EP1044293B1 - Multifilament textile yarns with hollow section, method for making same, and textile surfaces obtained from said yarns - Google Patents

Multifilament textile yarns with hollow section, method for making same, and textile surfaces obtained from said yarns Download PDF

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Publication number
EP1044293B1
EP1044293B1 EP98963617A EP98963617A EP1044293B1 EP 1044293 B1 EP1044293 B1 EP 1044293B1 EP 98963617 A EP98963617 A EP 98963617A EP 98963617 A EP98963617 A EP 98963617A EP 1044293 B1 EP1044293 B1 EP 1044293B1
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EP
European Patent Office
Prior art keywords
yarn
section
filaments
polyamide
cross
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Expired - Lifetime
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EP98963617A
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German (de)
French (fr)
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EP1044293A1 (en
Inventor
Vincent Pellerin
Walter Roggenstein
Uwe Schaffner
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Nylstar SA France
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Nylstar SA France
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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
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
    • 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
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
    • Y10T428/264—Up to 3 mils
    • Y10T428/265—1 mil or less
    • 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
    • Y10T428/2933—Coated or with bond, impregnation or core
    • Y10T428/2964—Artificial fiber or filament
    • Y10T428/2967—Synthetic resin or polymer
    • Y10T428/2969—Polyamide, polyimide or polyester
    • 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
    • Y10T428/2973—Particular cross section
    • Y10T428/2975—Tubular or cellular

Definitions

  • the present invention relates to a multifilament textile yarn, the filaments or strands have a hollow section, a method of making this hollow wire, and the surfaces textiles obtained with such a yarn.
  • It relates more particularly to the manufacture of multifilament yarns comprising hollow filaments obtained by melt spinning of a composition in polyamide.
  • This patent describes the manufacture of polyamide 6 filaments obtained at a speed 700 m / min. The filaments are then subjected to stretching to obtain the desired title.
  • the spinning speed is very low compared to the process speeds current industrialists who are often above 3000 m / min.
  • the stretching step is often integrated into the spinning, without rework filament intermediate.
  • One of the aims of the present invention is to provide a multifilament textile yarn whose strands have a hollow section obtained by a spinning or spinning-drawing process which has the advantages of current industrial processes for spinning filaments with a full section, namely productivity. and regularity of the properties of the yarn by using a polyamide of V R similar to that of the polyamides used in the manufacture of textile yarns.
  • the invention provides a multifilament textile yarn of polyamide of title strand less than 10 dtex, and whose strands have a hollow section comprising a central empty area representing at least 5% of the total section area transverse of said strand, characterized in that the wire has a USTER coefficient (U%) less than 3% and a number of strands with cross-section in the shape of an arc of a circle less than 30% of the total number of hollow section strands.
  • U% USTER coefficient
  • hollow section strand must be understood all the strands or filaments obtained at from a die hole in the shape of an arc of a circle as will be described below.
  • the hollow strands are those whose cross section is shaped closed or open crown.
  • the multifilament yarn has a U% of less than 2%, preferably less than 1%.
  • the number of filaments in the shape of an arc of a circle is advantageously less than 20% of the total number of hollow section filaments, preferably less than 10%.
  • U% or USTER coefficient is representative of the regularity of a thread continued. Thus, this coefficient is determined by measuring the variations in the titer of a thread continuous on a USTER device (Zellweger).
  • the wire kept under a certain tension passes at a constant speed between the plates of a capacitor, the variation of the element dielectric formed by the wire due to the variation in mass of the wire causes a variation in capacitance of the capacitor which is translated into irregularity in the title of the wire.
  • the percentage of empty area in the section of filaments or strands is greater than 10%, preferably greater than 15% of the cross section of each strand.
  • this value is between 15 and 50%.
  • the multifilament yarn is obtained by spinning from a die of a polyamide-based composition having a relative viscosity V R greater than 40 and preferably between 40 and 55, advantageously between 40 and 50.
  • the relative viscosity V R of the polyamide is determined on an 8.4% solution of polymer in formic acid.
  • the polyamide suitable for the invention is chosen from the group comprising advantageously, polyamide 6, polyamide 66, mixtures of polyamides comprising at least 80% by weight of polyamide 66 or polyamide 6, the copolyamides comprising at least 80% by number of polyamide 66 or polyamide 6 units.
  • the yarn of the invention has excellent regularity, and the absence of filaments open or cross-sectional, i.e. not coalescing at the exit from die, avoids breakage and jamming problems in downstream treatments yarn such as texturing, dyeing, weaving or knitting, for example, as well as irregularities on textile surfaces.
  • the invention also relates to a method for manufacturing a wire. multifilament having the characteristics indicated above.
  • the process for manufacturing a polyamide multifilament yarn comprising filaments of hollow section consists in extruding a composition polyamide through at least one die comprising several die holes for forming filaments or strands, to converge at least a portion of said strands into a distant point of the die to form said multifilament thread, then return said thread to a coil characterized in that each die hole is constituted by a slot in shape of a circular arc whose ends are distant by a length at most equal to 5 times the average width of said slot opening at the exit face of the die, with cooling of the filaments at the outlet of the die and with a speed of wire winding greater than 3000 m / min., preferably greater than 3500 m / min.
  • the width of the slot forming a die hole on the die exit surface is advantageously between 0.05 mm and 0.12 mm.
  • the ends of the arc of a circle forming each die hole are symmetrical over at least 5% of the total length of said circular arc, preferably over at least 15% of this total length.
  • the channels are produced according to the usual techniques such as by EDM
  • the density of holes on a die is between 0.25 hole / cm 2 and 3 holes / cm 2 .
  • the wire leaving the die is cooled.
  • the distance from the start of cooling and the exit from the die is as short as possible technologically. So a cooling immediately at the outlet of the die can be difficult to implement because it can cause deposits of polymer on the surface of the die which have for consequently a break in the filaments.
  • the cooling is obtained by a cooling fluid chosen from the group comprising air, a non-oxidizing gas, or an inert gas such as nitrogen.
  • this fluid is not saturated with water vapor.
  • the cooling fluid is air or an inert gas.
  • the methods of treating the wires thus formed are those usually used for the production of polyamide textile threads.
  • sizes to improve the surface lubrication, modify its hydrophilic or hydrophobic properties can be applied.
  • these threads are subjected to a drawing either cold or hot, in the presence of water vapor or not.
  • This stretching is generally integrated into the process of spinning, that is to say made before the rewinding.
  • the strands can also be drawn in an independent drawing process spinning, by taking up the returned thread.
  • the polyamide yarn can then be relaxed before rewinding on a spool.
  • the multifilament yarns of the invention can be subjected to crimping, texturing according to the field of use.
  • these threads can be used as flat thread, twisted or textured thread, in the weaving processes such as warp or weft thread, for example.
  • the yarns of the invention are also used for the manufacture of surfaces knitted. Such textile surfaces woven or knitted with at least one thread of the invention are also objects of the invention.
  • the yarns according to the invention are obtained by spinning a composition comprising a polyamide PA 66 with a relative viscosity VR equal to 49 and a matting agent consisting with titanium oxide at a concentration by weight of 0.3%.
  • This composition is fed into a conventional spinning device comprising a die suitable for spinning hollow wire.
  • the die comprises 40 die holes (hole density equal to 0.8 hole / cm 2 ) having a profile 1 in an arc of an outside diameter equal to 1.5 mm.
  • the ends 1a, 1b of the arc of a circle are separated by a distance e equal to 0.15 mm.
  • the width I of the slot is regular in the example illustrated and is equal to 0.08 mm. However, this width may be different over the length of the slot without thereby departing from the scope of the invention and while respecting the characteristic of symmetry of the end parts of the slot as defined above.
  • the filament bundle is cooled at the outlet of the die by a flow of cooling supplied in a direction substantially perpendicular to the direction beam travel.
  • This power supply is placed at a distance of 30 mm from the die exit surface.
  • the coolant is air at a temperature of 22 ° C.
  • the flow of coolant is fed at a speed which does not cause disturbance in the scrolling of the bundle of filaments.
  • the filaments are then converged at a point 130 cm from the outlet of the sector.
  • a sizing composition is deposited on the yarn thus formed according to conventional methods and devices.
  • the wire is then wound up on a spool at a winding speed equal to 4500 m / min.
  • the yarn obtained has a total titer of 165 dtex and comprises 40 filaments (thread title 165F40).
  • FIG. 2 representing a cross-sectional view of the wire obtained shows the hollow crown-shaped section of the filaments.
  • the percentage of vacuum is more than 15%.
  • the number of filaments with a cross-section, i.e. whose ends have not coalesced at the outlet of the die is equal to zero in the illustrated example.
  • a fabric was produced with threads obtained by the process described above and 165F40.
  • the fabric is made on a lance loom and is subjected to a calendar.
  • the yarns according to the invention are obtained by spinning in a drawing and drawing process Integrated, of a composition comprising a polyamide PA 6 of relative viscosity VR equal to 50 and a matting agent consisting of titanium oxide at a concentration 0.4% by weight.
  • This composition is fed into a conventional spinning device comprising a die suitable for spinning hollow wire identical to that used in Example 1, but having 20 holes per die.
  • the filament bundle is cooled at the outlet of the die by a flow of cooling supplied in a direction substantially perpendicular to the direction beam travel.
  • This power supply is placed at a distance of 40 mm from the die exit surface.
  • the coolant is air at a temperature of 20 ° C.
  • the flow of coolant is fed at a speed which does not cause disturbance in the scrolling of the bundle of filaments.
  • the filaments are then converged at a point 130 cm from the outlet of the sector.
  • a sizing composition is deposited on the yarn thus formed according to conventional methods and devices.
  • the wire is then wound up on a spool at a winding speed equal to 4500 m / min.
  • the yarn obtained has a total titer of 78 dtex and includes 20 filaments (thread title 78F20).
  • the yarn obtained has a percentage of void greater than 15%.
  • Number of filaments with an arcuate section, i.e. the ends of which do not have coalesced at the outlet of the die is equal to zero.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Artificial Filaments (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Woven Fabrics (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Knitting Of Fabric (AREA)

