EP1327013B1 - Gekräuselter faser und verfahren zu deren herstellung - Google Patents

Gekräuselter faser und verfahren zu deren herstellung Download PDF

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EP1327013B1
EP1327013B1 EP01986728A EP01986728A EP1327013B1 EP 1327013 B1 EP1327013 B1 EP 1327013B1 EP 01986728 A EP01986728 A EP 01986728A EP 01986728 A EP01986728 A EP 01986728A EP 1327013 B1 EP1327013 B1 EP 1327013B1
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EP
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Prior art keywords
fibre
weight
lyocell
thermoplastic polymer
percent
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EP01986728A
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English (en)
French (fr)
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EP1327013A1 (de
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Gregory James Askew
Malcom John Hayhurst
Andrew Peter Slater
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Lenzing AG
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Lenzing AG
Chemiefaser Lenzing AG
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F11/00Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/02Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins

Definitions

  • This invention relates to modified lyocell fibre and to a process for the preparation of modified lyocell fibre.
  • "Fibre” is used in this specification to include continuous filament yarns, tows of yarn for cutting into staple fibre and also staple fibre formed from such a tow.
  • Lyocell fibre is produced by dissolving cellulose in a suitable solvent, for example a tertiary amine N-oxide such as N-methyl morpholine oxide mixed with water.
  • a suitable solvent for example a tertiary amine N-oxide such as N-methyl morpholine oxide mixed with water.
  • a suitable method of manufacture is described in US-A-4,416,698.
  • the solution of cellulose in the amine oxide solvent which is solid at ambient temperature, is extruded at a temperature of 95-125°C from a spinneret through an air gap into a precipitation bath of water or dilute aqueous amine oxide, and the amine oxide solvent leaches into the bath, producing cellulose fibre.
  • JP-A-8-170224 discloses a disperse dyeable biconstituent fibre of the islands-in-the-sea type in which the continuous "sea" component is a cellulose polymer spun from an organic solvent system and the "islands" are composed of a polymer dyeable by a disperse dye and are 0.01-3 m in size and form 2-45% by weight of the fibre.
  • GB-A-2121069 discloses viscose rayon fibres for the production of non-wovens containing as mineral fillers barium sulphate, talcum, muskovite, or a mixture thereof, in an amount of from 15 to 60%, preferably 40 to 50%, of the total fibre mass, and, if desired, additionally hydrophobic, polymer or oligomer substances, such as polyethylene, polypropylene, polystyrene, polyacrylic acid ester, polyester, polytetrafluoroethylene or waxes, in an amount of from 1 to 60%, preferably 25 to 50%, of the total fibre mass.
  • GB-A-2008126 discloses the use of polystyrene as a delustrant for viscose rayon fibres.
  • WO-A-98/46814 discloses lyocell fibre containing elongated domains of polyester, polyamide or an olefin copolymer, the domains having an aspect ratio of at least 1.5 and being aligned substantially parallel to the axis of the fibre.
  • the domains are 70-1000 nm in length and 30-400 nm in diameter. It has however been found that it is difficult to control domain dimensions within these limits during commercial scale production.
  • the fibre can be carded without the use of a lubricant.
  • lyocell fibre which does not contain low-melting thermoplastic polymer requires a lubricant for carding, and the conventional stage to apply the lubricant is to the wet fibre, before it is dried during the production process.
  • Example 1 of WO-A-98/46814 forms spun fibre by extruding a solidified dope prepared from a cooled solution of cellulose in N-methylmorpholine oxide and dispersed polyester (Mpt 90°C; 2 wt% based on cellulose) to form filaments which cross an air gap into an aqueous spin bath. It then collects a tow of the filaments, dries the tow and crimps it in a stuffer-box before cutting it into 38mm staple fibre.
  • Mpt 90°C 2 wt% based on cellulose
  • Lyocell fibre is naturally uncrimped. However, crimp is desirable, particularly in staple fibre. Crimp can be generated in lyocell fibre by compression of wet fibre in accordance with the disclosure of EP-A- 0,797,696 or by stuffer-box crimping with the aid of dry steam, as disclosed in EP-A-0,703,997. Experience has shown that such a dry steam process, although less damaging to the fibre, is unable to generate more than about 2.3 crimps/cm without damage in conventional lyocell fibre.
  • conventional lyocell fibre as used herein, is meant lyocell fibre which does not contain low-melting thermoplastic polymer. Only conventional lyocell fibre is and ever has been commercially available.
