EP2280100A1 - Use of a regenerated cellulose fibre in a flame-retarded product - Google Patents

Use of a regenerated cellulose fibre in a flame-retarded product Download PDF

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Publication number
EP2280100A1
EP2280100A1 EP20090450141 EP09450141A EP2280100A1 EP 2280100 A1 EP2280100 A1 EP 2280100A1 EP 20090450141 EP20090450141 EP 20090450141 EP 09450141 A EP09450141 A EP 09450141A EP 2280100 A1 EP2280100 A1 EP 2280100A1
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EP
European Patent Office
Prior art keywords
fiber
flame
cellulose
cellulose fiber
regenerated 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.)
Withdrawn
Application number
EP20090450141
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German (de)
French (fr)
Inventor
Ingo Bernt
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.)
Kelheim Fibres GmbH
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Kelheim Fibres GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Kelheim Fibres GmbH filed Critical Kelheim Fibres GmbH
Priority to EP20090450141 priority Critical patent/EP2280100A1/en
Priority to PCT/EP2010/059867 priority patent/WO2011012422A1/en
Priority to US13/387,270 priority patent/US20120219784A1/en
Priority to JP2012522073A priority patent/JP2013501150A/en
Priority to CN2010800341913A priority patent/CN102639768A/en
Priority to EP10729914A priority patent/EP2459783A1/en
Priority to KR20127005141A priority patent/KR20120065339A/en
Priority to CA 2767932 priority patent/CA2767932A1/en
Publication of EP2280100A1 publication Critical patent/EP2280100A1/en
Withdrawn legal-status Critical Current

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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
    • A—HUMAN NECESSITIES
    • A41—WEARING APPAREL
    • A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
    • A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
    • 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
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/20—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
    • D03D15/283—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads synthetic polymer-based, e.g. polyamide or polyester fibres
    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/50—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the properties of the yarns or threads
    • 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
    • D10B2501/00—Wearing apparel
    • 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
    • D10B2503/00—Domestic or personal
    • 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
    • D10B2505/00—Industrial
    • D10B2505/04—Filters
    • 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
    • D10B2505/00—Industrial
    • D10B2505/12—Vehicles
    • 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
    • Y10T428/249921—Web or sheet containing structurally defined element or component
    • 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
    • Y10T428/298—Physical dimension