Abstract

The invention concerns a multifilament textile yarn whereof the filaments or staples have a hollow section, a method for making said hollow yarn, and textile surfaces obtained from said yarns. More particularly, it concerns a method for making multifilament yarns comprising hollow filaments obtained by melt-drawing of a polyamide composition having a yarn count less than 10 dtex for each staple and whereof the staples with hollow section have a central hollow surface representing at least 5% of the total surface in said staple transfer section. The invention is characterized in that the yarn has an USTER coefficient (U %) less than 3% and a number of staple with arc-shaped section less than 30% of the total number of staples with hollow section. The flat yarns, twisted and textured are used in particular for mixing textile surfaces, such as woven or knitted fabric.

Description

La présente invention concerne un fil textile multifilamentaire dont les filaments ou brins ont une section creuse, un procédé de fabrication de ce fil creux, et les surfaces textiles obtenues avec un tel fil.The present invention relates to a multifilament textile yarn, the filaments or strands have a hollow section, a method of making this hollow wire, and the surfaces textiles obtained with such a yarn.

Elle concerne plus particulièrement la fabrication de fils multifilamentaires comprenant des filaments creux obtenus par filage en fondu d'une composition en polyamide.It relates more particularly to the manufacture of multifilament yarns comprising hollow filaments obtained by melt spinning of a composition in polyamide.

