speed to be rotated as the galette 28 located in the conveying direction F; wherein between the godet 29 and the looped around the godet thread bundle 20, a slip can prevail, which essentially determines the tensile stress Z N.
  • One or both godets 28, 29 can be provided with an at least gas-permeable surface 30, through which a hot inert gas, steam or dry steam from the interior of the godet 28, 29 is pressed by the spun-thread bundle 20 looped around the godet 28, 29.
  • each Galette 28, 29 may also be associated with a steam-permeable, actively or passively co-rotating roller 28a, 29a in opposition, as shown schematically in FIG Fig. 3 is shown.
  • the rollers 28a, 29a also have permeable surfaces through which the inert gas or the vapor is sucked off. Instead of rollers and large drums can be provided.
  • godets 28, 29 and larger drums or suction drums can be used with perforated surface, through which the hot gas is sucked.
  • the bundle of fibers was dried without tension, remoistened and dried under tension.
  • the bundle of fibers was passed through two eyelets at a distance of 50 cm and was weighted during drying on both sides with 19 kg each.
  • the bundle of fibers was dried without tension, remoistened and dried under tension.
  • the bundle of fibers was passed through two eyelets at a distance of 50 cm and weighted on both sides with 38 kg each.
  • experiment 5 the bundle of fibers was dried wet under tension.
  • the thread bundle was guided through two eyelets at a distance of 50 cm and weighted on both sides, each with a weight of 9 kg.
  • experiment 6 the bundle of fibers was dried wet under tension.
  • the thread bundle was guided through two eyelets at a distance of 50 cm and weighted on both sides, each with a weight of 19 kg.
  • experiment 7 the bundle of fibers was dried wet under tension.
  • the thread bundle was guided through two eyelets at a distance of 50 cm and weighted on both sides, each with a weight of 38 kg.
  • the bundle of fibers was subjected to treatment with sodium hydroxide solution (NaOH) before drying.
  • NaOH sodium hydroxide solution
  • the filament bundle was treated with 5% NaOH solution for 5 minutes and then washed with completely deionized water.
  • the NaOH solution was neutralized with 1% formic acid and washed again with deionized water.
  • the spunbond bundle was then dried in the dryer at 73 ° C for 30 minutes.
  • the bundle of fibers was dried without tension, remoistened and dried under tension.
  • the bundle of fibers was guided through two eyelets at a distance of 50 cm and weighted on both sides with 19 kg each.
  • the bundle of fibers was dried without tension, remoistened and dried under tension.
  • the bundle of fibers was passed through two eyelets at a distance of 50 cm and weighted on both sides with 38 kg each.
  • experiment 12 the bundle of fibers was dried wet under tension.
  • the thread bundle was guided through two eyelets at a distance of 50 cm and weighted on both sides, each with a weight of 9 kg.
  • experiment 13 the bundle of fibers was dried wet under tension.
  • the thread bundle was guided through two eyelets at a distance of 50 cm and weighted on both sides, each with a weight of 19 kg.
  • experiment 14 the bundle of fibers was dried wet under tension.
  • the thread bundle was guided through two eyelets at a distance of 50 cm and weighted on both sides, each with a weight of 38 kg.
  • the titer For the dried bundles of fibers, the titer, the tenacity, the maximum tenacity, the wet denier, the wet maximum tenacity, the tenacity at break, the wet modulus, and the wet abrasion number were then determined. The procedure was as follows.
  • the titer was determined according to DIN EN ISO 1973.
  • the (wet) maximum tensile strength and the (wet) maximum tensile elongation were determined in accordance with DIN EN ISO 5079.
  • the maximum loop tension was determined in accordance with DIN 53843 Part 2.
  • the wet modulus was determined on a fiber bundle, which is usable according to DIN EN 1973. The procedure is based on the test specification ASG N 211 of Alceru Schwarza GmbH. The tests for determining the wet modulus were carried out on a tensile testing machine with constant strain rate and low-path electronic force measurement.
  • the gripping length of the thread bundle was 10.0 mm ⁇ 0.1 mm.