Definitions

  • the present invention relates to the use of a regenerated cellulose fiber obtained by the viscose process in flame retardant products.
  • Flame retardant viscose fibers have many uses such as e.g. in safety clothing; Mattress stuffing; Interior fabrics, etc. and are for general safety.
  • Such aftertreated textiles / fibers but have only a limited wash resistance.
  • the crosslinking chemistry used produces residual amounts of formaldehyde, which is harmful to health.
  • the crosslinking reaction causes embrittlement and stiffening of the fibers / textiles.
  • the object of the present invention is to provide a low-cost and effectively effective flame-retardant fiber which is easy to process in the usual textile processes.
  • This object is achieved by the use of a regenerated cellulose fiber incorporating carboxymethyl cellulose in a flame retardant product.
  • CMC carboxymethylcellulose
  • Viscose fibers with a content of carboxymethylcellulose are known. It is a mixed fiber, which is obtained by the spinning of carboxymethyl cellulose in the Viskosepinnmasse. Such fibers have also been produced commercially ( US 4,199,367 A . US 4,289,824 A ).
  • a Viskosepinnmasse is prepared by the usual methods.
  • An 8-12% by weight solution of carboxymethylcellulose (CMC) is added to the dope immediately prior to spinning, so that the desired amount of incorporation relative to underivatized cellulose results.
  • Post-processing and drying are carried out by the usual methods.
  • the proportion of incorporated carboxymethyl cellulose in the regenerated cellulose fiber is preferably 5% by weight to 50% by weight, more preferably 15% by weight to 40% by weight, most preferably 20% by weight to 30% by weight, based on underivatized cellulose ,
  • the carboxymethylcellulose may be a commercial product having a degree of substitution DS of 0.6-1.2, preferably 0.65-0.85 and a viscosity (2% solution, 25 ° C) of 30-800 mPas; preferably 50-100 mPas.
  • the CMC-containing regenerated cellulose fiber used in the present invention will hereinafter also be referred to as "viscose / CMC mixed fiber”.
  • the fiber titer of the viscose / CMC mixed fiber is preferably from 0.5 dtex to 8 dtex, more preferably from 1.3 to 6 dtex.
  • the fiber length of the viscose / CMC mixed fiber used according to the invention can be from 2 mm to 80 mm and depends in particular on the field of application. In particular, fiber lengths of 2 to 20 mm are suitable for a wetlaid process, and fiber lengths of 20 to 80 mm for a carding process.
  • Viscose / CMC blended fiber preferably contains another flame retardant additive.
  • This further additive may in particular be selected from the group consisting of halogen-containing additives, phosphorus-containing additives, aluminum and magnesium salts and polysilicic acids.
  • the other additive may in manner known per se by one spinning in the viscose spinning in fiber incorporated (eg in the case of phosphorus containing additives such as Exolit ® 5060) or be subsequently applied to the fiber (such as in the case of alkaline solutions of an aluminum salt) ,
  • viscose / CMC blended fibers used according to the invention differ in their properties - in contrast to some previously known flame-retardant viscose fibers
  • CMC additive used for the fibers according to the invention
  • the present invention also relates to a flame retardant product containing a regenerated cellulose fiber in which carboxymethyl cellulose is incorporated.
  • the flame retardant product according to the invention is preferably characterized in that the proportion of incorporated carboxymethylcellulose in the cellulose fiber is 5% by weight to 50% by weight, preferably 15% by weight to 40% by weight, particularly preferably 20% by weight to 30% by weight. , based on underivatized cellulose.
  • the flame retardant product according to the invention may preferably contain the viscose / CMC mixed fiber in a proportion of 10% to 100%.
  • the flame-retardant product according to the invention is preferably selected from the group consisting of clothing, in particular protective clothing, home textiles, in particular mattresses, automotive textiles, filter materials and insulation material for the construction and automotive sector.
  • Viscose / CMC mixed staple fibers with a proportion of 0% (zero pattern), 12% by weight, 20% by weight and 30% by weight of CMC based on underivatized cellulose were prepared in a manner known per se. The fibers were cut to a staple length of 40 mm.
  • Rotor rings of 10g were made from the fiber samples.
  • the rotor rings were then opened and pressed through a tampon calender.
  • the produced tapes have a surface weight of about 238 g / m 2 (206-260 g / m 2 ) at a thickness of about 5 mm.
  • For the fire tests specimens of size 8 x 2 cm were cut. The specimens were clamped horizontally or vertically and the free end of the sample was ignited with a Bunsen burner for a defined period of time.
  • the patterns were already inflamed at 1 s flame time and then burned with a lively flame until complete combustion.
  • Viscose fibers with 12% or 20% CMC (according to the invention):
  • test piece burns in direct contact with the burner flame. If the flame is removed, the sample will extinguish immediately ("self-extinguishing"). In some cases, after removal of the flame, individual fibers protruding loosely from the test piece burned off the surface.
  • the flame time was varied from 1s - 10s. All samples quenched immediately after removal of the flame. It only increased the proportion burned by prolonged contact with the burner flame.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Physical Education & Sports Medicine (AREA)
  • Artificial Filaments (AREA)

Abstract

Use of a regenerated cellulose fiber, into which carboxymethyl cellulose is incorporated, in a flame-retardant product, is claimed. An independent claim is included for the flame-retardant product containing the cellulose fiber.

Description

Die vorliegende Erfindung betrifft die Verwendung einer regenerierten Cellulosefaser, die durch das Viskoseverfahren erhalten wird, in flammhemmenden Produkten.The present invention relates to the use of a regenerated cellulose fiber obtained by the viscose process in flame retardant products.

Flammhemmende Viskose-Fasern haben viele Einsatzgebiete wie z.B. in Sicherheitsbekleidung; Matratzenfüllungen; Innenraum-Stoffen etc. und dienen der allgemeinen Sicherheit.Flame retardant viscose fibers have many uses such as e.g. in safety clothing; Mattress stuffing; Interior fabrics, etc. and are for general safety.

Es sind bereits verschiedenste Typen von flammhemmenden Viskosefasern bekannt:Various types of flame-retardant viscose fibers are already known:

Zum einen ist es bekannt, Viskosefasern durch die Einlagerung von Polykieselsäure flammhemmend auszurüsten. Die Einlagerung von Polykieselsäure führt aber zur Bildung von steifen, spröden Fasern, die zwar für Vliesstoffe, nicht aber für textile Anwendungen geeignet sind.On the one hand, it is known to provide viscose fibers flame retardant by the incorporation of polysilicic acid. However, the incorporation of polysilicic acid leads to the formation of stiff, brittle fibers, which are suitable for nonwovens, but not for textile applications.

