EP2664697B2 - Fibres de cellulose régénérée ignifuges et procédé destiné à leur fabrication - Google Patents

Fibres de cellulose régénérée ignifuges et procédé destiné à leur fabrication Download PDF

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Publication number
EP2664697B2
EP2664697B2 EP12007741.7A EP12007741A EP2664697B2 EP 2664697 B2 EP2664697 B2 EP 2664697B2 EP 12007741 A EP12007741 A EP 12007741A EP 2664697 B2 EP2664697 B2 EP 2664697B2
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Prior art keywords
regenerated cellulose
tex
produced
less
staple
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EP12007741.7A
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German (de)
English (en)
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EP2664697A2 (fr
EP2664697B1 (fr
EP2664697A3 (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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Priority claimed from PCT/EP2012/002069 external-priority patent/WO2012152451A1/fr
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • 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

Definitions

  • the invention relates to a regenerated cellulose fiber, and a process for its preparation.
  • WO 2011/026159 A1 discloses flame retarded cellulose regenerate fibers having increased strength properties.
  • the invention provides a flame-retarded cellulosic regenerate fiber having good dry strength properties according to claim 1. Further preferred embodiments and method aspects are specified in the following claims.
  • 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.
  • a further aspect is to develop 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.
  • a refinement is preferably characterized in that a dimensionless first parameter formed from the quotient of the draft dimensioned in percent and the final take-off speed formed in meters per minute is less than 2.5, preferably less than 2.0, in particular less than 1, 67th
  • the surface quality of the continuous fiber can thus be determined by the number of lint per unit of mass of the fiber, for example per 1000 meters of length (or per kilogram of yarn).
  • the number of lint per 1000 meters means the number of detectable by a meter defects on the yarn per 1000 meters in length, a single broken single filament may already cause such a defect, however, two or more broken at the same point individual capillaries can not be 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 more preferably less than 1.5, preferably less than 1.33, in particular 1.25. This makes it possible to produce particularly good surface properties of the fibers.
  • a dimensionless second parameter which is not formed from the quotient but from the product of the two variables as the first parameter, is in the range from 3200 upwards, preferably greater than 3600, in particular greater than 4000, but preferably in the range of less than 8000 , preferably less than 7500, in particular less than 7000.
  • At least a value of 40 m / min, preferably at least 50, more preferably at least 60 and in particular 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%. It is further preferred that the sized in meters per minute Endabzugs technically under the curve 95 is - 0.016 x scroll 2 to 0.025 x 2, preferably under the curve 90th
  • 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. Further, it is preferable that the total titre 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 relates in percent to the ⁇ -cellulose above 16.5 + (290-T) / 90, preferably 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 preferably be in the range of 17.5 to 19.0%.
  • a viscose spun and twisted multifilament is proposed, which was produced in particular according to one of the method aspects described above, and in which a number of flakes of 2 flakes per 1000 meters in length is not exceeded, preferably a number of flutes of 1 flute per 1000 meters, in particular of 0.5 lint 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 4.2% or less, preferably 4% or less, more preferably 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 washings), the fabric produced therefrom remains under 5% further shrinkage after another 50 washes.
  • the product of the chord modulus thus measured in cN / tex be in the range of not less than 280, preferably not less than 320, more preferably not less than 360, with the square root of the denier of the fiber expressed in dtex Furthermore, 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. In absolute terms, 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 [ ⁇ ]).
  • regenerated cellulose fibers represent a thoroughly high-quality base material for flame-resistant fibers, since it can be equipped excellent flame-resistant per se known techniques. Because they are able to absorb large amounts of moisture as a hydrophilic, non-thermoplastic polymer.
  • the use of the lyocell method (direct dissolution method with NMMO as solvent) is possible, but very high strengths at a low fibrillation tendency are preferably achieved with the viscose method in its form as a filament spinning method, as described above.