L'utilisation de fil textile creux dans la réalisation de surfaces textiles est recherchée depuis très longtemps pour réaliser des vêtements plus légers et plus isolants thermiquement. Toutefois, la fabrication de filaments comprenant un volume de creux important et présentant une bonne régularité s'est avérée très difficile, notamment à des vitesses de filage et des titres de filament compatibles avec une fabrication industrielle et convenables notamment pour les applications textiles.The use of hollow textile yarn in the production of textile surfaces is sought after for a very long time to make lighter and more thermally insulating. However, the manufacture of filaments comprising a volume of large hollow with good regularity has proven to be very difficult, in particular at spinning speeds and filament titles compatible with manufacturing industrial and particularly suitable for textile applications.

Il a été proposé en 1956, un procédé de fabrication d'un fil creux en polyamide. Ce procédé est décrit dans le brevet GB 843 179. Il consiste à filer le polyamide dans une filière comprenant des trous de filière en forme d'un seul arc de cercle, les extrémités dudit arc étant séparées par une distance comprise entre 0,05 et 0,3 mm.In 1956, a method for manufacturing a hollow polyamide wire was proposed. This process is described in patent GB 843 179. It consists in spinning the polyamide in a die comprising die holes in the form of a single arc of a circle, the ends of said arc being separated by a distance of between 0.05 and 0.3 mm.

Ce brevet décrit la fabrication de filaments en polyamide 6 obtenus à une vitesse de filage de 700 m/min. Les filaments sont ensuite soumis à un étirage pour obtenir le titre désiré.This patent describes the manufacture of polyamide 6 filaments obtained at a speed 700 m / min. The filaments are then subjected to stretching to obtain the desired title.

La vitesse de filage est très faible par rapport aux vitesses des procédés industriels actuels qui sont souvent supérieures à 3000 m/min. En outre, dans les procédés actuels, l'étape d'étirage est souvent intégrée au filage, sans reprise intermédiaire des filaments.The spinning speed is very low compared to the process speeds current industrialists who are often above 3000 m / min. In addition, within current processes, the stretching step is often integrated into the spinning, without rework filament intermediate.

Il a également été proposé dans la demande de brevet WO 95/25188 un procédé d'obtention de filaments polyamide à section creuse par un procédé de filage à vitesse élevée (supérieure à 1500 m/min.). Toutefois, ce procédé requiert le filage d'un polyamide de viscosité élevée (VR supérieure à 50 et de préférence supérieure à 60). Une telle viscosité est élevée par rapport à celle des polyamides employés pour la fabrication des fils textiles classiques qui est généralement inférieure à 50. Ce document précise que la réalisation de filaments creux selon le procédé décrit est impossible avec un polyamide de VR inférieur à 50. Ainsi, le procédé décrit dans ce document nécessite une étape supplémentaire pour accroítre la viscosité du polyamide, par exemple par post condensation ou utilisation de catalyseurs. La filière utilisée dans ce document comprend des trous de filières constitués par plusieurs arcs de cercle (au moins 2) dont les extrémités sont distantes d'une faible longueur.There has also been proposed in patent application WO 95/25188 a process for obtaining polyamide filaments with a hollow section by a spinning process at high speed (greater than 1500 m / min.). However, this process requires the spinning of a polyamide of high viscosity (V R greater than 50 and preferably greater than 60). Such a viscosity is high compared to that of the polyamides used for the manufacture of conventional textile yarns which is generally less than 50. This document specifies that the production of hollow filaments according to the method described is impossible with a polyamide of V R less than 50 Thus, the process described in this document requires an additional step to increase the viscosity of the polyamide, for example by post-condensation or the use of catalysts. The die used in this document comprises die holes constituted by several arcs of a circle (at least 2) whose ends are distant a short length.

Un des buts de la présente invention est de proposer un fil textile multifilamentaire dont les brins ont une section creuse obtenu par un procédé de filage ou filage-étirage qui présente les avantages des procédés industriels actuels de filage des filaments à section pleine, à savoir productivité et régularité des propriétés du fil par utilisation d'un polyamide de VR semblable à celle des polyamides utilisés dans la fabrication des fils textiles.One of the aims of the present invention is to provide a multifilament textile yarn whose strands have a hollow section obtained by a spinning or spinning-drawing process which has the advantages of current industrial processes for spinning filaments with a full section, namely productivity. and regularity of the properties of the yarn by using a polyamide of V R similar to that of the polyamides used in the manufacture of textile yarns.

A cet effet, l'invention propose un fil textile multifilamentaire en polyamide de titre au brin inférieur à 10 dtex, et dont les brins ont une section creuse comprenant une surface vide centrale représentant au moins 5 % de la surface totale de la section transversale dudit brin, caractérisé en ce que le fil possède un USTER coefficient (U %) inférieur à 3 % et un nombre de brin à section en forme d'arc de cercle inférieur à 30 % du nombre total des brins à section creuse.To this end, the invention provides a multifilament textile yarn of polyamide of title strand less than 10 dtex, and whose strands have a hollow section comprising a central empty area representing at least 5% of the total section area transverse of said strand, characterized in that the wire has a USTER coefficient (U%) less than 3% and a number of strands with cross-section in the shape of an arc of a circle less than 30% of the total number of hollow section strands.

Par brin à section creuse il faut comprendre tous les brins ou filaments obtenus à partir d'un trou de filière en forme d'arc de cercle comme cela sera décrit ci-dessous. En d'autres termes, les brins creux sont ceux dont la section transversale est en forme de couronne fermée ou ouverte.By hollow section strand must be understood all the strands or filaments obtained at from a die hole in the shape of an arc of a circle as will be described below. In other words, the hollow strands are those whose cross section is shaped closed or open crown.

Selon l'invention le fil multifilamentaire présente un U % inférieur à 2 %, de préférence inférieur à 1%.According to the invention, the multifilament yarn has a U% of less than 2%, preferably less than 1%.