  • WO-A-96/46814 is silent as to the number of crimps/cm generated and does not suggest a level of crimping above 2.3 crimps/cm.
  • a method for the manufacture of lyocell fibre including the steps of:
  • thermoplastic polymer used is sufficient to show a change in colour on dyeing with a disperse dye of the fibre containing the thermoplastic polymer.
  • the glass transition temperature (Tg) indicates the temperature region in which the polymer characteristically changes from a hard, more or less brittle glass to a rubbery or viscous polymer within which motions of portions of the chains, usually called segments, are comparatively unhampered by the interactions of neighbouring chains (Principles of Polymer Chemistry, Paul J Flory, Cornell University Press, 15 th printing 1992, ISBN 0-8014-0134-8, page 56).
  • the thermoplastic polymer has a melting point greater than 50°C, preferably of not more than 150°C, more preferably of between 80°C and 130°C, as measured by differential thermal analysis.
  • the glass transition temperature (Tg) of the polymer is preferably between -20°C and 130°C, more preferably between 30°C and 130°C.
  • thermoplastic polymer is preferably a thermoplastic polymer selected from the group consisting of polyesters, polyamides and olefin polymers.
  • thermoplastic polymer is preferably dispersed throughout the lyocell in domains, and the maximum dimension of substantially all of the domains is preferably no more than 50 nanometres (nm).
  • the fibre is preferably crimped so as to induce from 3.5 to 8 crimps/cm in the fibre.
  • the solution may have a matting agent such as titanium dioxide particles dispersed therein, whereby the resulting fibre contains dispersed therein from 0.1 to 5 percent by weight, preferably from 0.1 to 2 percent by weight, more preferably from 0.2 to 1 percent by weight, of titanium dioxide particles based on the weight of cellulose.
  • a matting agent such as titanium dioxide particles dispersed therein
  • soft finish (lubricant) is applied to the fibre prior to crimping.
  • the amount of soft finish applied is preferably in the range from 0.01 to 2 percent by weight, more preferably from 0.1 to 0.5 percent by weight, most preferably from 0.15 to 0.4 percent by weight, based on the weight of the fibre.
  • the achievable crimp level may be found to vary directly with the amount of soft finish applied, at least within the lower regions of these ranges.
  • Crimp may be induced in the fibre by the method disclosed in EP-A-0 703 997.
  • the resulting fibre preferably has a titre in the range from 0.5 to 5 decitex, more preferably from 1 to 3.5 decitex.
  • the method of the invention may further include the step of cutting the fibre to a staple length in the range from 3 to 100 mm, more preferably from 20 to 75mm.
  • the fibre has applied to it after washing and before drying a reagent having from two to six functional groups reactive with cellulose, which is reacted onto the fibre, either before or during drying.
  • lyocell fibre having dispersed therein from 0.01 to 30 percent by weight, more preferably from 0.01 to 10 percent by weight, most preferably from 0.1 to 10 percent by weight, based on the weight of cellulose, of particles of a thermoplastic polymer having a melting point of from greater than 50°C to 150°C, the fibre being characterised by having from 2.5 to 8 crimps/cm.
  • the low-melting thermoplastic polymer is preferably a low-melting thermoplastic polymer selected from the group consisting of polyesters, polyamides and olefin polymers.
  • fibre made by the method of the invention and fibre of the invention can be carded satisfactorily at remarkably high speeds, in some cases even at about twice the speed which can satisfactorily be used on conventional lyocell fibre.
  • Carding speed is a very significant rate-limiting factor in the production of non-wovens.
  • Non-wovens frequently use a dull or matt fibre and the presence of titanium dioxide as dulling or matting agent does not adversely affect the process of the invention or the properties of the fibre of the invention, including its high speed carding properties.
  • the lyocell fibre according to the invention may be in the form of a staple fibre of length preferably in the range from 3 to 100 mm, more preferably from 20 to 75 mm.
  • the lyocell fibre according to the invention has preferably had applied thereto from 0.01 to 2 percent by weight, more preferably from 0.1 to 0.5 percent by weight, most preferably from 0.15 to 0.4 percent by weight, of a soft finish, based on the weight of the fibre.