Unter dem Markennamen Lenzing FR® werden Viskosefasern vermarktet, die durch Einlagerung eines phosphorhaltigen Additivs gewonnen werden. Um mit phosphorhaltigen Additiven einen ausreichenden Flammschutz zu erreichen, muß aber eine große Einlagerungshöhe eingesetzt werden. Dies führt aufgrund der hohen Additivkosten zu einem hohen Endpreis der Faser.Under the brand name Lenzing FR ® viscose fibers are marketed, which are obtained by incorporation of a phosphorus-containing additive. In order to achieve sufficient flame retardancy with phosphorus-containing additives, however, a large storage height must be used. This leads to a high final price of the fiber due to the high additive costs.

Es gibt auch eine Vielzahl von Vorschlägen für eine nachträgliche flammhemmende Ausrüstung von Cellulosefasern, d.h. eine Aufbringung auf die bereits fertige Faser, wie z.B. Proban (THPC) und Pyrovatex® CP.There are also a variety of proposals for a subsequent flame retardant equipment of cellulose fibers, ie an application to the already finished fiber, such as Proban (THPC) and Pyrovatex ® CP.

Solcherart nachbehandelte Textilien/Fasern weisen aber nur eine beschränkte Waschbeständigkeit auf. Durch die eingesetzte Vernetzungschemie entstehen Restmengen an Formaldehyd, welches gesundheitlich bedenklich ist. Zudem bewirkt die Vernetzungsreaktion eine Versprödung und Versteifung der Fasern/Textilien.Such aftertreated textiles / fibers but have only a limited wash resistance. The crosslinking chemistry used produces residual amounts of formaldehyde, which is harmful to health. In addition, the crosslinking reaction causes embrittlement and stiffening of the fibers / textiles.

Die US 3 734 683 beschreibt den flammhemmenden Effekt von cellulosischen Fasern mit höherem Carboxylgruppenanteil durch Herstellung einer Carboxycellulose. Gemäß dieser Druckschrift werden Viskosefasern in einem aufwendigen Verfahren mit Stickstoffdioxid oxidiert und anschließend nachbehandelt. In einem wirtschaftlich sinnvollen Prozeß zur Faserherstellung lässt sich dieses Verfahren nicht umsetzen. Die genannte Oxidation würde außerdem zu einer Schädigung der Faserstruktur und einer mangelhaften Verarbeitbarkeit führen.The US 3,734,683 describes the flame retardant effect of higher carboxyl group content cellulosic fibers by producing a carboxycellulose. According to this publication, viscose fibers are oxidized in a complex process with nitrogen dioxide and then aftertreated. In an economically meaningful process for fiber production, this process can not be implemented. The said oxidation would also lead to damage to the fiber structure and poor processibility.

Die Aufgabe der vorliegenden Erfindung besteht darin, eine kostengünstige und effektiv wirksame flammhemmende Faser zur Verfügung zu stellen, die in den üblichen textilen Prozessen gut verarbeitbar ist.The object of the present invention is to provide a low-cost and effectively effective flame-retardant fiber which is easy to process in the usual textile processes.

Diese Aufgabe wird mit der Verwendung einer regenerierten Cellulosefaser, in welche Carboxymethylcellulose inkorporiert ist, in einem flammhemmenden Produkt, gelöst.This object is achieved by the use of a regenerated cellulose fiber incorporating carboxymethyl cellulose in a flame retardant product.

Bevorzugte Ausführungsformen sind in den Unteransprüchen aufgeführtPreferred embodiments are listed in the subclaims

DETALLIERTE BESCHREIBUNG DER ERFINDUNGDETAILED DESCRIPTION OF THE INVENTION

Es hat sich überraschenderweise gezeigt, dass eine regenerierte Cellulosefaser, welche Carboxymethylcellulose (CMC) inkorporiert hat, effektiv flammhemmend wirkt und sowohl vergleichsweise günstig herstellbar als auch gut verarbeitbar ist.It has surprisingly been found that a regenerated cellulose fiber, which has incorporated carboxymethylcellulose (CMC), effectively acts flame retardant and is both relatively inexpensive to produce and easy to process.