  • the inherent strength properties of cellulose can be utilized optimally.
  • a high degree of stretching can be advantageous here, but on the other hand drying in a non-relaxed state can also be advantageous.
  • the resulting micro-morphology, degree of crystallization and degree of alignment of the elemental cellulose strands may be advantageous for high strength properties.
  • staple fibers are formed by first producing endlessly produced fibers in a wet spinning process, then cutting them in a moist state and drying them later in a relaxed state.
  • the filaments are re-stretched between rolls rotating at different speeds and finally torn.
  • the length of the resulting staple fibers can be adjusted by adjusting the parameters of the stretch-breaking process.
  • Another preferred feature relates to the volume-to-surface ratio (or cross-sectional area to circumference, as determined by ImageJ Image Analysis Optical Software), which provides fewer targets for mechanical stress as well as heat exposure.
  • volume-to-surface ratio or cross-sectional area to circumference, as determined by ImageJ Image Analysis Optical Software
  • phosphorus-containing, halogen-free agents such as the above-mentioned Sandoflam / Exolit are preferred.
  • the staple fibers according to the invention are preferably produced by the viscose filament spinning process.
  • This is a Viskosepinnmasse in an acidic spin bath or acidic spinning baths regenerated to cellulose and thereby stretched.
  • the subsequent drying of the filaments thus produced can be done online or offline, wherein preferably the tension in the filaments is maintained. Subsequently, the stretch breakage of the fibers dried in the non-relaxed state can take place.
  • Preferred individual titers of the yarns according to the invention are in the range between 1.7 and 3.3 dtex, but in particular greater than 2.0 dtex and / or less than 2.7 dtex.
  • a textile fabric which is produced by incorporation of a cellulose regenerated fiber, in particular a staple fiber or a multifilament, according to one of the properties described above.
  • FIGS. 1 and 2 Based on FIGS. 1 and 2 describes a preparation of a flame-retardant fiber with the peculiarity of a direction of parallel preferred parallel direction preferred for the main particle axes of a flame-retardant entrained solid.
  • this is not essential to the gist of the present invention. Rather, the invention shown in particular in the further embodiments is basically independent of the shape and the nature of the spinning of a flame-retardant solid.
  • a stirred tank 1 From a stirred tank 1 is a dispersion of particles of a flame-retardant solid from a metering pump 2 via a check valve 5 a static
  • 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 multifilament produced in any case according to the first aspect of this invention. It can be seen, indicated by the arrows, the orientation of the particle main axis in the parallel preferred direction of the fiber.
  • an industrial process is understood to mean a process in which the machine used achieves an hourly production of at least 6 or preferably at least 8, in particular at least 10, kg per hour.
  • 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.
  • this multifilament yarn is twisted (S500) only 0.4 to 0.6 fluff per 1000 meters up. It is therefore ideal for further processing, especially as a warp material.
  • FIG. 3 An embodiment of the invention is based on the Figures 3 and 4 explained.
  • multifilament fibers were cut into staple fibers, for example, as in the example described above.
  • the strength properties of these staple fibers result from the in the Figures 3 and 4 illustrated force-strain curves ( Fig. 3 : dry, Fig. 4 : wet).
  • the abscissa indicates the relative elongation in percent and the ordinate the force measured in cN / tex.
  • Fig. 3 shows that the zero slope of the measured values is higher than the slope after reaching an elongation force of about 10 cN / tex.
  • an average slope here is 2 cN / tex /% in the range of 2 to 7% relative elongation. In terms of force, this range corresponds to values between about 10 and 20 cN / tex.
  • the strength properties are significantly better than comparable commercially available products such as the products already mentioned above.
  • Fig. 4 show that the exemplary staple fiber also has advantageous wet strength properties, in particular a very high force required to rupture the fiber, which exceeds the conventional fibers by more than 40%.
  • Fig. 5 still shown that the staple fibers of this embodiment of conventional fibers also differ in their structure.
  • Fibers shown on the right have a more favorable surface area to volume ratio than conventional flame resistant staple fibers.
  • Another embodiment is a staple fiber yarn 200 dtex of 70% Viscont FR staple fiber and 30% m-aramid (Conex): Titer / dtex Firmness [cN / tex] Strain [%] Firmness wet [cN / tex] 200 17.4 9.2 13.9

