EP3090081B1 - Cellulosische faser - Google Patents

Cellulosische faser Download PDF

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Publication number
EP3090081B1
EP3090081B1 EP14816301.7A EP14816301A EP3090081B1 EP 3090081 B1 EP3090081 B1 EP 3090081B1 EP 14816301 A EP14816301 A EP 14816301A EP 3090081 B1 EP3090081 B1 EP 3090081B1
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EP
European Patent Office
Prior art keywords
fiber
fibers
höller
der
lyocell
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EP14816301.7A
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German (de)
English (en)
French (fr)
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EP3090081A1 (de
Inventor
Christoph Schrempf
Kurt Christian Schuster
Hartmut Rüf
Heinrich Firgo
Karl Michael Hainbucher
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Lenzing AG
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Lenzing AG
Chemiefaser Lenzing AG
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Priority to PL14816301T priority Critical patent/PL3090081T3/pl
Priority to EP14816301.7A priority patent/EP3090081B1/de
Publication of EP3090081A1 publication Critical patent/EP3090081A1/de
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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
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres

Definitions

  • the present invention relates to a cellulosic fiber of the genus Lyocell.
  • NMMO N-methylmorpholine-N-oxide
  • a process for spinning cellulose solutions in amine oxides is known from US 5,156,062 US 4,246,221 known. According to this method, filaments extruded from a spinneret are passed through an air gap, stretched there, and the cellulose is subsequently precipitated in an aqueous spinning bath. The process is known as “dry / wet spinning” or "air gap spinning”.
  • amine oxide process The entire process for producing fibers from solutions of cellulose in a tertiary amine oxide is hereinafter referred to as "amine oxide process", wherein by the abbreviation "NMMO” in the following all tertiary amine oxides are meant, which can dissolve cellulose.
  • Fibers produced by the amine oxide process are characterized by high fiber strength in the conditioned and in the wet state, a high wet modulus and a high loop strength.
  • the WO 93/19230 describes a process in which the extruded filaments are cooled by blowing with air just below the nozzle.
  • the WO 94/28218 describes a nozzle design and a blowing method.
  • the WO 95/01470 claims a laminar flow in the WO 93/19230 described cooling gas flow.
  • the WO 95/04173 describes a further technical embodiment of the blowing.
  • the moisture content of the blown air is defined.
  • the blow-by airflow is directed downwards at an angle of 0 ° to 45 ° to the extruded filaments.
  • the WO 03/014436 describes a blowing device with extraction of the blowing air.
  • WO 03/057951 claims the shielding of a part of the air gap with respect to the blowing air.
  • a turbulent gas stream is described for cooling the filaments.
  • the WO 05/116309 also describes the shielding of a part of the air gap with respect to the blowing air.
  • the fibers / filaments obtained by the air-gap spinning process differ structurally from the known viscose fibers. While the crystalline orientation is approximately the same for both viscose fibers and lyocell fibers (largely parallel arrangement of the cellulose chains located in the ordered regions of the fiber to the fiber axis), there are marked differences in the amorphous orientation (higher parallelism of the disordered portions in lyocell fibers).
  • the properties of the lyocell fiber such as high crystallinity, long and thin crystallites and the high amorphous orientation prevent sufficient binding of the crystallites across the fiber axis.
  • the swelling of the fibers additionally reduces the binding forces transverse to the fiber axis and thus leads to the splitting off of fiber fragments under mechanical stress. This behavior is called wet fibrillation and results in reduced quality in the textile end product in the form of graying and hairiness.
  • EP 0 53 977 A examples of the method of chemical crosslinking are in the EP 0 53 977 A .
  • EP 0 665 904 A respectively.
  • a spinning solution of a single pulp is spun into a bath containing NMMO in amyl alcohol and isopropanol, respectively.
  • the WO 92/14871 claims a fiber with reduced fibrillation, characterized in that the pH of the spin bath and subsequent wash baths is below 8.5. No information is given on the type of pulp or spinning conditions.
  • the WO 94/19405 describes a process wherein a pulp mixture is used. However, no reference is made to the fibrillation tendency of the spun fibers.
