US20120177919A1 - Flame-resistant cellulosic fiber, its use and production process - Google Patents

Flame-resistant cellulosic fiber, its use and production process Download PDF

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Publication number
US20120177919A1
US20120177919A1 US13/392,987 US201013392987A US2012177919A1 US 20120177919 A1 US20120177919 A1 US 20120177919A1 US 201013392987 A US201013392987 A US 201013392987A US 2012177919 A1 US2012177919 A1 US 2012177919A1
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Prior art keywords
flame
resistant
fiber
cellulose
phosphorous
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Gert Kroner
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Lenzing AG
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Lenzing AG
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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
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2933—Coated or with bond, impregnation or core

Definitions

  • the present invention relates to flame-resistant cellulosic regenerated fibers with enhanced usability properties for textile applications which for example also satisfy the requirements of industrial dry cleaning, their use for the production of yarns and fabrics and a process for the production of these fibers.
  • Viscose fibers the flame-resistant effect of which is based on the use of silicates—described for example in patents WO9313249 or CN1847476—are ecologically harmless but do not at all meet the requirements of the modern textile industry with regard to the mechanical fiber properties and washing fastness. According to the present day level of knowledge, only completely water-insoluble solid flame-resistant agents containing phosphorous, which contain no halogens, can fulfill all the demands made in terms of ecology, flame-resistant behavior, the textile data and other usability properties.
  • Patent EP0836634 describes a flame-resistant regenerated fiber produced according to the Lyocell process and which would theoretically fulfill the demands named above.
  • the production of the phosphorous compound used there is, however, not possible on a large scale and, therefore, too expensive so that this fiber does not represent an alternative for conditions in practice.
  • Patents DE4128638A1 or DE102004059221A1 describe flame-resistant dispersion media on the basis of a 2,2′-oxybis[5,5-dimethyl-1,3,2 dioxaphosphorinane]2,2′ disulfide using different dispersion medium systems and also mention the use of these dispersion media for the flame-resistant finishing of viscose fibers.
  • EP1882760 describes the production of flame-retardant viscose fibers using flame-protection dispersion media on the basis of a 2,2′-oxybis[5,5-dimethyl-1,3,2 dioxaphosphorinane]2,2′ disulfid.
  • the particle size may equal a maximum of 10 ⁇ m is described as the most important characteristic of the invention and that the spinning mass, therefore, has to be cleaned before spinning through filters with a maximum aperture width of 10 ⁇ m. It has, however, be seen that this criterion does not suffice to produce fibers which satisfy the demands described here.
  • the maximum particle size described in EP1882760 of 10 ⁇ m is perhaps sufficient for viscose filaments i.e. endless filaments but it does not in any way satisfy the requirements of modern staple fiber production with fiber finenesses of approx. 1 to 4 dtex; a 1.3 dtex fiber has a diameter of approx. 10 ⁇ m.
  • the correlation with the wet modulus measured according to the regulations of BISFA and thus in the following simply referred to as the “BISFA wet modulus” (BISFA, testing methods viscose, Modal, Lyocell and acetate staple fibers and tows, 2004 Edition), is used.