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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)

Claims (15)

  1. Fibre de cellulose régénérée ignifuge, notamment fibre coupée et notamment fabriquée selon le procédé de production de la viscose, présentant des propriétés de résistance à sec accrues sous la forme d'une force moyenne nécessaire par % d'allongement, dans la plage d'allongement relatif allant de 2 à 7 %, qui est de 1,4 cN/tex ou plus, de préférence d'au moins 1,6 cN/tex ou plus, plus préférablement d'au moins 1,8 cN/tex ou plus et notamment d'au moins 2,0 cN/tex ou plus.
  2. Fibre de cellulose régénérée selon la revendication 1, présentant une résistance maximale à la traction (à sec) de 26 cN/tex, de préférence d'au moins 28 cN/tex, plus préférablement d'au moins 30 cN/tex.
  3. Fibre de cellulose régénérée selon la revendication 1 ou 2, présentant une résistance maximale à la traction (humide) d'au moins 15 cN/tex, de préférence d'au moins 18 cN/tex, notamment d'au moins 20 cN/tex.
  4. Fibre de cellulose régénérée selon l'une quelconque des revendications précédentes, dans laquelle l'effet ignifugeant est assuré par l'intégration par filage d'un agent ignifugeant, notamment d'un ignifugeant contenant du phosphore, la teneur en phosphore rapportée à la cellulose présente dans la fibre ne dépassant pas 3,4 %, ne dépassant de préférence pas 3,2 % et ne dépassant notamment pas 3,0 %.
  5. Fibre de cellulose régénérée, présentant un rapport entre la surface transversale moyenne exprimée en pixels et la circonférence moyenne exprimée en pixels de 16,6 ou moins, de préférence de 16,2 ou moins, notamment de 15,8 ou moins.
  6. Fibre de cellulose régénérée selon l'une quelconque des revendications précédentes, fabriquée à partir d'un fil continu sec.
  7. Fibre de cellulose régénérée selon la revendication 6, dans laquelle la fibre coupée est fabriquée par coupure du fil continu.
  8. Fibre de cellulose régénérée selon la revendication 6, dans laquelle la fibre coupée est fabriquée par rupture par étirement (stretch breaking) du fil continu.
  9. Fibre de cellulose régénérée selon l'une quelconque des revendications 6 à 8, dans laquelle la longueur de la fibre coupée se situe dans la plage allant de 30 à 150 mm.
  10. Fibre de cellulose régénérée selon l'une quelconque des revendications précédentes, dont la fabrication met en oeuvre un quotient de l'étirement dans le bain secondaire, mesuré en pourcentage, après précipitation dans le bain de filage par la vitesse de dévidage finale hors du bain secondaire mesurée en mètre par minute qui est inférieur à 2,5, de préférence inférieur à 2,0, notamment inférieur à 1,67.
  11. Fil à base de fibres coupées, présentant une fibre de cellulose régénérée selon l'une quelconque des revendications 1 à 10 sous la forme d'une fibre coupée, ainsi qu'un autre composant de préférence à base de fibre d'aramide, dans lequel la proportion de fibre de cellulose régénérée est de préférence d'au moins 20 % en poids (par rapport audit fil), plus préférablement d'au moins 50 % en poids, tout préférablement d'au moins 70 % en poids.
  12. Structure textile produite par incorporation d'une fibre de cellulose régénérée, notamment d'une fibre et/ou d'un fil selon l'une quelconque des revendications 1 à 11.
  13. Procédé de fabrication de fibres de cellulose régénérées selon revendication 1, dans lequel des filaments fabriqués selon le procédé de filage de filaments de viscose sont séchés « online » ou « offline », de préférence en maintenant la tension dans les filaments, et des fibres coupées sont fabriquées à partir des filaments secs.
  14. Procédé selon la revendication 13, dans lequel de la viscose est mélangée après ajout d'un solide selon un rapport quantitatif précis et le mélange ainsi produit est filé par voie humide selon des paramètres précis et, après précipitation dans le bain de filage, est étiré dans un bain secondaire d'où il est finalement dévidé, dans lequel un premier paramètre adimensionnel formé à partir du quotient de l'étirement mesuré en pourcentage par la vitesse de dévidage finale mesurée en mètre par minute est inférieur à 2,5, de préférence inférieur à 2,0, notamment inférieur à 1,67.
  15. Procédé selon la revendication 13 ou 14, dans lequel la fabrication des fibres coupées à partir du multifilament se produit à l'état sec par coupure ou par rupture par étirement.
EP12007741.7A 2012-05-14 2012-11-15 Fibres de cellulose régénérée ignifuges et procédé destiné à leur fabrication Not-in-force EP2664697B2 (fr)

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Application Number Priority Date Filing Date Title
EP12007741.7A EP2664697B2 (fr) 2012-05-14 2012-11-15 Fibres de cellulose régénérée ignifuges et procédé destiné à leur fabrication

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
PCT/EP2012/002069 WO2012152451A1 (fr) 2011-05-12 2012-05-14 Fibre de cellulose régénérée ignifuge et son procédé de fabrication
EP12007741.7A EP2664697B2 (fr) 2012-05-14 2012-11-15 Fibres de cellulose régénérée ignifuges et procédé destiné à leur fabrication

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EP2664697A2 EP2664697A2 (fr) 2013-11-20
EP2664697A3 EP2664697A3 (fr) 2014-01-01
EP2664697B1 EP2664697B1 (fr) 2016-03-02
EP2664697B2 true EP2664697B2 (fr) 2018-05-23

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
WO2011025159A2 (fr) † 2009-08-25 2011-03-03 두산인프라코어 주식회사 Mécanisme de chargement de palettes pour une machine-outil

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE547846A (fr) 1955-08-23 1900-01-01
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
DE1071277B (fr) 1957-12-26 1959-12-17 Algemene Kunstzijde Unie N.V., Arniheim (Niederlande)
NL270454A (fr) 1960-10-21
DE2311180C3 (de) 1973-03-07 1982-02-25 Chemiefaser Lenzing AG, 4860 Lenzing, Oberösterreich Verfahren zur Herstellung flammfester Celluloseregeneratfasern
DE2843989A1 (de) 1977-10-13 1979-04-19 Courtaulds Ltd Faeden aus regenerierter zellulose
US8070996B2 (en) * 2009-01-28 2011-12-06 Lenzing Aktiengesellschaft Process for the production of flame-retardant viscose fibres
AT508687A1 (de) * 2009-09-01 2011-03-15 Chemiefaser Lenzing Ag Flammgehemmte cellulosische faser, deren verwendung sowie verfahren zu deren herstellung

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
WO2011025159A2 (fr) † 2009-08-25 2011-03-03 두산인프라코어 주식회사 Mécanisme de chargement de palettes pour une machine-outil

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Publication number Publication date
ES2569859T3 (es) 2016-05-12
EP2664697A2 (fr) 2013-11-20
EP2664697B1 (fr) 2016-03-02
EP2664697A3 (fr) 2014-01-01

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