  • the WO 95/02082 describes a combination of process parameters, represented in a mathematical expression, for producing a low fibrillation fiber.
  • the mentioned process parameters are the spin hole diameter, the spin mass output, the filament titer, the air gap width and the air gap humidity.
  • the pulp used is not described in detail, the spinning temperature is only 115 ° C.
  • the WO 96/07779 uses as spinning spin an organic solvent, preferably polyethylene glycol. No details are given about the pulp used or about the textile mechanical properties of the resulting fibers.
  • the spinning temperature is 110 ° C indicated.
  • the WO 96/20301 describes a process wherein the shaped solution is passed in succession through at least two precipitation media, wherein in the first precipitation medium a slower Coagulation of the cellulose over the latter precipitation medium takes place.
  • a higher alcohol is preferably used as the first precipitation medium.
  • the pulp used is not specified, the spinning temperature is 115 ° C.
  • the WO 96/21758 describes a process in which the shaped solution is blown in the air gap in an upper zone with higher humidity air and in a lower zone with lower humidity air.
  • pulps individual pulps of different degrees of polymerization are used, the spinning temperature is 115 ° C.
  • the EP 0 853 146 describes a two-stage process wherein the residence time of the fibers in the first precipitation step is adjusted so that only the tackiness of the surface of the fiber-formed solution is inhibited and the fibers are coagulated in a later precipitation stage.
  • the spinning temperature in the examples is 109-112 ° C.
  • the spinning temperature is in the range of 80 - 120 ° C.
  • the fibers are treated with a solution of 40-80% NMMO, if appropriate with the addition of an additive.
  • the fibers are treated with a zinc chloride solution.
  • the fibers are treated with a NaOH solution.
  • the fibers are treated in a relaxed state with a NaOH solution.
  • the spinning temperature is 110 - 120 ° C.
  • the spinning mass is spun by a centrifugal spinning process, the spinning temperature is 80-120 ° C.
  • the fibers are treated with a concentrated NMMO solution.
  • a dope composed of a single pulp of high hemicellulose and lignin content is processed by a dry / wet or meltblown spinning process.
  • the WO 01/90451 describes a spinning process characterized by a mathematical relationship containing the heat flux density in the air gap and the length to diameter ratio of the extrusion channel. Fibers spun according to the invention should have a lower fibrillation tendency, but no further details are given.
  • meltblown fibers are not suitable for textile use due to their uneven titer.
  • a fiber of low fibrillation is prepared by spinning two spinning solutions of different cellulose concentration from a single pulp from a bicomponent nozzle. No example is given.
  • the special structure of the lyocell fiber leads to excellent textile-mechanical properties such as high strength both in the dry and wet state and a very good dimensional stability of the fabric produced therefrom, on the other hand too low flexibility (high brittleness) of the fibers, resulting in a drop in the Abrasion resistance viscose fibers in the fabric reflected.
  • a flexible lyocell fiber is described in US patent no EP 0 686 712 , The patent claims a fiber with reduced NMR order, obtained by adding nitrogen-containing substances such as urea, caprolactam or aminopropanol to the polymer solution or in the precipitation bath. However, a fiber with very low wet strength is obtained; Thus, the fiber clearly differs from the fibers of the invention described below.
  • WO 97/25462 there is described a process for producing a flexible and fibrillation-reduced fiber, wherein the shaped fiber after the precipitation bath is passed through a washing and aftertreatment bath containing an aliphatic alcohol, optionally additionally with a sodium hydroxide additive.
  • the properties of the resulting fibers are described only inadequate, in particular lacking dry strength and wet strength data, which would allow classification into the "Höller diagram" described in more detail below.
  • EP 2 097 563 and EP 2 292 815 describe fibers or filaments, preferably for the application of tire cord, prepared by adding polyvinyl alcohol to the NMMO / spinning solution.
  • the fibers / filaments are characterized by high strength but low elongation, accordingly, their flexibility according to the above definition can only be small.
