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EP2707526B2 - Procédé de fabrication des fibres de cellulose régénérées - Google Patents
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EP2707526B2 - Procédé de fabrication des fibres de cellulose régénérées - Google Patents

Procédé de fabrication des fibres de cellulose régénérées Download PDF

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Publication number
EP2707526B2
EP2707526B2 EP12722080.4A EP12722080A EP2707526B2 EP 2707526 B2 EP2707526 B2 EP 2707526B2 EP 12722080 A EP12722080 A EP 12722080A EP 2707526 B2 EP2707526 B2 EP 2707526B2
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process according
dtex
cellulose
parameter
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German (de)
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EP2707526B1 (fr
EP2707526A1 (fr
Inventor
Bernhard Müller
Martin GEBERT-GERM
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Glanzstoff Bohemia sro
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Glanzstoff Bohemia sro
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Classifications

    • 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
    • D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
    • D01F2/08—Composition of the spinning solution or the bath
    • 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
    • D01D5/12—Stretch-spinning methods
    • 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
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
    • 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
    • D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose

Definitions

  • the invention generally relates to a process for the production of cellulose regenerated fiber, in particular a multifilament fiber, in which viscose before wet-spinning still a solid is added, and in which after the at least partial coagulation of the filaments in the spinning bath following the extrusion of the dope still a stretching in Second bath takes place, from which the filaments are withdrawn at a final take-off speed.
  • Fiber products currently being used are based primarily on staple fiber yarns using the Lenzing FR fiber, particularly due to market shortages.
  • these staple fiber yarns are only of limited suitability for use as warp material.
  • Examples of staple fibers from which, for example, staple fiber yarns can be produced and which also have good service properties are disclosed in US Pat WO 2011/026159 A1 disclosed.
  • the invention is therefore based on the object of developing a method as mentioned above so that the further processability of the fiber products produced therewith improves, in particular with regard to use as a warp material, in particular for the production of high-quality textile products for use, for example, as protective clothing.
  • the surface quality of the continuous fiber can thus be determined by the number of lint per unit of quantity of the fiber, for example per 1000 meters of length (or per kilogram of yarn).
  • the number of lint per 1000 meters is understood to mean the number of defects on the yarn per 1000 meters of length detectable by a gauge, whereby a single broken single filament may already cause such a defect, two or more single capillaries fractured at the same location but not counted twice or more times.
  • a suitable measuring device is, for example, an Elkometer III from the company Textechno.
  • the first parameter is preferably greater than 0.75, in particular greater than 1.0. Also, the first parameter may be less than 1.33, especially 1.25. This can be special produce good surface properties of the fibers.
  • the dimensionless zwelte parameter which is not formed from the quotient but from the product of the two variables as in the first parameter, is greater than 3600, in particular greater than 4000, but less than 7500, in particular less than 7000.
  • a value of at least> 65 m / min is achieved as the absolute value for the final take-off speed.
  • the titer of the multifilament formed is specifically taken into account. It is provided that a dimensionless third parameter formed from the quotient of the second parameter and the root of the titer of the multifilament measured in dtex is not smaller than 300, preferably greater than 330, more preferably greater than 360, and in particular greater than 400.