En outre, le nombre de filament en forme d'arc de cercle est avantageusement inférieur à 20 % du nombre total de filaments à section creuse, de préférence inférieur à 10%.In addition, the number of filaments in the shape of an arc of a circle is advantageously less than 20% of the total number of hollow section filaments, preferably less than 10%.

Le terme U % ou USTER coefficient est représentatif de la régularité d'un fil continu. Ainsi, ce coefficient est déterminé par la mesure des variations du titre d'un fil continu sur un appareil USTER (Zellweger).The term U% or USTER coefficient is representative of the regularity of a thread continued. Thus, this coefficient is determined by measuring the variations in the titer of a thread continuous on a USTER device (Zellweger).

Pour réaliser cette mesure le fil maintenu sous une certaine tension défile à une vitesse constante entre les plaques d'un condensateur, la variation de l'élément diélectrique formé par le fil due à la variation de masse du fil provoque une variation de capacité du condensateur qui est traduite en irrégularité de titre du fil.To carry out this measurement, the wire kept under a certain tension passes at a constant speed between the plates of a capacitor, the variation of the element dielectric formed by the wire due to the variation in mass of the wire causes a variation in capacitance of the capacitor which is translated into irregularity in the title of the wire.

Un graphique représentant les irrégularités du titre ou variation de masse le long du fil est tracé, le coefficient USTER (U%) représentant la variation moyenne de masse exprimée en % de masse moyenne.A graph representing title irregularities or mass variation along of the wire is drawn, the coefficient USTER (U%) representing the average variation in mass expressed as% of average mass.

Selon une autre caractéristique préférentielle de l'invention, le pourcentage de surface vide dans la section des filaments ou brins est supérieur à 10 %, de préférence supérieur à 15 % de la section transversale de chaque brin. Avantageusement cette valeur est comprise entre 15 et 50 %. According to another preferred characteristic of the invention, the percentage of empty area in the section of filaments or strands is greater than 10%, preferably greater than 15% of the cross section of each strand. Advantageously this value is between 15 and 50%.

Selon une autre caractéristique de l'invention, le fil multifilamentaire est obtenu par filage à partir d'une filière d'une composition à base de polyamide présentant une viscosité relative VR supérieure à 40 et de préférence comprise entre 40 et 55, avantageusement entre 40 et 50.According to another characteristic of the invention, the multifilament yarn is obtained by spinning from a die of a polyamide-based composition having a relative viscosity V R greater than 40 and preferably between 40 and 55, advantageously between 40 and 50.

La viscosité relative VR du polyamide est déterminée sur une solution à 8,4 % de polymère dans de l'acide formique.The relative viscosity V R of the polyamide is determined on an 8.4% solution of polymer in formic acid.

Le polyamide convenable pour l'invention est choisi dans le groupe comprenant avantageusement, le polyamide 6, le polyamide 66, les mélanges de polyamides comprenant au moins 80 % en poids de polyamide 66 ou polyamide 6, les copolyamides comprenant au moins 80 % en nombre d'unités polyamide 66 ou polyamide 6.The polyamide suitable for the invention is chosen from the group comprising advantageously, polyamide 6, polyamide 66, mixtures of polyamides comprising at least 80% by weight of polyamide 66 or polyamide 6, the copolyamides comprising at least 80% by number of polyamide 66 or polyamide 6 units.

Le fil de l'invention présente une excellente régularité, et l'absence de filaments ouverts ou à section en forme d'arc de cercle, c'est-à-dire qui n'ont pas coalescé à la sortie de filière, évite les problèmes de casse et bourrage dans les traitements avals du fil tels que la texturation, la teinture, le tissage ou tricotage, par exemple, ainsi que les irrégularités sur les surfaces textiles.The yarn of the invention has excellent regularity, and the absence of filaments open or cross-sectional, i.e. not coalescing at the exit from die, avoids breakage and jamming problems in downstream treatments yarn such as texturing, dyeing, weaving or knitting, for example, as well as irregularities on textile surfaces.

L'invention a également pour objet un procédé de fabrication d'un fil multifilamentaire possédant les caractéristiques indiquées précédemment.The invention also relates to a method for manufacturing a wire. multifilament having the characteristics indicated above.

Selon l'invention, le procédé de fabrication d'un fil multifilamentaire en polyamide comprenant des filaments de section creuse consiste à extruder une composition polyamide à travers au moins une filière comprenant plusieurs trous de filière pour former des filaments ou brins, à faire converger au moins une partie desdits brins en un point distant de la filière pour former ledit fil multifilamentaire, puis renvider le dit fil sur une bobine caractérisé en ce que chaque trou de filière est constitué par une fente en forme d'arc de cercle dont les extrémités sont distantes d'une longueur au plus égale à 5 fois la largeur moyenne de ladite fente débouchant à la face de sortie de la filière, avec refroidissement des filaments à la sortie de la filière et avec une vitesse de renvidement du fil supérieure à 3000 m/min., de préférence supérieure à 3500 m/min.According to the invention, the process for manufacturing a polyamide multifilament yarn comprising filaments of hollow section consists in extruding a composition polyamide through at least one die comprising several die holes for forming filaments or strands, to converge at least a portion of said strands into a distant point of the die to form said multifilament thread, then return said thread to a coil characterized in that each die hole is constituted by a slot in shape of a circular arc whose ends are distant by a length at most equal to 5 times the average width of said slot opening at the exit face of the die, with cooling of the filaments at the outlet of the die and with a speed of wire winding greater than 3000 m / min., preferably greater than 3500 m / min.

Selon une autre caractéristique de l'invention, la largeur de la fente formant un trou de filière sur la surface de sortie de la filière est avantageusement comprise entre 0,05 mm et 0,12 mm.According to another characteristic of the invention, the width of the slot forming a die hole on the die exit surface is advantageously between 0.05 mm and 0.12 mm.