  • Preferred lyocell fibre according to the invention includes domains of the low-melting thermoplastic polymer, which is selected from the group consisting of polyesters, polyamides and olefin polymers, and it contains from 0.1 to 30 percent by weight, preferably from 0.5 to 10 percent by weight, most preferably from 1 to 5 percent by weight, based on the weight of cellulose, of the low-melting thermoplastic polymer, and substantially all of the domains are not visible when viewed by electron microscopy at x9000 enlargement
  • the maximum dimension of substantially all of the domains is no more than 50 nm.
  • the domains may be visible at higher magnifications, for example x55000 enlargement.
  • the fibre of the invention can be made from a solution of cellulose in an aqueous tertiary amine N-oxide ("amine oxide”), e.g. N-methylinorpholine N-oxide, which solution contains a suitable thermoplastic low-melting polymer in molten form.
  • amine oxide e.g. N-methylinorpholine N-oxide
  • the solution is extruded through a spinneret via an air-gap into an aqueous coagulating bath.
  • the extrusion temperature is typically in the range from 90 to 125°C.
  • the thusly-extruded fibre is then washed and dried.
  • thermoplastic low-melting polymer should generally be sufficiently compatible with the cellulose solution that the polymer when molten does not agglomerate as a separate phase from the cellulose solution, but it is preferably not soluble either in amine oxide at the dilution at which it is used in the coagulating bath or in water.
  • a polymer should be chosen which is essentially all retained in the fibre during the extrusion (spinning), washing and drying processes.
  • One type of preferred low-melting polymer is a polyester, carboxy-functional polyesters being particularly preferred.
  • the polymer preferably has an acid value of at least 10, up to for example 50 or 100 or even 150. We also believe that a branched polymer structure may be advantageous.
  • polyesters of this type having the required low melting point are formed from a mixture of aromatic dicarboxylic acids selected from isophthalic acid, terephthalic acid and phthalic acid or anhydride, optionally with an aliphatic dicarboxylic acid such as adipic, succinic or sebacic acid, and one or more aliphatic diols such as neopentyl glycol, ethylene glycol, propylene glycol, propane-1,3-diol, butane-1,4-diol, butylene glycol or diethylene glycol.
  • aromatic dicarboxylic acids selected from isophthalic acid, terephthalic acid and phthalic acid or anhydride
  • an aliphatic dicarboxylic acid such as adipic, succinic or sebacic acid
  • one or more aliphatic diols such as neopentyl glycol, ethylene glycol, propylene glycol, propane-1,3-diol, but
  • Branching can be introduced by a trifunctional reagent, for example trimellitic acid or anhydride or trimethylolpropane, glycerol or pentaerythritol.
  • the required acid value can be obtained by using an appropriate excess of carboxylic acid-functional reagent.
  • Such polyesters are sold for use in thermosetting powder coatings, for example under the Trade Marks "Alftalat”,”Uralac” or “Grilesta".
  • thermoplastic low-melting polymers include polyamides, for example polyamides formed from fatty acid dimers and aliphatic diamines or the copolyamide sold under the Trade Mark “Griltex”, or olefin copolymers, for example ethylene/vinyl acetate or ethylene/butylene/butyl acrylate copolymers, preferably containing a small amount of acrylic acid comonomer to give the preferred acid value.
  • a further alternative low-melting thermoplastic polymer is an olefinic polymer such as poly(vinyl alcohol).
  • the concentration of cellulose in the solution to be extruded is generally 10 to 20% by weight, preferably at least 13 or 15% up to 17 or 18% by weight.
  • the spinning solution preferably contains water, usually in the range 5-15% by weight, with the remainder, generally 65-83% by weight, being amine oxide.
  • the extrusion temperature is generally 95 to 125°C.
  • the low-melting polymer can be added to the cellulose solution at any of various points during its preparation.
  • the polymer can for example be premixed with cellulose pulp, the pulp then being mixed with amine oxide and water to form the spinning solution.
  • the polymer can alternatively be added, preferably in molten form, to a preformed cellulose solution.
  • a relatively high proportion of low-melting polymer is premixed with a preformed cellulose solution, for example forming 10 to 50% by weight of the mixture.
  • the premixture can then be used as a masterbatch to add the low-melting polymer to cellulose solution at the required level.
  • the polymer is added to the amine oxide solvent and the resulting mixture is used to dissolve the cellulose.
  • the cellulose solution containing a low-melting polymer can be extruded to form fibres using the same spinneret at the same temperature as is conventionally used for forming lyocell fibre.