  • the fineness biasing force was 2.5 mN / tex ⁇ 0.5 mN / tex for a titer greater than 2.4 dtex. At a titer of up to 2.4 dtex, a biasing mass of 50 mg was used.
  • the elongation rates were 2.5 mm / min with an average wet elongation at break up to 10%, 5.0 mm / min with an average wet elongation at break of more than 10 to 2% and 7.5 mm / min with a mean wet elongation at break of over 20%.
  • the spun yarn bundle to be clamped is clamped with its end opposite the biasing mass piece in the tensile testing machine, then the lower clamping clamp is closed and the submerged vessel with the wetting agent solution is raised so that the liquid level reaches as far as possible to the upper clamping clamp without them however, to touch.
  • the distance between the grips is at the strain rate indicated above to increase steadily until an elongation of 5% is reached. At this moment, stop the movement of the lower clamp and determine the wet pull force in mN down to one decimal.
  • the wet scrubbing number was determined using a Fasemassscheuerprüf réelle FNP SMK Complexing/Samples.
  • the wet scrub number is the number of revolutions of the scrubbing shaft until the breakage of the fiber clamped under defined pretension in the wet scrub tester.
  • the pretensioning weight is 70 mg at a titer between 1.2 and 1.8 dtex.
  • the speed of the scouring shaft was 400 rpm, the wrap angle 45 °.
  • the scouring shaft is provided with a fabric hose.
  • the maximum tensile force measured both wet and dry, is essentially unchanged from the non-post-stretched fibers of Experiment 1.

Claims (17)

  1. Procédé pour la fabrication de fibres Lyocell à partir d'une solution de filage renfermant de l'eau, de la cellulose et un oxyde d'amine tertiaire, selon lequel on exécute les étapes de procédé suivantes :
    - extrusion de la solution de filage en formant des fils de filage (10),
    - étirage des fils de filage (10),
    - passage des fils de filage à travers un bain de précipitation (16),
    caractérisé par l'étape de procédé suivante :
    - post-étirage et traitement thermique simultané des fils de filage (10) étirés, après le passage à travers le bain de précipitation (16).
  2. Procédé selon la revendication 1, caractérisé par l'étape de procédé suivante :
    - coagulation de la cellulose des fils de filage (10) avant l'étirage.
  3. Procédé selon la revendication 1 ou 2, caractérisé par l'étape de procédé suivante :
    - post-étirage pour une tension de traction d'au moins 0,8 cN/tex.
  4. Procédé selon la revendication 3, caractérisé par l'étape de procédé suivante :
    - post-étirage pour une tension de traction d'au moins 3,5 cN/tex.
  5. Procédé selon l'une des revendications précédentes, caractérisé par l'étape de procédé suivante :
    - traitement des fibres de filage pendant le traitement thermique, à l'aide de gaz inerte chaud.
  6. Procédé selon l'une des revendications précédentes,
    caractérisé par l'étape de procédé suivante :
    - traitement des fibres de filage pendant le traitement thermique, à l'aide de vapeur.
  7. Procédé selon l'une des revendications précédentes,
    caractérisé par l'étape de procédé suivante :
    - passage des fibres de filage (10) dans un interstice d'air (12) avant le bain de précipitation (16).
  8. Procédé selon la revendication 7, caractérisé par l'étape de procédé suivante :
    - soufflage d'un écoulement ou courant de gaz de refroidissement sur les fils de filage (10) dans l'interstice d'air (12).
  9. Procédé selon l'une des revendications précédentes, caractérisé par l'étape de procédé suivante :
    - transport exempt de tension de traction des fils de filage entre l'étirage et le post-étirage.
  10. Procédé selon l'une des revendications précédentes, caractérisé par l'étape de procédé suivante :
    - frisage des fils de filage (10) ayant subi le post-étirage.
  11. Procédé selon l'une des revendications précédentes, caractérisé par l'étape de procédé suivante :
    - coupe des fils de filage ayant subi le post-étirage, pour former des fibres coupées.