Selon une nouvelle caractéristique de l'invention, les extrémités de l'arc de cercle formant chaque trou de filière sont symétriques sur au moins 5 % de la longueur totale dudit arc de cercle, de préférence sur au moins 15% de cette longueur totale.According to a new characteristic of the invention, the ends of the arc of a circle forming each die hole are symmetrical over at least 5% of the total length of said circular arc, preferably over at least 15% of this total length.

Les filières sont réalisées selon les techniques habituelles telles que par électroérosionThe channels are produced according to the usual techniques such as by EDM

Avantageusement, la densité de trous sur une filière est comprise entre 0,25 trou/cm2 et 3 trous/cm2. Advantageously, the density of holes on a die is between 0.25 hole / cm 2 and 3 holes / cm 2 .

Le fil en sortie de filière est refroidi. La distance entre le début du refroidissement et la sortie de la filière est la plus courte possible technologiquement. Ainsi, un refroidissement immédiatement en sortie de filière peut être difficile à mettre en oeuvre car il peut provoquer des dépôts de polymère sur la surface de la filière qui ont pour conséquence une casse des filaments.The wire leaving the die is cooled. The distance from the start of cooling and the exit from the die is as short as possible technologically. So a cooling immediately at the outlet of the die can be difficult to implement because it can cause deposits of polymer on the surface of the die which have for consequently a break in the filaments.

Selon l'invention, le refroidissement est obtenue par un fluide de refroidissement choisi dans le groupe comprenant l'air, un gaz non oxydant, ou un gaz inerte comme l'azote. De préférence, ce fluide n'est pas saturé en vapeur d'eau.According to the invention, the cooling is obtained by a cooling fluid chosen from the group comprising air, a non-oxidizing gas, or an inert gas such as nitrogen. Preferably, this fluid is not saturated with water vapor.

Dans un mode de réalisation préféré de l'invention, le fluide de refroidissement est de l'air ou un gaz inerte.In a preferred embodiment of the invention, the cooling fluid is air or an inert gas.

Les procédés de traitement des fils ainsi formés sont ceux usuellement utilisés pour la fabrication des fils textiles polyamides. Ainsi, des ensimages pour améliorer la lubrification de surface, modifier les propriétés hydrophiles ou hydrophobes de celle-ci peuvent être appliqués.The methods of treating the wires thus formed are those usually used for the production of polyamide textile threads. Thus, sizes to improve the surface lubrication, modify its hydrophilic or hydrophobic properties can be applied.

Généralement ces fils sont soumis à un étirage soit à froid soit à chaud, en présence de vapeur d'eau ou non. Cet étirage est généralement intégré au procédé de filage, c'est-à-dire réalisé avant le renvidement. Toutefois, sans sortir du cadre de l'invention, les fils peuvent également être étirés dans un procédé d'étirage indépendant du filage, par reprise du fil renvidé.Generally these threads are subjected to a drawing either cold or hot, in the presence of water vapor or not. This stretching is generally integrated into the process of spinning, that is to say made before the rewinding. However, without going beyond the ambit of the invention, the strands can also be drawn in an independent drawing process spinning, by taking up the returned thread.

On peut réaliser également un entremêlement des filaments pour améliorer la cohésion du fil. Cet entremêlement est souvent mis en oeuvre avant l'étirage, mais peut être fait pendant ou après celui-ci.It is also possible to intertwine the filaments to improve the cohesion of the wire. This intermingling is often done before stretching, but can be done during or after it.

Le fil polyamide peut être ensuite relaxé avant le renvidage sur une bobine.The polyamide yarn can then be relaxed before rewinding on a spool.

Les fils multifilamentaires de l'invention peuvent être soumis à un frisage, une texturation selon le domaine d'utilisation.The multifilament yarns of the invention can be subjected to crimping, texturing according to the field of use.

Ainsi, ces fils peuvent être utilisés comme fil plat, fil retordu ou texturé, dans les procédés de tissage comme fil de chaíne ou fil de trame, par exemple.Thus, these threads can be used as flat thread, twisted or textured thread, in the weaving processes such as warp or weft thread, for example.

Les fils de l'invention sont également utilisés pour la fabrication de surfaces tricotées. De telles surfaces textiles tissées ou tricotées avec au moins un fil de l'invention sont également des objets de l'invention.The yarns of the invention are also used for the manufacture of surfaces knitted. Such textile surfaces woven or knitted with at least one thread of the invention are also objects of the invention.

D'autres détails, avantages de l'invention apparaítront plus clairement au vu de la description détaillée d'au moins un exemple de réalisation, donné à titre indicatif uniquement et faite en référence aux dessins annexés dans lesquels :

  • la figure 1 représente une vue schématique de la forme d'un trou de filière conforme à la présente invention, et
  • la figure 2 est une vue photographique en coupe d'un fil multifilamentaire conforme à l'invention.
Other details, advantages of the invention will appear more clearly in the light of the detailed description of at least one embodiment, given for information only and with reference to the appended drawings in which:
  • FIG. 1 represents a schematic view of the shape of a die hole according to the present invention, and
  • Figure 2 is a photographic sectional view of a multifilament yarn according to the invention.

EXEMPLE 1EXAMPLE 1

Les fils selon l'invention sont obtenus par filage d'une composition comprenant un polyamide PA 66 de viscosité relative VR égale à 49 et un agent matifiant constitué par de l'oxyde de titane à une concentration pondérale de 0,3%.The yarns according to the invention are obtained by spinning a composition comprising a polyamide PA 66 with a relative viscosity VR equal to 49 and a matting agent consisting with titanium oxide at a concentration by weight of 0.3%.

Cette composition est alimentée dans un dispositif de filage conventionnel comprenant une filière adaptée pour le filage de fil creux.This composition is fed into a conventional spinning device comprising a die suitable for spinning hollow wire.