  • the fibers described in the state of the art, or commercially available, are all produced by standard viscose processes. They show by comparison good mechanical fiber data for flame-resistant viscose fibers since the phosphorous contents are very low. Tests with a variety of flame-protection agents on the basis of phosphorous have, however, shown that a sufficient flame-resistant effect is achieved as of a phosphorous content of more than 2.8%. The flame-protection capability correlates very well with the content of flame-protection agent converted to pure phosphorous.
  • flame-resistant fibers could be used to particular advantage in products which are also exposed to strong mechanical loads, for example in professional clothing for particularly dangerous activities in fire brigades, casting mills, the armed forces, the oil and chemical industry.
  • synthetic high-performance fibers such as (aromatic) polyamides, aramides, polyimides and similar products are normally used.
  • these fibers have a low wear comfort since they are not able to absorb moisture to a sufficient extent.
  • the task was to make a flame-resistant cellulosic fiber available which satisfies today's requirements with regard to an economically and ecologically responsible production process and the higher textile mechanical requirements such as for example when industrially dry cleaning the articles of clothing produced in this way.
  • the demands of a flame-resistant fiber for modern textile applications can be described in practical terms by the product with a phosphorous content (this complies with the flame-resistance capacity) and a wet modulus, measured according to the regulations of BISFA (correlates with the area shrinkage).
  • the product with a phosphorous content and BISFA wet modulus is therefore to be designated in the following as the “usability value”.
  • a flame-resistant regenerated cellulose fiber for textile applications which contains an incorporated, particle-shaped phosphorous compound as a flame-resistant substance, preferably an organophosphorus compound and a usability value of between 6 and 35, preferably between 8 and 35 and most preferably between 10 and 35. It was possible to produce a fiber of this kind for the first time by means of a viscose process modified in accordance with the invention.
  • FIG. 1 is a graph showing the correlation between area shrinkage (after washing) and the BISFA wet modulus for viscose fibers.
  • FIG. 2 is graph showing suitable size distributions for pigment dispersions in accordance with the invention.
  • This flame-resistant substance preferably has a particle size distribution with an X 50 value of less than 1.0 ⁇ m and an X 99 value of less than 5.0 ⁇ m.
  • the fiber according to the invention contains at least 2.8%, in a preferred embodiment of the invention preferably between 3.2% and 6.0%, and most preferably between 3.5% and 6.0% of phosphorous in relation to cellulose. Lower contents of phosphorous than 2.8% do not produce a sufficient flame-resistant effect. Higher contents of phosphorous than 6% reduce the mechanical properties of the fibers and are, moreover, no longer economical.
  • a flame-resistant fiber in accordance with the invention is particularly suited which has a BISFA wet modulus B m of more than or equivalent to 0.5 ⁇ ( ⁇ T) ⁇ 10/T with an elongation of 5% in the wet state.
  • T is the titer of an individual fiber, expressed in dtex;
  • B m is expressed in cN/tex.
  • the fiber in accordance with the invention is preferably in the form of a staple fiber i.e. it is cut to a unified length within the course of the production process. Usual cut lengths for staple fibers for the textile field lie between approx. 20 and 150 mm. Only a unified length like this of all of the fibers allows for non-problematic processing on the machines common today in the textile chain with a high productivity.