  12. Dispositif (1) pour la fabrication de fibres de filage (10) à partir d'une solution de filage renfermant de l'eau, de la cellulose et un oxyde d'amine tertiaire, comprenant une filière de filage (9) par laquelle la solution de filage peut, en service, être extrudée en des fils de filage (10), comprenant également un bain de précipitation (16) avec un agent de précipitation provoquant la précipitation de la cellulose, et à travers lequel sont menés les fils de filage, en service, comprenant en outre un premier moyen d'étirage (13, 18, 19) par lequel les fils de filage peuvent être étirés en service, ainsi qu'un deuxième moyen d'étirage (28, 29) par lequel les fils de filage (10) ayant été étirés par le premier moyen d'étirage (13, 18, 19) peuvent, en service, être post-étirés, et le dispositif comprenant finalement un dispositif de chauffage (27, 30) agencé dans la zone du deuxième moyen d'étirage (28, 29) et permettant, en service, d'échauffer les fils de filage (10) pendant le post-étirage, caractérisé en ce que les fils de filage (10) peuvent être étirés par le premier moyen détirage (13, 18, 19) dans un interstice d'air (12), avant l'entrée dans le bain de précipitation (16).
  13. Fibre Lyocell, notamment fabriquée d'après le procédé selon l'une des revendications 1 à 11, caractérisée par un module humide d'au moins 250 cN/tex et par un indice ou nombre de résistance à l'abrasion ou fibrillation par 25 fibres d'au moins 18.
  14. Fibre Lyocell selon la revendication 13, caractérisée par un module humide d'au moins 300 cN/tex.
  15. Fibre Lyocell selon la revendication 14, caractérisée par un module humide d'au moins 350 cN/tex.
  16. Fibres de cellulose selon l'une des revendications 13 à 15, caractérisées par un allongement sous force de traction en condition humide, d'au plus 12%.
  17. Fibres de cellulose selon l'une des revendications 13 à 16, caractérisées par un indice ou nombre de résistance à l'abrasion ou fibrillation par 25 fibres d'au moins 25.
EP04710007A 2003-04-01 2004-02-11 Procede et dispositif pour produire des fils de cellulose post-etires Expired - Lifetime EP1608803B1 (fr)

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DE10314878 2003-04-01
DE10314878A DE10314878A1 (de) 2003-04-01 2003-04-01 Verfahren und Vorrichtung zur Herstellung nachverstreckter Cellulose-Spinnfäden
PCT/EP2004/001268 WO2004088010A1 (fr) 2003-04-01 2004-02-11 Procede et dispositif pour produire des fils de cellulose post-etires

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Families Citing this family (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10200405A1 (de) 2002-01-08 2002-08-01 Zimmer Ag Spinnvorrichtung und -verfahren mit Kühlbeblasung
DE10200406A1 (de) * 2002-01-08 2003-07-24 Zimmer Ag Spinnvorrichtung und -verfahren mit turbulenter Kühlbeblasung
DE10204381A1 (de) 2002-01-28 2003-08-07 Zimmer Ag Ergonomische Spinnanlage
DE10206089A1 (de) 2002-02-13 2002-08-14 Zimmer Ag Bersteinsatz
DE10213007A1 (de) * 2002-03-22 2003-10-09 Zimmer Ag Verfahren und Vorrichtung zur Regelung des Raumklimas bei einem Spinnprozess