  • the domains of low-melting polymer are believed to be distributed uniformly throughout the fibre as a separate phase.
  • the level of low-melting polymer present in the fibre is from 0.01 to 30 percent by weight, based on cellulose.
  • the presence of the domains of low-melting polymer gives rise to various effects depending on the concentration of low-melting polymer and on the type of low-melting polymer used. More specifically, an amount of up to 15 percent by weight, preferably from 0.01 to 5 percent by weight, may be preferred if only crimp effects (explained hereinafter) are desired, whereas an amount from 1 to 20 percent by weight, preferably from 5 to 15 percent by weight, may be preferred if textile effects (explained hereinafter) are desired.
  • the desired small domains of the thermoplastic polymer can be obtained in various ways.
  • the polymer may be synthesised as small particles.
  • large particles can be comminuted, for example by milling or grinding or, preferably, by subjecting the spinning solution to high-shear conditions.
  • fibre of the invention is considerably easier to dry than conventional lyocell fibre. This permits useful energy savings.
  • lyocell can be reacted with polyfunctional reagents in order to reduce its fibrillation tendency. See, for example, EP 0 538 977, EP 0 665 904 and EP 0 755 467, the contents of all of which are incorporated herein by this reference. Such reactions can be performed either on never-dried or on previously-dried fibre. Similar reactions can be performed on fibre of the invention.
  • fibre of the invention containing more than 6 percent by weight of low melting thermoplastic polyester may react less readily with such polyfunctional reagents than does conventional fibre. This can be counteracted by using more forcing conditions, for example a higher reagent concentration.
  • yarn spun from fibre of the invention advantageously has improved textile effects including higher tenacity and extensibility and contains fewer irregularities (thick and thin spots and neps) and is less hairy than yarn spun from conventional fibre. The differences are especially marked if the fibres being compared were reacted in never-dried state.
  • Yarn spun from crimped fibre of the invention, and fabric formed therefrom, may be more bulky than yarn and fabric of conventional crimped lyocell fibre. This means that fabrics having acceptable porosity to light can be produced from finer yarns, i.e. yarns having a lower tex. The fabric produced from these finer yarns is more uniform and drapes more fluidly.
  • Fibre of the invention may be continuous filament or staple fibre.
  • Fibre of the invention can be formed into woven, knitted or nonwoven (e.g. hydroentangled, needlepunched or meltbonded) fabrics. Such fabrics can be subjected to conventional processing treatments, such as being given a crease-resistant finishing resinated treatment. We have found that such resinated fabric may exhibit a cleaner appearance after repeated laundering than resinated fabric of conventional lyocell fibre. We have found that care should be taken if fibre of the invention containing polyester is to be hot causticised at temperatures above about 50°C, because sodium hydroxide tends to hydrolyse the ester linkages.
  • Fibre of the invention may be dyed with conventional dyes for cellulose, for example direct and reactive dyes.
  • the fibre of the invention generally has a lower water imbibition than conventional fibre. This means that the fibre is less inclined to swell and this enhances the uniformity of dyeing in some applications.
  • One known finishing treatment for lyocell fabric involves deliberate induction of fibrillation, for example by harsh wet processing; defibrillation, for example by enzymatic treatment with a cellulase and dyeing.
  • fabric formed from fibre of the invention is preferably treated with less aggressive cellulases than is fabric formed from conventional fibre.
  • fabric finished in this way may be more absorbent and exhibit better wicking properties than conventional fabric finished in this way, even though the fibre from which it is formed had lower absorbency.
  • the low-melting polymer is generally a hydrophobic polymer, and thus susceptible to dyeing with disperse dyes.
  • Crimp in lyocell fibre can be assessed as follows. A sample of titre about 200 tex is taken from a dry tow and placed under sufficient tension to pull out the crimp. Marks are made on the sample 10 cm apart, and the tension removed. The number of crimps between the marks is then counted. The ratio of tensioned to untensioned length gives the crimp intensity or crimp ratio.
  • a carboxy-functional saturated polyester resin of the kind used in powder coatings, having acid value about 40, melting within the range 95°C to 130°C, and having a branched structure was mixed with 77/23 N-methylmorpholine N-oxide (NMMO)/water in a ploughshare mixer at about 70°C. After about 2 minutes, shredded woodpulp was added, after which mixing was continued for a further 10 minutes. The ratio of woodpulp to resin was 92.8:7.2.