  • a yarn like this in accordance with the invention can, in addition to the fibers in accordance with the invention, also contain fibers of another origin, for example wool, flame-resistant wool, para and meta aramides, polybenzimidazole (PBI), p-phenyl-2,6-bezobisoxazole (PBO), polyimide (P84®), polyamide-imide (Kermel®), modacryl, polyamide, flame-resistant polyamide, flame-resistant acrylic fibers, melamine fibers, polyester, flame-resistant polyester, polyphenylene sulphide (PPS), polytetrafluorethylene (PTFE), glass fibers, cotton, silk, carbon fibers, oxidized thermally stabilized polyacrylnitrile fibers (
  • this fabric can also contain other fibers, for example and in particular wool, flame-resistant wool, para and meta aramides, polybenzimidazole (PBI), p-phenyl-2,6-bezobisoxazole (PBO), polyimide (P84®), polyamide-imide (Kermel®), modacryl, polyamide, flame-resistant polyamides, flame-resistant acrylic fibers, melamine fibers, polyester, flame-resistant polyester, polyphenylensulphide (PPS), polytetrafluorethylene (PTFE), glass fibers, cotton, silk, carbon fibers, oxidized thermally stabilized polyacrylnitrile fibers (PANOX®) and electrically conductive fibers and blends of these fibers.
  • PBI polybenzimidazole
  • PBO p-phenyl-2,6-bezobisoxazole
  • P84® polyimide
  • Kermel® polyamide-imide
  • modacryl polyamide, flame-resistant polyamides, flame-resistant acrylic fibers,
  • the fabric is preferably a woven fabric, hosiery fabric or knitted fabric, but it can basically also be a non-woven.
  • the use of fibers with a high BISFA wet modulus and a high strength is of decisive importance.
  • the blend of fibers in accordance with the invention with the other fibers is possible either by blending prior to the production of the yarn, a so-called intimate blend, or by the joint use of in each case pure yarns of the different fiber types when weaving, warping or knitting.
  • the fiber in accordance with the invention can be produced using a viscose process in accordance with the invention and modified which is likewise the subject matter of the present invention.
  • Viscose processes for staple fibers and endless filaments have principally been known for many years and are for example described in detail in K. Götze, Chemiefasern nach dem Viskosemaschinen, 1967.
  • the textile properties of the fibers and filaments obtained from this are, however, considerably influenced by many parameters.
  • limits are stipulated for many of the influencing variables due to the design of the existing production units, which can for technical or economic reasons, not be surpassed so that various variations of the parameters are often not possible and the specialist is not even called upon to do this.
  • the subject matter of the invention is, therefore, also a process for the production of a flame-resistant regenerated cellulose fiber for textile applications by spinning a viscose with a content of 4 to 7% cellulose, 5 to 10% NaOH, 36 to 42% (in relation to cellulose) carbon disulphide and 1 to 5% (in relation to cellulose) of a modification agent into a spinning bath, drawing off the coagulated threads, whereby a viscose is used the spinning gamma value of which is 50 to 68, preferably 55 to 58, and the spinning viscosity of which equals 50 to 120 ballfall seconds; and that the temperature of the spinning bath equals 34 to 48° C. whereby
  • a particle shaped organophosphorous compound in the form of a pigment dispersion is incorporated as the flame-resistant substance.
  • the spinning gamma value one understands the share of carbon disulphide molecules bound to 100 cellulose molecules.
  • the spinning gamma value is determined in accordance with Zellcheming-data sheet draft of R. Stahn [1958] respectively sheet III/F 2.
  • the ballfall value stands for the viscosity determined according to the ballfall method; this is expressed in ballfall seconds.
  • the definition is provided in K. Götze, Chemiefasern [1951], p. 175.