Ainsi, en référence à la figure 1 la filière comprend 40 trous de filière (densité de trous égale à 0,8 trou/cm2) présentant un profil 1 en arc de cercle de diamètre extérieur égal à 1,5 mm. Les extrémités 1a, 1b de l'arc de cercle sont séparées par une distance e égale à 0,15 mm. La largeur I de la fente est régulière dans l'exemple illustré et est égale à 0,08 mm. Toutefois, cette largeur peut être différente sur la longueur de la fente sans pour cela sortir du cadre de l'invention et en respectant la caractéristique de symétrie des parties extrêmes de la fente telle que définie précédemment.Thus, with reference to FIG. 1, the die comprises 40 die holes (hole density equal to 0.8 hole / cm 2 ) having a profile 1 in an arc of an outside diameter equal to 1.5 mm. The ends 1a, 1b of the arc of a circle are separated by a distance e equal to 0.15 mm. The width I of the slot is regular in the example illustrated and is equal to 0.08 mm. However, this width may be different over the length of the slot without thereby departing from the scope of the invention and while respecting the characteristic of symmetry of the end parts of the slot as defined above.

Les conditions de filage sont les suivantes :

  • pression : 250 bar
  • température : 280°C
  • débit de polymère :2,3 g/min/trou
The spinning conditions are as follows:
  • pressure: 250 bar
  • temperature: 280 ° C
  • polymer flow: 2.3 g / min / hole

Le faisceau de filaments est refroidi en sortie de filière par un flux de fluide de refroidissement alimenté selon une direction sensiblement perpendiculaire à la direction de défilement du faisceau. Cette alimentation est disposée à une distance de 30 mm de la surface de sortie de la filière. Dans l'exemple illustré, le fluide de refroidissement est de l'air à une température de 22°C. Bien entendu, le flux de fluide de refroidissement est alimenté selon une vitesse qui ne provoque pas de perturbation dans le défilement du faisceau de filaments.The filament bundle is cooled at the outlet of the die by a flow of cooling supplied in a direction substantially perpendicular to the direction beam travel. This power supply is placed at a distance of 30 mm from the die exit surface. In the example illustrated, the coolant is air at a temperature of 22 ° C. Of course, the flow of coolant is fed at a speed which does not cause disturbance in the scrolling of the bundle of filaments.

Les filaments sont ensuite convergés en un point distant de 130 cm de la sortie de la filière. Une composition d'ensimage est déposée sur le fil ainsi formé selon des procédés et dispositifs conventionnels.The filaments are then converged at a point 130 cm from the outlet of the sector. A sizing composition is deposited on the yarn thus formed according to conventional methods and devices.

Le fil est ensuite renvidé sur une bobine à une vitesse de renvidage égale à 4500 m/min.The wire is then wound up on a spool at a winding speed equal to 4500 m / min.

Le fil obtenu a un titre total de 165 dtex et comprend 40 filaments (titre du fil 165F40).The yarn obtained has a total titer of 165 dtex and comprises 40 filaments (thread title 165F40).

La figure 2 représentant une vue de coupe transversale du fil obtenu montre la section creuse en forme de couronne des filaments. Le pourcentage de vide est supérieur à 15%. Le nombre de filaments à section en forme d'arc de cercle, c'est à dire dont les extrémités n'ont pas coalescé à la sortie de la filière est égal à zéro dans l'exemple illustré. FIG. 2 representing a cross-sectional view of the wire obtained shows the hollow crown-shaped section of the filaments. The percentage of vacuum is more than 15%. The number of filaments with a cross-section, i.e. whose ends have not coalesced at the outlet of the die is equal to zero in the illustrated example.

Les caractéristiques du fil obtenu sont les suivantes :

  • USTER coefficient (U %) : 0,9 (valeur déterminée par intégration)
  • Allongement à la rupture : 45%
  • Ténacité : 35 cN/Tex
  • REB : 10% (Retrait à l'eau bouillante)
  • Facteur de cohésion (déterminé par la méthode manuelle au crochet) : 15 noeuds/m
The characteristics of the wire obtained are as follows:
  • USTER coefficient (U%): 0.9 (value determined by integration)
  • Elongation at break: 45%
  • Tenacity: 35 cN / Tex
  • R EB : 10% (Withdrawal with boiling water)
  • Cohesion factor (determined by manual crochet method): 15 knots / m

Un tissu a été réalisé avec des fils obtenus par le procédé décrit précédemment et de titre 165F40. Le tissu est réalisé sur un métier à lance et est soumis à un calendrage.A fabric was produced with threads obtained by the process described above and 165F40. The fabric is made on a lance loom and is subjected to a calendar.

Un tissu identique a été réalisé avec un fil classique à section ronde et pleine. Le titre des fils de chaíne et trame est 235F34.An identical fabric was produced with a classic wire with a round and solid section. The title of the warp and weft threads is 235F34.

Les propriétés de ces deux tissus sont rassemblées dans le tableau ci-dessous : Caractéristiques Tissu avec fils de l'invention Tissu avec fils à section pleine    Grammage (g/m2) 95 136 Perméabilité à l'air (l/m2/s) Pression : 100 Pa 79,8 72,9 Pression : 160 Pa 114 111 Propriétés thermiques ΔT = 10 °K G = 200 g Epaisseur (mm) 0,1872 0,1456 Coefficient résistance thermique (K.m2/W) 0,00638 0,00606 Coefficient de conductivité (W/m2K) 0,02834 0,0241 The properties of these two fabrics are gathered in the table below: Characteristics Fabric with yarns of the invention Full section yarn fabric Weight (g / m 2 ) 95 136 Air permeability (l / m 2 / s) Pressure: 100 Pa 79.8 72.9 Pressure: 160 Pa 114 111 Thermal properties ΔT = 10 ° KG = 200 g Thickness (mm) 0.1872 0.1456 Thermal resistance coefficient (Km 2 / W) 0.00638 0.00606 Conductivity coefficient (W / m 2 K) 0.02834 0.0241

Ces essais ont été mesurés avec l'appareil ALAMBETTA T675 commercialisé par la société VOLTA S.p.A.These tests were measured with the ALAMBETTA T675 device sold by VOLTA S.p.A.