  • NMMO N-methylmorpholine N-oxide
  • the mixture was passed through a Buss 5.5m 2 Filmtruder (Trade Mark) Unit HS0055 to remove excess water and thereby form the spinning solution.
  • the mixture was heated by a water jacket at a temperature of 130°C under a vacuum of 200 mm of mercury. However, temperatures of between 80°C and 150°C could be used and higher or lower vacuums could be used.
  • the mixture was subjected to high-shear conditions in a layer about 2-2.5 mm thick with blade speed about 5 m/sec for about 10 minutes.
  • the spinning solution contained 13.5% cellulose, 1.1% polyester, 75.4% NMMO and the balance water.
  • the solution was extruded at 105°C through a spinnerette by way of an airgap into an aqueous coagulating bath to form a fibre tow in conventional manner.
  • the fibre was then dried as a tow and crimped in the general manner described in EP - A - 0 703 997.
  • the dried fibre was of titre 1.7 dtex, contained about 8.1% polyester on cellulose, and had 8% moisture content.
  • a fibre having a diameter of approximately 10 x 10 -6 m was produced.
  • a cross section of the fibre produced, photographed using transmission electron microscopy at x9000 enlargement, is shown in Figure 1 of the accompanying Figures. The large black cracks are a result of the sample preparation and do not indicate the presence of another material other than cellulose.
  • Polyester domains show as white areas in these Figures. From Figures 2 and 3, it can be seen that the visible polyester domains, compared to the scale at the bottom of the Figures, have a maximum dimension of about 20 nm.
  • the fibre had 2.6 crimps/cm and crimp intensity 1.3.
  • conventional lyocell fibre crimped under the same conditions had 2.3 crimps/cm and crimp intensity 1.23.
  • Example 1 was repeated, except that crimper conditions and fibre soft finish levels were varied.
  • Conventional fibre can be crimped as set out in EP-A-0,703,997 using a stuffer box pressure of about 8psig (55 kPa) and steam pressure of about 20 psig (138 kPa). Higher pressures lead to uneven crimp, tow damage, and stuffer box blockage.
  • fibre of the invention is capable of withstanding more forcing crimping conditions (higher stuffer box pressure, higher steam pressure and higher nip roller pressure) which would irrevocably damage conventional lyocell fibre. These more forcing conditions result in a greater number of crimps per centimetre.
  • the graph also shows that the maximum stuffer box pressure can also be doubled compared to conventional lyocell. Further; the graph shows that the increase in maximum crimp is directly related to increasing the soft finish level. Lower pressures yielded fibre with a similar number of crimps per centimetre to crimped conventional fibre, but with reduced crimp intensity due to reduced crimp amplitude.
  • Example 1 was repeated, except that the fibre was reacted in never-dried state with 1,3,5-triacryloylhexahydro-1,3,5-hexahydrotriazine (TAHT) as described in EP-A-0,755,467 at an application level of 0.7% by weight on the fibre as an anti-fibrillation treatment.
  • TAHT 1,3,5-triacryloylhexahydro-1,3,5-hexahydrotriazine
  • Dyed single-jersey knitted fabrics made from yarns spun from treated fibre of the invention showed no signs of fibrillation after 10 domestic wash/tumble cycles at 40°C.
  • 1.7 dtex lyocell fibre was spun from a solution of cellulose in aqueous NMM0 in conventional manner, the solution containing 4% dispersed thermoplastic carboxy-functional saturated polyester resin of the kind used in powder coatings, having acid value about 40, melting within the range 95°C to 130°C, and having a branched structure and 0.5% titanium dioxide as a matting or dulling agent, both based on the weight of cellulose.
  • the fibre was washed and 0.25% soft finish based on the weight of fibre applied to it.
  • the fibre was then dried, and compressed in a stuffer box in the presence of dry steam so as to induce crimp in the fibre.
  • the conditions under which the fibre was crimped are shown in the following table and illustrated in the graph of Figure 5.
  • Stuffer box pressure (psig) Relative stuffer box pressure Mean crimp level (crimps per extended 10 cm) 8 1 25 20 2.5 35 26 3.3 40
  • the fibre was then cut to 38 mm staple length.
  • the fibre was carded on a Thibeau CA 11 card, 2.5 m wide and equipped with double doffing rollers.
  • the target basis weight for the carded web was 30 gsm.