  • the titer specification refers to the total titer of the multifilament, this is 225, for example, and the second parameter is 6300, the third parameter is 420.
  • these values of the third parameter relate primarily to multifibers with a total denier of 330 dtex or Less, but can also be used for slightly higher titers to about in the range of 600 dtex. In principle, however, for total titers of greater than 330 dtex, in particular of greater than 600 dtex or even greater than 900 dtex, a lower limit for the third parameter of 160, in particular 200, is preferred.
  • the value 680 is preferable. More preferably, the third parameter should be 600 or smaller, more preferably less than 530 and in particular less than 500.
  • the total amount of such water-insoluble pigments should preferably not exceed 25%. Furthermore, it is preferred that the final take-off speed measured in meters per minute move below the curve 95 - 0.025 x 2 , preferably below the curve 90 - 0.016 x 2 .
  • a phosphorus-containing flame retardant is preferably added as solid.
  • the addition is preferably carried out by adding a dispersion of the particles.
  • the addition may be made to the otherwise ready-to-spin mass.
  • the above-mentioned dispersants can also find application here.
  • a fiber thickness of not less than 60 dtex is preferred. Furthermore, it is preferable that the total denier of the fiber is not larger than 2500 dtex. With respect to the Kapillartiter a range of 1.8 to 2.6 dtex is considered to be preferred, in particular in the range of 2.2 to 2.6 dtex, the latter being particularly advantageous for Automatgarntiter of less than 330 dtex. As the average diameter of the single fiber, a range between 10 and 30 microns, preferably between 11 and 20 microns is considered advantageous.
  • the amount x FR of the phosphorus-containing flame retardant solid is metered in at a given total titer T of the multifilament in such a way that it is based on the ⁇ -cellulose in percent over 16.5 + (290-T) / 90 is above 17 + (290-T) / 90, and especially below 19 + (290-T) / 90, more preferably below 18.5 + (290-T) / 90.
  • the flame retardant recited in claim 10 is intended.
  • These quantities for x FR are primarily for total titers in the range of 330 or less. For total titers in the range of 330 or greater, x FR should be in the range of 17.5 to 19.0%.
  • a viscose-spun and twisted multifilament is achieved in which, on the one hand, a number of flutes of 2 flutes per 1000 meters in length is not exceeded, preferably a number of flutes of 1 flute per 1000 meters is not exceeded, in particular of 0.5 fluff per 1000 meters, and on the other hand, a phosphorus content based on the ⁇ -cellulose of 2.8% or higher, preferably 3% or higher, in particular 3.2% or higher and of 4.2% or less, preferably 4% or less, especially 3.8% or less.
  • the twisting takes place on suitable twisting machines, for example and preferably on ring twisting machines of the brand Ratti on S500.
  • an upper limit for the product of fluff number per 1000 meters in length and in terms of ⁇ -cellulose in percent phosphorus content is not greater than 8, more preferably not greater than 6, even more preferably not greater than 4, and in particular not greater than 3.
  • Dry tensile strengths in the conditioned state in the range of over 25 cN / tex are achieved for the finished fiber. Furthermore, after the initial shrinkage (first to second wash), the fabric produced therefrom remains under 5% further shrinkage after another 50 washes.
  • this product should preferably not exceed 560, more preferably 520 and in particular 480 do not exceed. These product values apply in particular to fibers with a total titer of 330 dtex or less.
  • the chord modulus should preferably be at least 20 cN / tex for yarn titers ⁇ 200 dtex, and at least 30 cN / tex for yarn titers of 120 dtex or less.
  • the roller temperature of the drying rollers is in this second aspect of the invention preferably in the range of 40 ° C or higher, preferably 45 ° C or higher, in particular 50 ° C or higher, and preferably 95 ° C or lower, preferably 80 ° C or lower, in particular 70 ° C or lower.
