EP2664697A2 - 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
EP2664697A2
EP2664697A2 EP12007741.7A EP12007741A EP2664697A2 EP 2664697 A2 EP2664697 A2 EP 2664697A2 EP 12007741 A EP12007741 A EP 12007741A EP 2664697 A2 EP2664697 A2 EP 2664697A2
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EP
European Patent Office
Prior art keywords
fiber
less
tex
produced
cellulose
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP12007741.7A
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German (de)
English (en)
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EP2664697B1 (fr
EP2664697A3 (fr
EP2664697B2 (fr
Inventor
Bernhard Müller
Martin GEBERT-GERM
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
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
Application filed by Glanzstoff Bohemia sro filed Critical Glanzstoff Bohemia sro
Priority to EP12007741.7A priority Critical patent/EP2664697B2/fr
Publication of EP2664697A2 publication Critical patent/EP2664697A2/fr
Publication of EP2664697A3 publication Critical patent/EP2664697A3/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.
  • the invention generally relates to a process for producing regenerated cellulose fiber, in particular a multifilament fiber wherein a solid is added to the viscose prior to wet spinning, and after at least partially coagulating the filaments in the spin bath following extrusion of the dope still a stretching takes place in the secondary bath, 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.
  • This aspect of the invention is therefore the object of developing a method as mentioned above so that the further processing of the fiber products produced therewith improved, 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 dimensionless first parameter formed of the quotient of the percentage dimensioned draft 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 1.67.
  • 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 is understood to mean the number of defects on the yarn per 1000 meters of length detectable by a meter, with a single broken single filament already causing such a defect, two or more individual capillaries broken 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 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 final take-off speed, measured in meters per minute, be 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. It is further preferred that the total denier of the fiber is not greater than 2500 dtex.
  • 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.
  • 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 protected, which has been 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 one Flusenress of 1 flute per 1000 meters is not exceeded, 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, 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 based on the ⁇ -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 [n]).
  • the high strength properties achieved according to the invention are also considered worthy of protection.
  • cellulose regenerated fibers constitute a thoroughly high-quality base material for flameproof fibers, since it can be provided with excellent flameproofing by techniques known per se. Because as a hydrophilic, non-thermoplastic polymer they are able to absorb large quantities of moisture.
  • 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.
  • a further advantage of the fiber according to the invention is an appropriate volume-to-surface ratio (or cross-sectional area to circumference, eg determined by optical image analysis software ImageJ), which offers fewer points of attack with respect to mechanical stress, but also to heat.
  • volume-to-surface ratio or cross-sectional area to circumference, eg determined by optical image analysis software ImageJ
  • ImageJ optical image analysis software
  • the staple fibers according to the invention are preferably produced by the viscose filament spinning process.
  • a viscose spinning composition is regenerated to cellulose in an acid-containing spinning bath or acid-containing spinning baths and drawn.
  • 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 preferred direction 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 other embodiments basically independent of the shape and type of spinning of a flame-retardant solid.
  • a dispersion of particles of a flame-retardant solid from a metering pump 2 via a check valve 5 is fed to a static mixer 6.
  • the static mixer 6 is fed via a viscose pump 3 viscose. From the static mixer 6, the mixture of viscose and dispersion formed therein flows into another static mixer 7 and continues to be mixed there.
  • 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.
  • 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 (S500) has only 0.4 to 0.6 fluff per 1000 meters. It is therefore ideal for further processing, especially as a warp material.
  • FIG. 3 Another embodiment is based on the Figures 3 and 4 explained.
  • multifilament fibers were cut into staple fibers, for example, as in the previously described embodiment.
  • 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)
EP12007741.7A 2012-05-14 2012-11-15 Fibres de cellulose régénérée ignifuges et procédé destiné à leur fabrication Not-in-force EP2664697B2 (fr)

Priority Applications (1)

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

Publications (4)

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

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ID=47227416

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EP12007741.7A Not-in-force EP2664697B2 (fr) 2012-05-14 2012-11-15 Fibres de cellulose régénérée ignifuges et procédé destiné à leur fabrication

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EP (1) EP2664697B2 (fr)
ES (1) ES2569859T3 (fr)

Family Cites Families (10)

* 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
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
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
KR101574348B1 (ko) † 2009-08-25 2015-12-03 두산인프라코어 주식회사 공작기계의 팰리트 이송장치
AT508687A1 (de) * 2009-09-01 2011-03-15 Chemiefaser Lenzing Ag Flammgehemmte cellulosische faser, deren verwendung sowie verfahren zu deren herstellung

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None

Also Published As

Publication number Publication date
ES2569859T3 (es) 2016-05-12
EP2664697B1 (fr) 2016-03-02
EP2664697A3 (fr) 2014-01-01
EP2664697B2 (fr) 2018-05-23

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