  • the fibre of the invention could be stably crimped under higher pressures than the conventional fibre; and the level of crimp induced by a given pressure was higher for the fibre of the invention than for the conventional fibre.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
  • Multicomponent Fibers (AREA)
  • Nonwoven Fabrics (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)

Claims (23)

  1. Verfahren zur Herstellung von Lyocellfaser, bei dem man
    (i) eine Lösung von Cellulose in einem wäßrigen tertiären Amin-N-oxid als Lösungsmittel bei einer über der Umgebungstemperatur liegenden Temperatur herstellt, die 0,01 bis 30 Gewichtsprozent, bezogen auf das Gewicht der Cellulose, an Teilchen eines thermoplastischen Polymers mit einer unterhalb der Herstellungstemperatur der Lösung liegenden Glasübergangstemperatur dispergiert enthält,
    (ii) die Lösung über eine Düse in ein wäßriges Fällbad zu Lyocellfaser ausformt,
    (iii) die Faser von restlichem Amin-N-oxid freiwäscht und trocknet und
    (iv) die Faser kräuselt,
    dadurch gekennzeichnet, daß man beim Kräuseln der Faser darin 2,5 bis 8 Kräuselbögen/cm auslöst.
  2. Verfahren nach Anspruch 1, bei dem die Celluloselösung 0,01 bis 20 und bevorzugt 0,1 bis 10 Gewichtsprozent der Partikel des thermoplastischen Polymers enthält.
  3. Verfahren nach Anspruch 1 oder 2, bei dem das thermoplastische Polymer einen Schmelzpunkt von höher als 50°C, bevorzugt von höchstens 150°C und besonders bevorzugt zwischen 80 und 130°C aufweist.
  4. Verfahren nach einem der Ansprüche 1 bis 3, bei dem das thermoplastische Polymer eine Glasübergangstemperatur zwischen -20 und +130°C und bevorzugt zwischen 30 und 130°C aufweist.
  5. Verfahren nach einem der Ansprüche 1 bis 4, bei dem man das thermoplastische Polymer unter Polyestern, Polyamiden und Olefinpolymeren auswählt.
  6. Verfahren nach einem der Ansprüche 1 bis 5, bei dem sich das thermoplastische Polymer im ganzen Lyocell in Domänen verteilt, wobei die maximale Ausdehnung im wesentlichen aller Domänen höchstens 50 Nanometer (nm) beträgt.
  7. Verfahren nach einem der Ansprüche 1 bis 6, bei dem man die gewaschene Faser vor dem Kräuseln mit einem Weichgriffmittel aviviert, und zwar zweckmäßigerweise in einer Menge von 0,01 bis 2, bevorzugt 0,1 bis 0,5 und besonders bevorzugt 0,15 bis 0,4 Gewichtsprozent, bezogen auf das Gewicht der Faser.
  8. Verfahren nach einem der Ansprüche 1 bis 7, bei dem man in der Faser 3,5 bis 8 Kräuselbögen/cm auslöst.
  9. Verfahren nach einem der Ansprüche 1 bis 8, bei dem man der Lösung ein Spinnmattierungsmittel zusetzt.
  10. Verfahren nach einem der Ansprüche 1 bis 9, bei dem man die Faser nach dem Waschen und vor dem Trocknen mit einem Reagens mit zwei bis sechs gegenüber Cellulose reaktionsfähigen funktionellen Gruppen beaufschlagt, welches entweder vor oder bei dem Trocknen auf die Faser aufreagiert.
  11. Verfahren nach einem der Ansprüche 1 bis 10, bei dem man eine Faser mit einem Einzeltiter im Bereich von 0,5 bis 5 Dezitex und bevorzugt von 1 bis 3,5 Dezitex herstellt.
  12. Verfahren nach einem der Ansprüche 1 bis 11, bei dem man ferner die Faser zu einer Stapellänge im Bereich von 3 bis 100 mm und bevorzugt von 20 bis 75 mm zerschneidet.
  13. Verfahren nach Anspruch 12, bei dem man anschließend die Faser zu einem Kardenvlies bevorzugt mit einem Flächengewicht von 30 g/m2 verarbeitet, und zwar bevorzugt nach einem Verfahren, bei dem man die Faser auf der Kardiermaschine Thibeau CA 11 mit einer Vliesgeschwindigkeit im Bereich von 150 bis 275 Meter pro Minute bzw. auf einer wirkungsmäßig äquivalenten Maschine mit einer wirkungsmäßig äquivalenten Geschwindigkeit kardiert.