  • the WO 2014/029748 (not prepublished) describes the preparation of solvent-spun cellulose fibers especially from solutions in ionic liquids. Further prior art is from the documents DE 10 2011 119 840 A1 . AT 506 268 A1 . US 6,153,136 . CN 102477591A . WO 2006/000197 . EP 1 657 258 A1 . US 2010/0256352 A1 . WO 2011/048608 A2 . JP 2004/159231 A and CN 101285213 A known.
  • the change in properties should be achieved solely by choosing suitable process parameters in the production of the fiber, without resorting to chemicals foreign to the process as additives to the spinning mass, to the spinning bath or during the aftertreatment have to. Any additional chemical in the system, be it as an additive to the spinning mass or spin bath conditioned increased effort in the recovery and represents a cost factor.
  • novel and inventive lyocell fibers are described on the basis of the so-called "Höller factors" F1 and F2 as well as demarcated from known cellulosic man-made fibers of the prior art.
  • a lyocell fiber e.g. from a viscose fiber by textile mechanical parameters (such as strength values), but also by less clearly definable properties, e.g. the textile "handle" is different.
  • cellulose fiber produced by the viscose process, e.g. (Standard) viscose fiber, modal fiber or polynose fiber.
  • Factor analysis is a multivariate statistical method that allows a set of correlated features to be reduced to a smaller number of uncorrelated factors.
  • the textile mechanical properties used by Höller for the factor analysis were the maximum tensile strength conditioned (FFk) and wet (FFn), the maximum tensile elongation conditioned (FDk) and wet (FDn), the wet modulus (NM), the loop strength conditioned (SFk) and the knot strength conditioned ( KFK).
  • Höller Factor F 1 - 1,109 + 0.03992 xFFk - 0.06502 xFDk + 0.04634 xFFn - 0.04048 xFDn + 0.08936 X nm + 0.02748 xSFk + 0.02559 xKFk
  • Höller Factor F 2 - 7,070 + 0.02771 xFFk - 0.04335 xFDk + 0.02541 FFn + 0.03885 FDn - 0.01542 X nm + .2891 xSFk + .1640 xKFk ,
  • FIG. 1 shows in the coordinate system of the Höller factors F1 and F2 the Höller-tested fiber collective of 70 samples using commercially available fibers from regenerated cellulose.
  • F1 the division into (standard) viscose fibers and modal fibers can be seen, which are also cited by the BISFA as different Fasergattungen (although they are prepared by the same basic process, just the viscose process).
  • BISFA the Fa
  • modal fiber region which is subdivided into two subgroups, namely HWM ("high wet modulus") fibers and polynosic (“PN”) fibers.
  • HWM high wet modulus
  • PN polynosic
  • the graph also shows a border (dashed line), beyond which none of the fibers of regenerated cellulose investigated at that time was located.
  • lyocell fibers were still at the experimental stage and not commercially available at the time of this publication.
  • Lyocell fiber in Höller diagram is in FIG. 2 shown.
  • the fiber according to the invention thus occupies the Höller diagram roughly speaking the space above the abscissa and around the ordinate as well as to the left of it and is clearly delimited from currently commercially available lyocell fibers, roughly speaking (clearly) to the right of the ordinate in the Höller diagram.
  • the Lyocell fiber according to the invention in the Höller diagram is close to the field of (standard) viscose.
  • the lyocell fiber according to the invention by far has "viscose-like" properties in terms of its processability than the currently commercially customary lyocell fibers.
  • the fiber of the present invention retains the high dimensional stability of washing processes characteristic of the lyocell fiber.
  • the wet scrubbing behavior of the fiber according to the invention is between 300 and 5000 revolutions by the method described below up to fiber breakage, preferably between 500 and 3000 revolutions.
  • the flexibility (i.e., the quotient FDk / FFk) of the fiber of the invention is preferably between 0.55 and 1.00, preferably between 0.65 and 1.00.
  • the fiber according to the invention is preferably characterized in that it is produced by the amine oxide process.
  • the fiber of the invention is preferably as a staple fiber, i. as cut fibers, before.
  • the fiber according to the invention a defined molecular weight distribution of the raw material used is required. This is achieved in particular by mixing two or more individual pulps. Accordingly, the fiber according to the invention is preferably characterized in that it is made from a mixture of at least two different pulps.
  • pulps made from recycled cotton fibers are also suitable for the production of fibers according to the invention.