  • Particularly preferred pulp of the viscose is a pulp having an intrinsic viscosity of greater than 560 ml / g and an ⁇ -cellulose content of greater than 97.5%, in particular monomodal molecular weight distribution, in particular a kraft-softwood pulp.
  • the intrinsic viscosity should be determined according to ISO / FDIS 5351: 2009 (Limiting Viscosity Number [ ⁇ ]).
  • a textile fabric which is produced by incorporation of a cellulose regenerated fiber, in particular a multifilament, according to one of the properties described above.
  • aspects of the invention thus relate to a process for the production of cellulose regenerated fiber in which viscose is mixed with a dispersion of particles of a flame retardant solid in a dispersing agent in a certain proportion and the resulting mixture is wet-spun according to certain spinning parameters, as well as one in particular Process for the production of regenerated cellulose fibers, in particular in the form of multifilaments, and on multifilament yarns and textile fabrics formed therefrom (in particular according to ISO 11612).
  • the particles are brought into a form whose dimension is greater in a particle main axis than in the two orthogonal thereto particle secondary axes and the particle main axes are aligned in the fiber in a direction parallel to their spin direction preferred direction.
  • the main axes of the particles incorporated into the fiber are aligned such that in Ideatfall their main axes are aligned parallel to the spinning direction of the filament.
  • an approximation to this ideal state is that the orientation density function of the incorporated particles in the spinning direction of the filament assumes its maximum.
  • the ratio of the particle diameter in the plane spanned by the two particle secondary axes to the length of the particle measured along the main axis is preferably about 1: 3.
  • the shape of the particles is a rotational ellipsoid.
  • flame-retardant regenerated cellulose fibers with an LOI greater than 26, in particular 27 and strengths greater than 25 cN / tex and preferably greater than 26 cN / tex, more preferably greater than 29 and especially 30 cN / tex produce.
  • the decrease in the tensile strength in the conditioned state of the regenerated cellulose filament fiber-flame retardant fiber compared to a comparable regenerated filament fiber which does not contain flame retardant particles is less than 28%.
  • a decrease in strength of less than 25% and particularly preferably a reduction in strength of less than 20% can be achieved.
  • the condition is to follow the re-stretching of the fiber in the second bath.
  • the particle size distribution of the dispersion used as the starting material of the process is adjusted before it is fed to the mixing process in a nozzle-based dispersing device.
  • the total solids content of a flame-retardant dispersion obtainable under the trade name Viskofil® Exolit 5060 VP2988 is between 51 and 56 percent depending on the batch and formulation, the proportion of the flame retardant being between 41 and 47, in particular 45 and especially 47 to 45 (45) depending on the batch. Percent varies.
  • nozzle-based dispersing device which is preferably a device available under the product name Serendip Dispersion Device, for example Serendip LPN 60 or Serendip 500
  • Serendip Dispersion Device for example Serendip LPN 60 or Serendip 500
  • agglomerates of this commercially available dispersion formed by transport and / or storage are broken up. After only a short amount of energy, this results in a particle size distribution whose average particle diameter lies in a particularly favorable range between 0.7 and 0.8 ⁇ m and which has a very narrow particle size distribution.
  • the dispersant may be derived from the group of anionic, cationic and nonionic dispersants.
  • the addition of the additional dispersants favors, in particular, a process procedure in which filtering of the mixture from which the cellulose regenerated fiber is spun is carried out only in two coarse filters in which particles larger than 25 ⁇ m are retained.
  • An apparative filter sequence of a 10 micron fine filter and a 30 micron coarse filter, as in the prior art according to EP 1 882 760 is proposed, this is not required.