  • the flame-resistant phosphorous compound which is made as a pigment, is added to the viscose spinning solution in the form of a pigment dispersion.
  • the finished fiber contains at least 2.6%, preferably between 3.2% and 6.0%, and most preferably between 3.5% and 6.0% of phosphorous, in relation to cellulose.
  • a particularly suitable flame-resistant organophosphorus compound for the purposes of the present invention is the 2,2′-oxybis[5,5-dimethyl-1,3,2-dioxaphosphorinane]2,2′ disulphide.
  • the quality of the pigment dispersion has a considerable influence on the fiber properties. This is determined by the average and maximum particle size of the pigments, the concentration of the dispersion in use, i.e. when adding to the viscose spinning solution, and the type and amount of the dispersing agent.
  • FIG. 2 shows a size distribution of a pigment dispersion still suitable.
  • the pigment dispersion should contain between 10 and 50% of the flame-resistant substance.
  • the dispersing agents which have turned out to be best for the flame-resistant pigment dispersions for the production of fibers in accordance with the invention, which do not have a negative influence on the fiber strength, are those from the group containing modified polycarboxylates, water-soluble polyester, alkyl ether phosphates, end-capped nonoxynols, recinus oil alkoxylester and carboxymethylated alcoholpolyglycolether.
  • the pigment dispersion should contain between 1.5 and 13% of the dispersing agent.
  • the alkali cellulose fleece was disintegrated, ripened and reacted with CS 2 to form the xanthate.
  • the xanthate was dissolved in a diluted soda lye to give a viscose containing 5.6% cellulose, 6.8% NaOH and 39% CS 2 , in relation to the cellulose.
  • the viscose was filtered 4 times and de-aerated.
  • the spinning bath temperature equaled 38° C.
  • the final draw-off speed equaled 42 m/min.
  • the tow was cut to staples of 40 mm length which were fully regenerated in diluted sulphuric acid, then washed free of acid with hot water, desulphurated with soda lye, washed again, bleached with diluted sodium hypochlorite solution, washed out again, finished, squeezed and dried.
  • the jets used reveal a jet diameter of 50 ⁇ m.
  • the spinning bath contains 73 g/l of sulphuric acid, 120 g/l of sodium sulphate and 58 g/l of zinc sulphate.
  • a fiber was produced in accordance with the teachings of CN101037812. Since no indication is made in this publication with regard to the wet modulus, the conditions of the example there with the highest wet strength (example 2, 1,52 cN/tex) of the fiber obtained were selected and in accordance with this, the following process conditions were set: cellulose 8.86%, NaOH 6.24%, 31% CS 2 , in relation to cellulose. A modifying agent was not added. The viscose was spun at a viscosity of 42 ballfall seconds.
  • the nozzles used reveal a nozzle hole diameter of 60 ⁇ m.
  • the spinning bath contains 115 g/l of sulphuric acid, 330 g/l of sodium sulphate and 45 g/l of zinc sulphate.
  • a fiber was produced according to CN1904156 whereby there the concrete recommended process conditions were set:
  • the nozzles used reveal a nozzle hole diameter of 60 ⁇ m.
  • the spinning bath contains 115 g/l of sulphuric acid, 350 g/l of sodium sulphate and 11 g/l of zinc sulphate.
  • the spinning bath temperature equaled 49° C.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)
US13/392,987 2009-09-01 2010-07-27 Flame-resistant cellulosic fiber, its use and production process Abandoned US20120177919A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AT0137109A AT508687A1 (de) 2009-09-01 2009-09-01 Flammgehemmte cellulosische faser, deren verwendung sowie verfahren zu deren herstellung
ATA1371/2009 2009-09-01
PCT/AT2010/000273 WO2011026159A1 (de) 2009-09-01 2010-07-27 Flammgehemmte cellulosische faser, deren verwendung sowie verfahren zu deren herstellung