DE10223268B4 (de) * 2002-05-24 2006-06-01 Zimmer Ag Benetzungseinrichtung und Spinnanlage mit Benetzungseinrichtung
DE102004024030A1 (de) 2004-05-13 2005-12-08 Zimmer Ag Lyocell-Verfahren mit polymerisationsgradabhängiger Einstellung der Verarbeitungsdauer
DE102004024028B4 (de) * 2004-05-13 2010-04-08 Lenzing Ag Lyocell-Verfahren und -Vorrichtung mit Presswasserrückführung
DE102004024029A1 (de) * 2004-05-13 2005-12-08 Zimmer Ag Lyocell-Verfahren und -Vorrichtung mit Steuerung des Metallionen-Gehalts
DE102005024433A1 (de) * 2005-05-24 2006-02-16 Zimmer Ag Verfahren und Vorrichtung zum Schneiden von NMMO-haltigen Spinnfäden sowie für Zellulose-Stapelfasern
AT503803B1 (de) * 2006-06-14 2008-01-15 Chemiefaser Lenzing Ag Lyocell-stapelfaser
AT504144B1 (de) * 2006-08-17 2013-04-15 Chemiefaser Lenzing Ag Verfahren zur herstellung von zellulosefasern aus einer lösung von zellulose in einem tertiären aminoxid und vorrichtung zur durchführung des verfahrens
ES2434019T3 (es) * 2006-12-22 2013-12-13 Reifenhäuser GmbH & Co. KG Maschinenfabrik Procedimiento y dispositivo para la fabricación de una tela hilada por adhesión a partir de filamentos de celulosa
KR101205940B1 (ko) * 2007-06-11 2012-11-28 코오롱인더스트리 주식회사 라이오셀 번들 및 이를 포함하는 타이어 코드
AT505511B1 (de) * 2007-07-11 2014-03-15 Chemiefaser Lenzing Ag Füllfaser mit verbessertem öffnungsverhalten, verfahren zu deren herstellung und deren verwendung
EP2235240B1 (fr) * 2008-01-16 2012-02-08 Lenzing AG Mélanges de fibres, fils et tissus faits à partir de ces mélanges
CN106894114A (zh) * 2017-04-18 2017-06-27 广东洪兴实业有限公司 一种具有服装用的高韧性天丝纤维的制备工艺
JP2020536186A (ja) * 2017-10-06 2020-12-10 レンチング アクチエンゲゼルシャフト 難燃性リヨセルフィラメント
EP3505659A1 (fr) * 2018-08-30 2019-07-03 Aurotec GmbH Procédé et dispositif de filage des filaments à déviation
CN112442775A (zh) * 2019-09-02 2021-03-05 连津格股份公司 在莫代尔纺丝方法中施加拉伸
CN114351316B (zh) * 2022-01-13 2023-09-19 碧菲分离膜（大连）有限公司 一种纳米细菌纤维素超细纤维加工设备
CN115386991A (zh) * 2022-06-14 2022-11-25 青纺联（枣庄）纤维科技有限公司 一种仿麻型莱赛尔花式纱及其制备方法

Family Cites Families (58)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1655433A (en) * 1924-08-23 1928-01-10 Int Paper Co Vacuum relief means for water-pipe lines
US1765883A (en) * 1926-07-14 1930-06-24 Ruschke Ewald Safety device for boiler feed and delivery pipings
US2518827A (en) * 1945-02-23 1950-08-15 Dryco Corp Protected metal water confining means
US3061402A (en) * 1960-11-15 1962-10-30 Dow Chemical Co Wet spinning synthetic fibers
US3404698A (en) * 1965-05-26 1968-10-08 Navy Usa Fluid charging valve
IT987063B (it) * 1973-04-06 1975-02-20 Smia Viscosa Soc Nazionale Ind Macchina perfezionata per la fila tura ed il trattamento in continuo di filamenti e filati di rayon viscosa
FI752732A (fr) * 1974-10-03 1976-04-04 Teijin Ltd
US3932576A (en) * 1974-12-23 1976-01-13 Concorde Fibers, Inc. Apparatus for and method of melt spinning
US4033742A (en) * 1976-02-13 1977-07-05 Kaiser Glass Fiber Corporation Method for producing glass fibers
US4246221A (en) * 1979-03-02 1981-01-20 Akzona Incorporated Process for shaped cellulose article prepared from a solution containing cellulose dissolved in a tertiary amine N-oxide solvent