  • the inventive method is thereby significantly more economical, because only the two cheaper in the purchase and maintenance coarse filters are used.
  • a Kapellartiters of 1.8 dtex and hole diameters of the spinnerets from 40 to 60 microns.
  • the average diameter of the single fiber is between 10 to 30 microns, preferably 11 to 20 microns, a preferred upper limit for the Kapillartiter is 2.6 dtex.
  • the preferred capillary density is in the range of 2.2 to 2.6 dtex.
  • the viscose is fed to the mixing process as a flow of a viscous pump, whose delivery rate is controlled in dependence on a measurement of the pressure in the outflowing from the mixing flow.
  • This viscous pump may be, for example, a gear pump.
  • a further advantageous embodiment of the method according to the invention consists in that the dispersion is supplied to the mixing process by a metering pump, the delivery rate of which is regulated as a function of a measurement of the mass flow of the dispersion fed to the mixing process.
  • a uniform dosage of the input of dispersion into the cellulose is of particular importance for the strength of the regenerated fiber.
  • the maintenance of a fixed constant ratio of dispersion to viscose could, for example, be realized mechanically in the form of a transmission between the viscose pump and the metering pump. However, this would only keep the ratio of the volume flows constant.
  • the mass flow-dependent control of the metering pump allows a uniform metering of the dispersion.
  • a Coriolis mass flow meter is preferably used.
  • an eccentric screw pump is preferably used, since it enables significantly longer service lives in dispersions with a high solids content.
  • the alpha-cellulose content of the pulp used is greater than 97.5, in particular 98 percent with a DP greater than 400, in particular greater than 1500 in order to achieve the strengths according to the invention, and a DP of viscose greater than 400.
  • the pulp is also a kraft softwood pulp having an ⁇ -cellulose content of greater than 97.5%, in particular monomodal molecular weight distribution.
  • the viscosity of the viscose is preferably greater than 100 kfs at 20 ° C and the incorporated, water-insoluble flame-retardant particles have a rotational ellipsoidal shape, the longer major axes are aligned in a preferred direction parallel to the direction of stretching of the fiber. As a result, a particularly high strength can be achieved.
  • the flame-retardant substance used is preferably a phosphorus-containing substance, in particular 2,2'-oxybis [5,5-dimethyl-1,3,2-dioxaphosphorinane] 2,2'-disulphide.
  • the phosphorus content of the finished fiber is preferably in the range from 2.8% to 4.2%, more preferably from 3% to 4%, based on the ⁇ -cellulose.
  • the flow leaving the static mixer 7 passes through a mass flow meter 8 to a spinning machine in which the cellulose regenerated fiber is spun.
  • a control unit 10 generates in response to the measurement signals of the mass flow meter 8 and 9, a control signal for driving the metering pump 2, by the mass ratio of the two flow rates to a desired value is regulated.
  • the pressure of the conveyed to the spinning machine flow rate is detected by a pressure sensor 4 and regulated in response to the measurement signal, the delivery rate of the viscose pump 3.
  • Fig. 2 is an SEM image of a manufactured according to any of the variants described multifilament. It can be seen, indicated by the arrows, the orientation of the particle main axis in the parallel preferred direction the fiber.
  • the temperature of the coagulation spinning bath is in the range of 58 to 63 ° C, that of the coagulation bath in the range of 90 to 94 ° C.
  • the addition of the flame retardant is such that a solids content in the yarn (based on the ⁇ -cellulose) of 19.8% results.
  • the dimensionless second parameter is 6800 and the dimensionless third parameter is 480.
  • the phosphorus content of the fiber relative to the ⁇ -cellulose is in the range of 3.5%. Nevertheless, in the conditioned state, the fiber retains a dry tensile strength in the range of 265 to 285 cN / 100dtex.
  • the multifilament yarn thus produced (S500) has only 0.4 to 0.6 lint per 1000 meters. It is therefore ideal for further processing, especially as a warp material.