Ces essais montrent que le tissu réalisé avec les fils de l'invention a une perméabilité à l'air équivalente pour un grammage inférieur à 30% par rapport à un tissu réalisé avec des fils conventionnels. En outre, le coefficient de conductivité est nettement inférieur pour le tissu réalisé avec les fils de l'invention permettant ainsi de réaliser des vêtements plus isolants pour un poids plus faible ou équivalent. These tests show that the fabric produced with the threads of the invention has a equivalent air permeability for a grammage of less than 30% compared to a fabric made with conventional threads. In addition, the conductivity coefficient is significantly lower for the fabric produced with the threads of the invention, thus making it possible to make more insulating clothing for a lower weight or equivalent.

EXEMPLE 2EXAMPLE 2

Les fils selon l'invention sont obtenus par filage dans un procédé de Filage Etirage Intégré, d'une composition comprenant un polyamide PA 6 de viscosité relative VR égale à 50 et un agent matifiant constitué par de l'oxyde de titane à une concentration pondérale de 0,4%.The yarns according to the invention are obtained by spinning in a drawing and drawing process Integrated, of a composition comprising a polyamide PA 6 of relative viscosity VR equal to 50 and a matting agent consisting of titanium oxide at a concentration 0.4% by weight.

Cette composition est alimentée dans un dispositif de filage conventionnel comprenant une filière adaptée pour le filage de fil creux identique à celle utilisée dans l'exemple 1, mais comportant 20 trous par filière.This composition is fed into a conventional spinning device comprising a die suitable for spinning hollow wire identical to that used in Example 1, but having 20 holes per die.

Les conditions de filage sont les suivantes :

  • pression : 220 bar
  • température : 272°C
  • débit de polymère :1,75 g/min/trou
The spinning conditions are as follows:
  • pressure: 220 bar
  • temperature: 272 ° C
  • polymer flow: 1.75 g / min / hole

Le faisceau de filaments est refroidi en sortie de filière par un flux de fluide de refroidissement alimenté selon une direction sensiblement perpendiculaire à la direction de défilement du faisceau. Cette alimentation est disposée à une distance de 40 mm de la surface de sortie de la filière. Dans l'exemple illustré, le fluide de refroidissement est de l'air à une température de 20°C. Bien entendu, le flux de fluide de refroidissement est alimenté selon une vitesse qui ne provoque pas de perturbation dans le défilement du faisceau de filaments.The filament bundle is cooled at the outlet of the die by a flow of cooling supplied in a direction substantially perpendicular to the direction beam travel. This power supply is placed at a distance of 40 mm from the die exit surface. In the example illustrated, the coolant is air at a temperature of 20 ° C. Of course, the flow of coolant is fed at a speed which does not cause disturbance in the scrolling of the bundle of filaments.

Les filaments sont ensuite convergés en un point distant de 130 cm de la sortie de la filière. Une composition d'ensimage est déposée sur le fil ainsi formé selon des procédés et dispositifs conventionnels.The filaments are then converged at a point 130 cm from the outlet of the sector. A sizing composition is deposited on the yarn thus formed according to conventional methods and devices.

Le fil est ensuite renvidé sur une bobine à une vitesse de renvidage égale à 4500 m/min.The wire is then wound up on a spool at a winding speed equal to 4500 m / min.

Le fil obtenu a un titre total de 78 dtex et comprend 20 filaments (titre du fil 78F20).The yarn obtained has a total titer of 78 dtex and includes 20 filaments (thread title 78F20).

le fil obtenu présent un pourcentage de vide supérieur à 15%. Le nombre de filaments à section en forme d'arc de cercle, c'est à dire dont les extrémités n'ont pas coalescé à la sortie de la filière est égal à zéro.the yarn obtained has a percentage of void greater than 15%. Number of filaments with an arcuate section, i.e. the ends of which do not have coalesced at the outlet of the die is equal to zero.

Les caractéristiques du fil obtenu sont les suivantes :

  • USTER coefficient (U %) : 1 (valeur déterminée par intégration)
  • Allongement à la rupture : 35%
  • Ténacité : 38 cN/Tex
  • Facteur de cohésion : 10 noeuds/m
    (déterminé par la méthode manuelle du crochet)
The characteristics of the wire obtained are as follows:
  • USTER coefficient (U%): 1 (value determined by integration)
  • Elongation at break: 35%
  • Tenacity: 38 cN / Tex
  • Cohesion factor: 10 knots / m
    (determined by manual hook method)

Claims (23)