  14. Lyocellfaser mit einem darin verteilten 0,01 bis 30 gewichtsprozentigen Anteil, bezogen auf das Gewicht der Cellulose, an Partikeln eines thermoplastischen Polymers mit einem Schmelzpunkt von höher als 50°C bis 150°, dadurch gekennzeichnet, daß die Faser 2,5 bis 8 Kräuselbögen/cm aufweist.
  15. Lyocellfaser nach Anspruch 14, bei der der darin verteilte Anteil an Partikeln des thermoplastischen Polymers 0,01 bis 20 und bevorzugt 0,1 bis 10 Gewichtsprozent beträgt.
  16. Lyocellfaser nach Anspruch 14 oder 15, bei der der thermoplastische Polymer unter Polyestern, Polyamiden und Olefinpolymeren ausgewählt ist.
  17. Lyocellfaser nach einem der Ansprüche 14 bis 16, bei der die Faser als Naßfaser mit einem zwei bis sechs gegenüber Cellulose reaktionsfähige funktionelle Gruppen aufweisenden Reagens beaufschlagt wurde, welches entweder vor oder bei dem Trocknen darauf aufreagiert ist.
  18. Lyocellfaser nach einem der Ansprüche 14 bis 17, bei der das thermoplastische Polymer im ganzen Lyocell in Domänen verteilt ist, wobei die maximale Ausdehnung im wesentlichen aller Domänen höchstens 50 Nanometer (nm) beträgt.
  19. Lyocellfaser nach einem der Ansprüche 14 bis 18 mit einem darin verteilten Anteil an Titaniumdioxidteilchen von 0,1 bis 5, bevorzugt von 0,1 bis 2 und besonders bevorzugt von 0,2 bis 1 Gewichtsprozent, bezogen auf das Gewicht der Cellulose.
  20. Lyocellfaser nach einem der Ansprüche 14 bis 19 mit einem in einer Menge von 0,01 bis 2, bevorzugt von 0,1 bis 0,5 und besonders bevorzugt von 0,15 bis 0,4 Gewichtsprozent, bezogen auf das Gewicht der Faser, aufgebrachten Weichgriffmittel.
  21. Lyocellfaser nach einem der Ansprüche 15 bis 20, enthaltend 0,1 bis 30 Gewichtsprozent, bezogen auf das Gewicht der Cellulose, des unter Polyestern, Polyamiden und Olefinpolymeren ausgewählten thermoplastischen Polymers in Domänen, die im wesentlichen alle unter dem Elektronenmikroskop bei 9000facher Vergrößerung nicht erkennbar sind.
  22. Lyocellfaser nach einem der Ansprüche 15 bis 20, enthaltend 0,1 bis 30 Gewichtsprozent, bezogen auf das Gewicht der Cellulose, des unter Polyestern, Polyamiden und Olefinpolymeren ausgewählten thermoplastischen Polymers in Domänen, deren maximale Ausdehnung bei im wesentlichen allen Domänen höchstens 50 nm beträgt.
  23. Lyocellfaser nach Anspruch 21 oder Anspruch 22, bei der das thermoplastische Polymer in einem Anteil von 0,5 bis 10 und bevorzugt von 1 bis 5 Gewichtsprozent in der Faser enthalten ist.