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US (1) US20120177919A1 (de)
EP (1) EP2473657B1 (de)
CN (1) CN102482800B (de)
AT (1) AT508687A1 (de)
ES (1) ES2487494T3 (de)
TW (1) TWI476309B (de)
WO (1) WO2011026159A1 (de)

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US20140205830A1 (en) * 2011-06-21 2014-07-24 Lenzing Ag High strength cellulosic filament its use, and method for the production thereof
US9828697B2 (en) 2011-05-12 2017-11-28 Glanzstoff Bohemia S.R.O. Flame-retardant regenerated cellulose filament fibers and process for production thereof
JP2019515151A (ja) * 2016-04-28 2019-06-06 レンチング アクチエンゲゼルシャフト 改変されたビスコース繊維
US10456340B2 (en) 2014-10-28 2019-10-29 Lenzing Aktiengesellschaft Liquid-impregnated nonwoven fabric which contains zinc oxide-containing cellulose fibers
CN111148864A (zh) * 2017-10-06 2020-05-12 连津格股份公司 阻燃莱赛尔长丝
US11905630B2 (en) 2019-02-22 2024-02-20 Jess Black Inc. Fire-resistant double-faced fabric of knitted construction

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AT511746B1 (de) * 2011-08-10 2013-12-15 Chemiefaser Lenzing Ag Aktivkohle-enthaltende cellulosische man-made faser sowie verfahren zu deren herstellung und verwendung
TW201335450A (zh) * 2012-02-24 2013-09-01 Acelon Chem & Fiber Corp 具耐燃功能之天然纖維素纖維的製法
ES2569859T3 (es) * 2012-05-14 2016-05-12 Glanzstoff Bohemia S.R.O. Fibras regeneradas de celulosa retardantes de la llama y procedimiento para su fabricación
CN103668619B (zh) * 2012-09-14 2017-06-09 美利肯公司 纱线、纺织品材料及含有其的服装
AT513426A1 (de) * 2012-09-17 2014-04-15 Chemiefaser Lenzing Ag Spinngefärbte Modalfaser, deren Verwendung sowie Verfahren zu deren Herstellung
AT514469B1 (de) * 2013-01-11 2015-04-15 Chemiefaser Lenzing Ag Schwerentflammbares textiles Flächengebilde für Schutzbekleidungs- und Möbelbezugsstoffanwendungen und seine Verwendung
DE102015103187A1 (de) 2014-03-11 2015-09-17 Smartpolymer Gmbh Schwer entflammbare Cellulose-Formkörper, hergestellt nach einem Direktlöseverfahren
CN104988616A (zh) * 2015-05-28 2015-10-21 安徽省含山县顺天纺织有限公司 一种释放负离子具有保健效果的混纺再生棉纱及其制备方法
CN105040207A (zh) * 2015-05-29 2015-11-11 安徽省含山县顺天纺织有限公司 一种工业用具有阻燃效果的聚丙烯纤维再生棉混纺纱及其制备方法
CN104963048A (zh) * 2015-05-29 2015-10-07 安徽省含山县顺天纺织有限公司 一种具有防辐射功效的混纺再生棉纱及其制备方法
CN104988618A (zh) * 2015-05-29 2015-10-21 安徽省含山县顺天纺织有限公司 一种抗拉伸聚丙烯纤维混纺再生棉纱及其制备方法
CN105586679A (zh) * 2016-01-26 2016-05-18 安徽省无为天成纺织有限公司 一种防护服用复合阻燃耐高温混纺纱线
DE102016001910B4 (de) 2016-02-18 2019-10-10 Viscose Faser Gmbh Verfahren zum Bereitstellen einer Pigmentmenge und Verwendung der damit bereitgestellten Pigmentmenge
EP3260595B1 (de) 2016-06-20 2018-05-09 Viscose Faser GmbH Verfahren zur gewinnung von schwer entflammbaren synthesefasern aus textilabfällen
EP3476985A1 (de) 2017-10-27 2019-05-01 Lenzing Aktiengesellschaft Flammgehemmte cellulosische man-made-fasern
EP3754053A1 (de) 2020-05-04 2020-12-23 Lenzing Aktiengesellschaft Spinngefärbte zellulosefaser
CN114059208A (zh) * 2020-07-30 2022-02-18 湖南科力嘉纺织股份有限公司 一种易清洗的纺织用纱线

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
US9828697B2 (en) 2011-05-12 2017-11-28 Glanzstoff Bohemia S.R.O. Flame-retardant regenerated cellulose filament fibers and process for production thereof
US20140205830A1 (en) * 2011-06-21 2014-07-24 Lenzing Ag High strength cellulosic filament its use, and method for the production thereof
US10456340B2 (en) 2014-10-28 2019-10-29 Lenzing Aktiengesellschaft Liquid-impregnated nonwoven fabric which contains zinc oxide-containing cellulose fibers
JP2019515151A (ja) * 2016-04-28 2019-06-06 レンチング アクチエンゲゼルシャフト 改変されたビスコース繊維
CN111148864A (zh) * 2017-10-06 2020-05-12 连津格股份公司 阻燃莱赛尔长丝
US11905630B2 (en) 2019-02-22 2024-02-20 Jess Black Inc. Fire-resistant double-faced fabric of knitted construction

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TWI476309B (zh) 2015-03-11
EP2473657B1 (de) 2014-04-30
AT508687A1 (de) 2011-03-15
CN102482800B (zh) 2015-04-22
ES2487494T3 (es) 2014-08-21
TW201129744A (en) 2011-09-01
CN102482800A (zh) 2012-05-30
EP2473657A1 (de) 2012-07-11

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