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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)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)

Claims (15)

  1. Procédé de fabrication d'une fibre de cellulose régénérée, notamment d'une fibre à multifilaments, dans lequel est ajouté de la viscose après ajout d'un solide selon un rapport quantitatif précis, le solide comprenant des pigments, et dans lequel le mélange ainsi produit est filé par voie humide et, après précipitation dans le bain de filage, est étiré dans un bain secondaire et en est finalement dévidé, la quantité totale des pigments incorporés pour le filage étant supérieure à 15 % relatif à l'α-cellulose, caractérisé en ce que
    un premier paramètre adimensionnel constitué par le quotient entre l'étirement exprimé en pourcentage et la vitesse de dévidage finale exprimée en mètre par minute est inférieur à 1,5, un deuxième paramètre adimensionnel constitué par le produit entre l'étirement exprimé en pourcentage et la vitesse de dévidage finale exprimée en mètre par minute est supérieur à 3600 et inférieur à 7500, la vitesse de dévidage finale étant au moins 65 m/min et l'étirement étant non supérieur à 100 %.
  2. Procédé selon la revendication 1, dans lequel le premier paramètre est supérieur à 0,75, de préférence supérieur à 1,0.
  3. Procédé selon la revendication 1 ou 2, dans lequel le premier paramètre est inférieur à 1,33, notamment inférieur à 1,25.
  4. Procédé selon l'une quelconque des revendications 1 à 3, dans lequel le deuxième paramètre est supérieur à 4000 et/ou inférieur à 7000.
  5. Procédé selon la revendication 4, dans lequel un troisième paramètre adimensionnel constitué par le quotient entre le deuxième paramètre et la racine du titre du multifilament mesuré en dtex est supérieur à 300, de préférence supérieur à 330, plus préférablement supérieur à 360 et notamment supérieur à 400.
  6. Procédé selon la revendication 4 ou 5, dans lequel un/le troisième paramètre adimensionnel constitué par le quotient entre le deuxième paramètre et la racine du titre du multifilament mesuré en dtex est inférieur à 680, de préférence inférieur à 600, plus préférablement inférieur à 530, notamment inférieur à 500.
  7. Procédé selon l'une quelconque des revendications 1 à 6, dans lequel la quantité totale x de quantité de solide ajoutée rapportée à l'a-cellulose indiquée en pourcentage ne dépasse de préférence pas 25 % et la vitesse de dévidage finale mesurée en mètre par minute se situe sous la courbe 95 - 0,025 x2, de préférence sous la courbe 90 - 0,016 x2.
  8. Procédé selon l'une quelconque des revendications 1 à 7, dans lequel le solide a un effet ignifugeant et contient notamment du phosphore, et son ajout s'effectue sous la forme d'une dispersion de particules ajoutée.
  9. Procédé selon l'une quelconque des revendications 1 à 8, dans lequel la fibre fabriquée est une fibre à multifilaments présentant un titre global supérieur à 60 dtex et de préférence inférieur à 2500 dtex, son titre capillaire étant notamment dans la plage allant de 1,8 à 2,6 dtex, tout préférablement dans la plage allant de 2,2 à 2,6 dtex.
  10. Procédé selon l'une quelconque des revendications 1 à 9, dans lequel la quantité XFR de solide ignifugeant contenant du phosphore est ajoutée en fonction du titre global T indiqué en dtex du multifilament de manière à se situer, en pourcentage par rapport à l'a-cellulose, au-dessus de 16,5+(290-T)/90, de préférence au-dessus de 17+(290-T)/90, et notamment en dessous de 19+(290-T)/90, plus préférablement en dessous de 18,5+(290-T)/90, lorsque T est de 330 dtex ou moins, et elle est notamment dans la plage allant de 17,5 à 19,0 % lorsque T est supérieur à 330 dtex.
  11. Procédé selon l'une quelconque des revendications 1 à 10, dans lequel le nombre de grosseurs pour 1000 m de multifilament non retordu est inférieur à 4, de préférence inférieur à 2.
  12. Procédé selon l'une quelconque des revendications 9 à 11, dans lequel il est formé par retordage, à partir de la fibre à multifilaments fabriquée, un muitifilament retordu présentant un nombre de grosseurs de 2 grosseurs pour 1000 mètres de longueur ou moins, de préférence 1 grosseur pour 1000 mètres ou moins, notamment 0,6 grosseur pour 1000 mètres ou moins, la teneur en phosphore rapportée à l'a-cellulose étant de 2,8 % ou plus, de préférence de 3 % ou plus, notamment de 3,2 % ou plus, en étant de 4,2 % ou moins, de préférence de 4 % ou moins, notamment de 3,8 % ou moins.
  13. Procédé selon la revendication 12, dans lequel le produit du module entre deux points indiqué en cN/tex [3,5 %-4 % humide] du multifilament retordu avec la racine carrée du titre indiqué en dtex est de 280 ou plus, de préférence de 320 ou plus, notamment de 360 ou plus, en étant de préférence de 560 ou moins, plus préférablement de 520 ou moins, notamment de 480 ou moins.
  14. Procédé selon l'une quelconque des revendications 1 à 13, dans lequel la cellulose mise en oeuvre est une cellulose présentant une viscosité limite supérieure à 560 ml/g et une teneur en α-cellulose supérieure à 97,5 % avec notamment une répartition monomo-dale des masses moléculaires, notamment une cellulose kraft-bois de résineux.
  15. Procédé selon l'une quelconque des revendications 12 à 14, dans lequel il est produit une structure textile par incorporation du multifilament retordu fabriqué.
EP12722080.4A 2011-05-12 2012-05-14 Procédé de fabrication des fibres de cellulose régénérées Active EP2707526B2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP15003343.9A EP3006608B1 (fr) 2011-05-12 2012-05-14 Fibres filaments de cellulose régénérée ignifuges