  • Such pulps can be made according to the teaching of the publication "Process for pretreating reclaimed cotton fibers used in the production of molded bodies from regenerated cellulose” (Research Disclosure, www.researchdisclosure.com , database number 609040, published on December 11, 2014) become.
  • the present invention also relates to a fiber bundle containing a plurality of fibers according to the invention.
  • fiber bundle is meant a plurality of fibers, e.g. a plurality of staple fibers, a strand of continuous filaments or a bale of fibers.
  • the loop strength was determined in accordance with DIN 53843 Part 2 as follows: The titers of the two fibers used for the test are determined on a vibroscope. For the determination of the loop strength, the first fiber is formed into a loop and clamped with both ends in the biasing weight (size of the bias weight according to the above BISFA regulation Chapter 7). The second fiber is drawn into the loop of the first fiber and the ends are clamped in the top clamp (gauge head) of the tensile tester so that the loop is in the middle of the two clamps. After settling the preload, the lower clamp is closed and the tensile test is started (clamping length 20 mm, pulling speed 2 mm / min). It must be ensured that the fiber break occurs at the loop of the loop. As titer-related Loop strength, the maximum tensile force value obtained is divided by the smaller of the two fiber titres.
  • the knot strength was determined in accordance with DIN 53842 Part 1 as follows: A loop is formed from the fiber to be tested, an end of the fiber is pulled through the loop, thus forming a loose knot. The fiber is clamped in the upper clamp of the tensile tester in such a way that the knot is midway between the clamps. After settling the preload, the lower clamp is closed and the tensile test is started (clamping length 20 mm, pulling speed 2 mm / min). For the evaluation, only results are used, where the fiber is actually torn at the node.
  • Example 3 titres FFk FDk FFn FDn NM SFk KFK dtex CN / tex % CN / tex % cN / tex, 5% CN / tex CN / tex example 1 1.37 21.8 15.2 16.7 22.8 4.2 14.8 21.3
  • Example 2 1.37 25.1 21.5 17.8 28.2 3.9 15.7 23.3
  • Example 3 1.37 26.4 17.4 19.0 22.2 4.8 16.3 23.3
  • Example 4 1.37 26.3 16.5 20.8 22.8 5.4 17.5 25.1
  • Example 5 1.36 26.0 14.0 17.5 20.5 4.7 14.5 22.7
  • Example 6 1.23 24.5 19.0 18.7 25.5 4.4 16.1 22.5
  • Example 7 1.34 24.7 17.5 20.0 24.4 5.5 16.7 24.1
  • Example 8 1.54 26.4 16.1 19.5 21.7 4.7 17.4 23.6
  • Example 9 1.29 27.5 14.9 20.5 21.0 5.8 20.6 24.9
  • Example 10 1.37 24.8 17.8
  • examples 1 to 17 according to the invention are indicated by their respective numbers, and comparative examples 1 to 4 are each preceded by a "V".
  • Comparative Example 1 demonstrates that, if all production parameters except the spinning temperature, which is 122 ° C below the required value of at least 130 ° C, with the parameters for producing the fiber according to the invention, the object of the invention is not achieved.
  • Comparative Example 2 demonstrates that if all the production parameters, with the exception of the delay, which is higher than the required value of 9.64 with 9.64, coincide with the parameters for producing the fiber according to the invention, the object according to the invention is not achieved.
  • Comparative Example 3 demonstrates the importance of the pulp. If all manufacturing parameters except for the pulp composition, with a Single pulp does not have the required proportion of very high and low molecular weight, consistent with the parameters for producing the fiber according to the invention, the object of the invention is not achieved.
  • Comparative Example 4 shows the properties and the position in the Höller diagram of a commercial lyocell fiber (Tencel® from Lenzing AG)
  • a 130 kg bale of a fiber 1.3 dtex / 38 mm according to Example 11 was processed into a ring yarn Nm 50. From this yarn, a single jersey basis weight 150 g / m2 was produced. A sample of this single jersey was stained for 45 min with 4% Novacronmarine FG, liquor ratio 1:30 at 60 ° C in the laboratory jet and then subjected to 15 household washes at 60 ° C.
  • Table 5 shows the scrub and wash performance of this single jersey as compared to a fabric of the same construction of a commercial viscose or lyocell fiber.
  • Table 5 Fiber according to Example 11 Viscose 1.3 dtex Lyocell standard 1.3 dtex Scouring Martindale tours until hole formation 57 500 58 750 15,500 washing trial Gray scale * Note after 1st wash 4-5 4 3-4 Note after 5th wash 4-5 4 1 Note after 10th wash 3 4-5 2 Note after 15. laundry 2-3 4-5 1 * Grades from 1 to 5, the best grade is 5