EP01986728A 2000-10-12 2001-10-12 Gekräuselter faser und verfahren zu deren herstellung Expired - Lifetime EP1327013B1 (de)

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GB0025080A GB2368342A (en) 2000-10-12 2000-10-12 Lyocell fibre and its production
GB0025080 2000-10-12
PCT/GB2001/004562 WO2002031236A1 (en) 2000-10-12 2001-10-12 Fibre and its production

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EP1327013B1 true EP1327013B1 (de) 2007-01-10

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KR (1) KR100808724B1 (de)
CN (1) CN1214136C (de)
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DE (1) DE60125964T2 (de)
GB (1) GB2368342A (de)
WO (1) WO2002031236A1 (de)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020207767A1 (en) * 2019-04-10 2020-10-15 Lenzing Aktiengesellschaft Lyocell fiber tow, its manufacture and use
US11359309B2 (en) 2018-12-21 2022-06-14 Target Brands, Inc. Ring spun yarn and method

Families Citing this family (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
AT505511B1 (de) * 2007-07-11 2014-03-15 Chemiefaser Lenzing Ag Füllfaser mit verbessertem öffnungsverhalten, verfahren zu deren herstellung und deren verwendung
CN102317515B (zh) * 2007-08-31 2015-06-10 可隆工业株式会社 莱赛尔长纤的制备方法、莱赛尔长纤、轮胎帘线以及轮胎帘线的制备方法
KR200457862Y1 (ko) * 2009-09-10 2012-01-05 세원셀론텍(주) 연골 조직 채취기
KR101627768B1 (ko) * 2009-12-23 2016-06-08 코오롱인더스트리 주식회사 라이오셀 필라멘트 섬유의 제조방법, 라이오셀 필라멘트 섬유, 및 타이어 코오드
KR101455002B1 (ko) * 2013-06-28 2014-11-03 코오롱인더스트리 주식회사 담배필터용 라이오셀 소재 및 그 제조방법
KR102211219B1 (ko) 2014-06-30 2021-02-03 코오롱인더스트리 주식회사 담배필터용 이형단면 라이오셀 소재 및 그 제조방법
WO2016003145A1 (ko) * 2014-06-30 2016-01-07 코오롱인더스트리 주식회사 담배필터용 이형단면 라이오셀 소재 및 그 제조방법
WO2016052998A1 (ko) * 2014-09-30 2016-04-07 코오롱인더스트리 주식회사 라이오셀 크림프 섬유
KR102211186B1 (ko) * 2014-12-31 2021-02-03 코오롱인더스트리 주식회사 담배필터용 라이오셀 소재 및 그 제조방법
CN105200670B (zh) * 2015-08-17 2017-08-01 赖明荣 一种耐低温无纺布
EP3467174A1 (de) * 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Gewirktes endlosfilamentlyocellgewebe
EP3868929A1 (de) * 2018-01-15 2021-08-25 Lenzing Aktiengesellschaft Formkörper der in cellulose inkorporiertes elastan aufweist und herstellungsverfahren
TWI814782B (zh) * 2018-03-06 2023-09-11 奧地利商蘭仁股份有限公司 溶劑紡絲之纖維素纖維
WO2021199497A1 (ja) * 2020-03-30 2021-10-07 日東紡績株式会社 ガラスダイレクトロービング、及び、ガラス長繊維強化熱可塑性樹脂ペレット
CN115559007B (zh) * 2022-09-23 2024-04-12 当阳市鸿阳新材料科技有限公司 一种消光莱赛尔纤维及其生产方法

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2008126A (en) * 1977-10-13 1979-05-31 Courtaulds Ltd Regenerated cellulose filaments
AT384628B (de) * 1982-05-17 1987-12-10 Chemiefaser Lenzing Ag Cellulosefasern, insbesondere fuer die herstellung von vliesen und verfahren zur herstellung der fasern
MY131648A (en) * 1993-05-24 2007-08-30 Courtaulds Fibres Holdings Ltd Manufacture of crimped solvent-spun cellulose fibre
GB9407496D0 (en) * 1994-04-15 1994-06-08 Courtaulds Fibres Holdings Ltd Fibre treatment
JPH08170224A (ja) * 1994-12-20 1996-07-02 Kuraray Co Ltd 分散染料に可染性の有機溶剤系セルロース繊維及びその製法
JPH09302520A (ja) * 1996-05-14 1997-11-25 Kuraray Co Ltd 易フィブリル化繊維の製造方法
GB2324064A (en) * 1997-04-11 1998-10-14 Courtaulds Fibres Modified lyocell fibre and method of its formation

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11359309B2 (en) 2018-12-21 2022-06-14 Target Brands, Inc. Ring spun yarn and method
US11767618B2 (en) 2018-12-21 2023-09-26 Target Brands, Inc. Ring spun yarn and method
WO2020207767A1 (en) * 2019-04-10 2020-10-15 Lenzing Aktiengesellschaft Lyocell fiber tow, its manufacture and use

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CN1214136C (zh) 2005-08-10
GB0025080D0 (en) 2000-11-29
DE60125964D1 (de) 2007-02-22
EP1327013A1 (de) 2003-07-16
WO2002031236A1 (en) 2002-04-18
AU2001294030A1 (en) 2002-04-22
DE60125964T2 (de) 2007-10-18
GB2368342A (en) 2002-05-01
CN1469943A (zh) 2004-01-21
KR100808724B1 (ko) 2008-02-29
KR20030061374A (ko) 2003-07-18

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