US4142913A (en) * 1977-07-26 1979-03-06 Akzona Incorporated Process for making a precursor of a solution of cellulose
US4144080A (en) * 1977-07-26 1979-03-13 Akzona Incorporated Process for making amine oxide solution of cellulose
US4416698A (en) * 1977-07-26 1983-11-22 Akzona Incorporated Shaped cellulose article prepared from a solution containing cellulose dissolved in a tertiary amine N-oxide solvent and a process for making the article
US4211574A (en) * 1977-07-26 1980-07-08 Akzona Incorporated Process for making a solid impregnated precursor of a solution of cellulose
US4219040A (en) * 1978-02-15 1980-08-26 Draft Systems, Inc. Rupture disc safety valve
US4193962A (en) * 1978-08-11 1980-03-18 Kling-Tecs, Inc. Melt spinning process
US4477951A (en) * 1978-12-15 1984-10-23 Fiber Associates, Inc. Viscose rayon spinning machine
US4263929A (en) * 1979-01-08 1981-04-28 Kearney John G Electropneumatic pressure relief indicator
US4261941A (en) * 1979-06-26 1981-04-14 Union Carbide Corporation Process for preparing zeolite-containing detergent agglomerates
US4261943A (en) * 1979-07-02 1981-04-14 Akzona Incorporated Process for surface treating cellulose products
US4425293A (en) * 1982-03-18 1984-01-10 E. I. Du Pont De Nemours And Company Preparation of amorphous ultra-high-speed-spun polyethylene terephthalate yarn for texturing
US4713290A (en) * 1982-09-30 1987-12-15 Allied Corporation High strength and modulus polyvinyl alcohol fibers and method of their preparation
US4529368A (en) * 1983-12-27 1985-07-16 E. I. Du Pont De Nemours & Company Apparatus for quenching melt-spun filaments
US4869860A (en) * 1984-08-09 1989-09-26 E. I. Du Pont De Nemours And Company Spinning process for aromatic polyamide filaments
JPH0376822A (ja) * 1989-03-17 1991-04-02 Toray Ind Inc アクリル系耐炎化繊維の製造方法
AT395863B (de) * 1991-01-09 1993-03-25 Chemiefaser Lenzing Ag Verfahren zur herstellung eines cellulosischen formkoerpers
AT395862B (de) * 1991-01-09 1993-03-25 Chemiefaser Lenzing Ag Verfahren zur herstellung eines cellulosischen formkoerpers
US5191990A (en) * 1991-06-24 1993-03-09 Bs&B Safety Systems, Inc. Flash gas venting and flame arresting apparatus
JP3076822B2 (ja) * 1991-07-18 2000-08-14 ウェルファイド株式会社 イソチオシアン酸アリル噴霧剤
US5658524A (en) * 1992-01-17 1997-08-19 Viskase Corporation Cellulose article manufacturing method
US5275545A (en) * 1992-02-26 1994-01-04 Kabushiki Kaisha San-Al Vacuum cast molding apparatus
ATA53792A (de) * 1992-03-17 1995-02-15 Chemiefaser Lenzing Ag Verfahren zur herstellung cellulosischer formkörper, vorrichtung zur durchführung des verfahrens sowie verwendung einer spinnvorrichtung
US5262099A (en) * 1992-04-01 1993-11-16 E. I. Du Pont De Nemours And Company Process of making high tenacity polyamide monofilaments
DE4312219C2 (de) * 1993-04-14 2002-05-08 Thueringisches Inst Textil Verfahren zur Reduzierung der Fibrillierbarkeit von lösungsgesponnenen Cellulosefasern
MY115308A (en) * 1993-05-24 2003-05-31 Tencel Ltd Spinning cell
US5362430A (en) * 1993-07-16 1994-11-08 E. I. Du Pont De Nemours And Company Aqueous-quench spinning of polyamides