  1. Multifilament polyamide textile yarn having a filament count of less than 10 dtex and the filaments of which have a hollow cross section having a central empty area representing at least 5% of the total area of the cross section of the said filament, characterized in that the yarn has an Uster coefficient (U%) of less than 3% and the number of filaments having a cross section in the form of a circular arc is less than 30% of the total number of filaments having a hollow cross section.
  2. Yarn according to Claim 1, characterized in that it has a U% of less than 2%.
  3. Yarn according to Claim 2, characterized in that it has a U% of less than 1%.
  4. Yarn according to one of Claims 1 to 3, characterized in that the number of filaments having an open cross section or a cross section in the form of a circular arc is less than 20%, preferably less than 10%, with respect to the number of filaments having a hollow cross section in the yarn.
  5. Yarn according to one of the preceding claims, characterized in that the empty area of a hollow cross section of a filament represents at least 10% of the total cross section of the said filament.
  6. Yarn according to one of the preceding claims, characterized in that the polyamide is in the group comprising nylon-6, nylon-6,6, polyamide blends comprising at least 80% by weight PA 66 or nylon-6, copolyamides at least 80% by number of which are nylon-6,6 or nylon-6 units.
  7. Yarn according to one of the preceding claims, characterized in that the polyamide has a relative viscosity VR of between 40 and 55.
  8. Yarn according to Claim 7, characterized in that the relative viscosity is between 40 and 50.
  9. Process for manufacturing a multifilament polyamide yarn comprising filaments of hollow cross section, consisting in extruding a polyamide composition through at least one spinneret comprising several spinneret holes in order to form filaments, in making at least some of the said filaments converge at a point remote from the spinneret in order to form the said multifilament yarn and then to wind up the said yarn on a reel, characterized in that each spinneret hole consists of a slot in the form of a circular arc, the ends of which are separated by a length at most equal to 5 times the mean width of the said slot emerging at the exit face of the spinneret, the filaments being cooled on leaving the spinneret and the yarn being wound up at a rate of greater than 3000 m/min.
  10. Process according to Claim 9, characterized in that the hollow area of the cross section of each filament is equal to at least 5% of the total area of the cross section of the filament.
  11. Process according to Claim 10, characterized in that the amount of hollow area is equal to at least 10% of the area of the cross section of the filament.
  12. Process according to one of Claims 9 to 11, characterized in that the mean width of the slot is between 0.05 mm and 0.12 mm.
  13. Process according to one of Claims 9 to 12, characterized in that the coolant for cooling the filaments beneath the spinneret is chosen from the group comprising air and an inert gas.
  14. Process according to one of Claims 9 to 12, characterized in that the yarn comprises at most 30% by number of filaments having a cross section in the form of a circular arc compared with the number of filaments having a closed hollow cross section.
  15. Process according to one of Claims 9 to 14, characterized in that the yarn has an Uster coefficient of less than 3%.
  16. Process according to one of Claims 9 to 14, characterized in that the ends of the circular arc forming each spinneret hole are symmetrical over at least 5% of the length of the said circular arc.
  17. Process according to Claim 16, characterized in that the symmetrical ends of each circular arc have a length equal to at least 15% of the total length of a circular arc.
  18. Process according to one of Claims 9 to 17, characterized in that the polyamide has a relative viscosity of between 40 and 55.
  19. Process according to Claim 18, characterized in that the polyamide has a relative viscosity of between 40 and 50.
  20. Process according to one of the preceding claims, characterized in that the polyamide is chosen from the group comprising nylon-6, nylon-6,6, polyamide blends comprising at least 80% by weight of nylon-6,6 or nylon-6, and copolyamides comprising at least 80% by number of nylon-6,6 or nylon-6 units.
  21. Process according to one of Claims 9 to 20, characterized in that the yarn is subjected to a drawing operation before it is wound up.
  22. Flat, textured or twisted yarn obtained from a multifilament yarn according to one of Claims 1 to 8.
  23. Woven or knitted textile surface obtained from at least one yarn according to one of Claims 1 to 8 or 22.
EP98963617A 1997-12-29 1998-12-23 Multifilament textile yarns with hollow section, method for making same, and textile surfaces obtained from said yarns Expired - Lifetime EP1044293B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR9716833A FR2773178B1 (en) 1997-12-29 1997-12-29 MULTIFILAMENTARY TEXTILE THREADS WITH HOLLOW SECTION - PROCESS FOR MANUFACTURING THESE THREADS, AND TEXTILE SURFACES OBTAINED THEREWITH
FR9716833 1997-12-29
PCT/FR1998/002857 WO1999034040A1 (en) 1997-12-29 1998-12-23 Multifilament textile yarns with hollow section, method for making same, and textile surfaces obtained from said yarns

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US6855425B2 (en) * 2000-07-10 2005-02-15 Invista North America S.A.R.L. Polymer filaments having profiled cross-section
DE202007005259U1 (en) * 2007-04-10 2007-06-28 X-Technology Swiss Gmbh Garment to be worn by jogger, cyclist or skater, comprises outer and inner surface made of different but interconnected material
CN102041593B (en) * 2007-05-10 2015-11-25 可隆株式会社 A kind of method by multiple filament production filaments bundles
CN102418160A (en) * 2011-08-09 2012-04-18 马海燕 Large-diameter circular hollow polymer monofilament and production method thereof
KR101586554B1 (en) * 2011-12-07 2016-01-18 아사히 가세이 셍이 가부시키가이샤 Synthetic fiber
CN104178828A (en) * 2013-05-23 2014-12-03 东丽纤维研究所（中国）有限公司 Hollow false-twisted textured yarn and cloth formed by same

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IT589708A (en) * 1955-09-17
AR204352A1 (en) * 1974-04-03 1975-12-22 Du Pont POLYHEXAMETHYLENADIPAMIDE THREAD WITHOUT STRETCHING VAPORIZED AND PROCEDURE FOR OBTAINING IT
JPS5721510A (en) * 1980-07-08 1982-02-04 Toray Ind Inc Spinneret for hollow fiber
JPS58169507A (en) * 1982-03-26 1983-10-06 Tanaka Kikinzoku Kogyo Kk Spinneret for hollow fiber
JPS61289110A (en) * 1985-06-14 1986-12-19 Toray Ind Inc Spinneret for hollow fiber
DE4334004A1 (en) * 1993-10-06 1995-04-13 Hoechst Ag Aramid fibers of high strength and high titer, process for their production and their use
US5439626A (en) * 1994-03-14 1995-08-08 E. I. Du Pont De Nemours And Company Process for making hollow nylon filaments

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CN1193119C (en) 2005-03-16
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US6565972B1 (en) 2003-05-20
CN1284140A (en) 2001-02-14
PL341523A1 (en) 2001-04-23
DE69802841T2 (en) 2002-06-20
EP1044293A1 (en) 2000-10-18
SK285172B6 (en) 2006-07-07
KR100361197B1 (en) 2002-11-22
CA2316819A1 (en) 1999-07-08

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