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102011101321A DE102011101321A1 (de) 2011-05-12 2011-05-12 Flammhemmende Celluloseregeratfilamentfasern und Verfahren zu dessen Herstellung
PCT/EP2012/002069 WO2012152451A1 (fr) 2011-05-12 2012-05-14 Fibre de cellulose régénérée ignifuge et son procédé de fabrication

Related Child Applications (2)

Application Number Title Priority Date Filing Date
EP15003343.9A Division EP3006608B1 (fr) 2011-05-12 2012-05-14 Fibres filaments de cellulose régénérée ignifuges
EP15003343.9A Division-Into EP3006608B1 (fr) 2011-05-12 2012-05-14 Fibres filaments de cellulose régénérée ignifuges

Publications (3)

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EP2707526A1 EP2707526A1 (fr) 2014-03-19
EP2707526B1 EP2707526B1 (fr) 2015-11-25
EP2707526B2 true EP2707526B2 (fr) 2017-12-27

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EP15003343.9A Not-in-force EP3006608B1 (fr) 2011-05-12 2012-05-14 Fibres filaments de cellulose régénérée ignifuges

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US (1) US9828697B2 (fr)
EP (2) EP2707526B2 (fr)
DE (1) DE102011101321A1 (fr)
WO (1) WO2012152451A1 (fr)

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DE102012018814A1 (de) 2012-09-24 2014-03-27 Glanzstoff Bohemia S.R.O. Garn mit Flammschutzwirkung und daraus gebildete textile Flächengebilde
AT515152B1 (de) 2013-11-26 2015-12-15 Chemiefaser Lenzing Ag Verfahren zum Vorbehandeln von rückgewonnenen Baumwollfasern zur Verwendung bei der Herstellung von Formkörpern aus regenerierter Cellulose

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DE1242791B (de) † 1960-10-21 1967-06-22 Phrix Werke Ag Verfahren zum Herstellen von metallsulfidhaltigen Fasern, Faeden oder Folien aus regenerierter Cellulose
DE2311180C3 (de) † 1973-03-07 1982-02-25 Chemiefaser Lenzing AG, 4860 Lenzing, Oberösterreich Verfahren zur Herstellung flammfester Celluloseregeneratfasern

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AT193069B (de) 1955-10-25 1957-11-25 Glanzstoff Ag Verfahren zur Herstellung von künstlichen Fäden oder anderen Erzeugnissen, wie Roßhaar, Bändchen, Filmen, aus Viskose
GB861831A (en) 1957-12-26 1961-03-01 Algemene Kunstzijde Unie Nv An improved process for the manufacture of artificial threads and staple fibres fromviscose, as well as the threads and staple fibres thus obtained
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US9828697B2 (en) 2017-11-28
EP3006608B1 (fr) 2017-07-05
EP2707526B1 (fr) 2015-11-25
US20140210120A1 (en) 2014-07-31
WO2012152451A1 (fr) 2012-11-15
EP3006608A1 (fr) 2016-04-13
DE102011101321A1 (de) 2012-11-15
EP2707526A1 (fr) 2014-03-19

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