AT403584B (de) * 1993-09-13 1998-03-25 Chemiefaser Lenzing Ag Verfahren und vorrichtung zur herstellung cellulosischer flach- oder schlauchfolien
DE4336097A1 (de) * 1993-10-22 1995-04-27 Bayer Ag Kontinuierliches Verfahren zum Schmelzspinnen von monofilen Fäden
DE4444140A1 (de) * 1994-12-12 1996-06-13 Akzo Nobel Nv Lösungsmittelgesponnene cellulosische Filamente
US5984655A (en) * 1994-12-22 1999-11-16 Lenzing Aktiengesellschaft Spinning process and apparatus
DE19511151A1 (de) * 1995-03-27 1996-10-02 Alfred Steinforth Verfahren und Vorrichtung zum multifilen Spinnen semipermiabeler Hohlfäden aus Cellulose
DE19512053C1 (de) * 1995-03-31 1996-10-24 Akzo Nobel Nv Verfahren zum Herstellen von cellulosischen Fasern
DE19600090A1 (de) * 1996-01-03 1997-07-10 Bayer Faser Gmbh Verfahren und Vorrichtung zur Herstellung von schmelzgesponnenen Monofilen
US6173767B1 (en) * 1996-10-11 2001-01-16 Sgcm Partnership, L.P. Pressure release device for cooling coils
DE19753806A1 (de) * 1996-12-12 1998-06-18 Barmag Barmer Maschf Verfahren und Vorrichtung zum kontinuierlichen Herstellen von einem Viskose-Faden
DE19721609A1 (de) * 1997-05-23 1998-11-26 Zimmer Ag Verfahren und Vorrichtung zum Verspinnen von Cellulosecarbamat-Lösungen
AT406386B (de) * 1998-07-28 2000-04-25 Chemiefaser Lenzing Ag Verfahren und vorrichtung zur herstellung cellulosischer formkörper
US6117379A (en) * 1998-07-29 2000-09-12 Kimberly-Clark Worldwide, Inc. Method and apparatus for improved quenching of nonwoven filaments
US6692687B2 (en) * 2000-01-20 2004-02-17 E. I. Du Pont De Nemours And Company Method for high-speed spinning of bicomponent fibers
DE10005163A1 (de) * 2000-02-08 2001-08-16 Thueringisches Inst Textil Verfahren zur Herstellung und Verarbeitung einer Celluloselösung
DE10016307C2 (de) * 2000-03-31 2002-05-08 Thueringisches Inst Textil Verfahren zur Herstellung und Verarbeitung einer Celluloselösung
DE10200405A1 (de) * 2002-01-08 2002-08-01 Zimmer Ag Spinnvorrichtung und -verfahren mit Kühlbeblasung
DE10200406A1 (de) * 2002-01-08 2003-07-24 Zimmer Ag Spinnvorrichtung und -verfahren mit turbulenter Kühlbeblasung
US6890435B2 (en) * 2002-01-28 2005-05-10 Koch Membrane Systems Hollow fiber microfiltration membranes and a method of making these membranes
DE10204381A1 (de) * 2002-01-28 2003-08-07 Zimmer Ag Ergonomische Spinnanlage
DE10206089A1 (de) * 2002-02-13 2002-08-14 Zimmer Ag Bersteinsatz
DE10213007A1 (de) * 2002-03-22 2003-10-09 Zimmer Ag Verfahren und Vorrichtung zur Regelung des Raumklimas bei einem Spinnprozess
DE10223268B4 (de) * 2002-05-24 2006-06-01 Zimmer Ag Benetzungseinrichtung und Spinnanlage mit Benetzungseinrichtung

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EP1608803A1 (fr) 2005-12-28
CN1774527A (zh) 2006-05-17
CN100410430C (zh) 2008-08-13
TW200422447A (en) 2004-11-01
US20060083918A1 (en) 2006-04-20
DE502004007553D1 (de) 2008-08-21
DE10314878A1 (de) 2004-10-28
BRPI0409544B1 (pt) 2014-07-22
BRPI0409544A (pt) 2006-04-18
ATE400677T1 (de) 2008-07-15
KR100691913B1 (ko) 2007-03-09
KR20050119675A (ko) 2005-12-21
WO2004088010A1 (fr) 2004-10-14
ZA200507946B (en) 2009-01-28

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