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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)
EP14816301.7A 2014-01-03 2014-12-22 Cellulosische faser Active EP3090081B1 (de)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PL14816301T PL3090081T3 (pl) 2014-01-03 2014-12-22 Włókna celulozowe
EP14816301.7A EP3090081B1 (de) 2014-01-03 2014-12-22 Cellulosische faser

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
EP14150132 2014-01-03
PCT/EP2014/079043 WO2015101543A1 (de) 2014-01-03 2014-12-22 Cellulosische faser
EP14816301.7A EP3090081B1 (de) 2014-01-03 2014-12-22 Cellulosische faser

Publications (2)

Publication Number Publication Date
EP3090081A1 EP3090081A1 (de) 2016-11-09
EP3090081B1 true EP3090081B1 (de) 2018-02-07

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Country Status (11)

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US (2) US10883196B2 (ko)
EP (1) EP3090081B1 (ko)
JP (1) JP6456396B2 (ko)
KR (1) KR102196770B1 (ko)
CN (1) CN105849324B (ko)
BR (1) BR112016014441B1 (ko)
ES (1) ES2668695T3 (ko)
PL (1) PL3090081T3 (ko)
PT (1) PT3090081T (ko)
TW (1) TWI667378B (ko)
WO (1) WO2015101543A1 (ko)

Families Citing this family (16)

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Publication number Priority date Publication date Assignee Title
AT515180B1 (de) 2013-10-15 2016-06-15 Chemiefaser Lenzing Ag Dreidimensionaler cellulosischer Formkörper, Verfahren zu seiner Herstellung und seine Verwendung
AT515174B1 (de) 2013-10-15 2019-05-15 Chemiefaser Lenzing Ag Cellulosesuspension, Verfahren zu ihrer Herstellung und Verwendung
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
AT517020B1 (de) 2015-02-06 2020-02-15 Chemiefaser Lenzing Ag Recycling von cellulosischen Kunstfasern
TWI622679B (zh) * 2016-04-29 2018-05-01 財團法人紡織產業綜合研究所 高摩擦性纖維及其製造方法
EP3467163A1 (en) * 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Lyocell filament lining fabric
EP3467171A1 (en) * 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Lyocell filament denim
EP3467161A1 (en) * 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Lyocell type cellulose filament production process
EP3467172A1 (en) 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Silk-like woven garment containing or consisting of lyocell filaments
EP3467174A1 (en) * 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Knitted continuous filament lyocell fabrics
EP3511449B1 (de) 2018-01-15 2022-03-23 Lenzing Aktiengesellschaft Wiederverwendung von lyocell-cellulose für lyocell-verfahren
EP3511874A1 (de) * 2018-01-15 2019-07-17 Lenzing Aktiengesellschaft Kodierung eines celluloseprodukts
TWI814782B (zh) * 2018-03-06 2023-09-11 奧地利商蘭仁股份有限公司 溶劑紡絲之纖維素纖維
EP3536853A1 (en) 2018-03-06 2019-09-11 Lenzing Aktiengesellschaft Lyocell fiber with decreased pill formation
EP3536829A1 (en) * 2018-03-06 2019-09-11 Lenzing Aktiengesellschaft Lyocell fiber with viscose like properties
EP3771755A1 (de) * 2019-08-02 2021-02-03 Lenzing Aktiengesellschaft Verfahren zur herstellung von lyocell-stapelfasern

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BR112016014441B1 (pt) 2021-12-28
ES2668695T3 (es) 2018-05-21
CN105849324B (zh) 2019-07-16
KR20160104643A (ko) 2016-09-05
PL3090081T3 (pl) 2018-07-31
CN105849324A (zh) 2016-08-10
US20210087714A1 (en) 2021-03-25
BR112016014441A2 (pt) 2017-08-08
JP6456396B2 (ja) 2019-01-23
TW201540883A (zh) 2015-11-01
US20160326671A1 (en) 2016-11-10
EP3090081A1 (de) 2016-11-09
WO2015101543A1 (de) 2015-07-09
TWI667378B (zh) 2019-08-01
US10883196B2 (en) 2021-01-05
KR102196770B1 (ko) 2020-12-31
JP2017501315A (ja) 2017-01-12

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