Unter der Maßnahme, dass in die Faser Carboxymethylcellulose inkorporiert ist, versteht der Fachmann, dass in die Matrix der (nach Regeneration der Faser) underivatisierten Cellulose CMC eingelagert ist. Dies ist - im Unterschied zu einem Aufbringen von CMC auf die bereits fertige Faser - insbesondere durch Einspinnnen von CMC in die Spinnviskose möglich.Under the measure that incorporated into the fiber carboxymethylcellulose, the skilled worker understands that in the matrix of (after regeneration of the fiber) underivatized cellulose CMC is embedded. This is possible - in contrast to applying CMC to the already finished fiber - in particular by spinning CMC into the spinning viscose.

Viskosefasern mit einem Anteil an Carboxymethylcellulose (CMC) sind bekannt. Es handelt sich dabei um eine Mischfaser, die durch das Einspinnen von Carboxymethylcellulose in die Viskosespinnmasse erhalten wird. Solche Fasern wurden auch kommerziell hergestellt ( US 4,199,367 A , US 4,289,824 A ).Viscose fibers with a content of carboxymethylcellulose (CMC) are known. It is a mixed fiber, which is obtained by the spinning of carboxymethyl cellulose in the Viskosepinnmasse. Such fibers have also been produced commercially ( US 4,199,367 A . US 4,289,824 A ).

Beispielsweise wird dazu nach den üblichen Verfahren eine Viskosespinnmasse hergestellt. Der Spinnmasse wird unmittelbar vor dem Ausspinnen eine 8-12 Gew.%ige Lösung von Carboxymethylcellulose (CMC) zugesetzt, so dass sich die gewünschte Einlagerungsmenge bezogen auf underivatisierte Cellulose ergibt. Nachbearbeitung und Trocknung erfolgen nach den üblichen Verfahren.For example, a Viskosepinnmasse is prepared by the usual methods. An 8-12% by weight solution of carboxymethylcellulose (CMC) is added to the dope immediately prior to spinning, so that the desired amount of incorporation relative to underivatized cellulose results. Post-processing and drying are carried out by the usual methods.

Der Anteil an inkorporierter Carboxymethylcellulose in der regenerierten Cellulosefaser beträgt bevorzugt 5 Gew.% bis 50 Gew.%, besonders bevorzugt 15 Gew.% bis 40 Gew.%, am meisten bevorzugt 20 Gew.% bis 30 Gew.%, bezogen auf underivatisierte Cellulose.The proportion of incorporated carboxymethyl cellulose in the regenerated cellulose fiber is preferably 5% by weight to 50% by weight, more preferably 15% by weight to 40% by weight, most preferably 20% by weight to 30% by weight, based on underivatized cellulose ,

Die Carboxymethylcellulose kann ein handelsübliches Produkt mit einem Substitutionsgrad DS von 0,6 - 1,2, bevorzugt 0,65 - 0,85 und einer Viskosität (2%ige Lösung; 25°C) von 30-800 mPas; bevorzugt 50-100 mPas sein.The carboxymethylcellulose may be a commercial product having a degree of substitution DS of 0.6-1.2, preferably 0.65-0.85 and a viscosity (2% solution, 25 ° C) of 30-800 mPas; preferably 50-100 mPas.

Die erfindungsgemäß verwendete CMC enthaltende regenerierte Cellulosefaser wird im folgenden auch als "Viskose/CMC-Mischfaser" bezeichnet.The CMC-containing regenerated cellulose fiber used in the present invention will hereinafter also be referred to as "viscose / CMC mixed fiber".

Der Fasertiter der Viskose/CMC-Mischfaser beträgt bevorzugt von 0,5 dtex bis 8 dtex, besonders bevorzugt von 1,3 bis 6 dtex.The fiber titer of the viscose / CMC mixed fiber is preferably from 0.5 dtex to 8 dtex, more preferably from 1.3 to 6 dtex.

Die Faserlänge der erfindungsgemäß eingesetzten Viskose/CMC-Mischfaser kann von 2 mm bis 80 mm betragen und hängt insbesondere vom Anwendungsgebiet ab. Für einen Wetlaidprozess sind insbesondere Faserlängen von 2 bis 20 mm geeignet, für einen Kardierprozess Faserlängen von 20 bis 80 mm.The fiber length of the viscose / CMC mixed fiber used according to the invention can be from 2 mm to 80 mm and depends in particular on the field of application. In particular, fiber lengths of 2 to 20 mm are suitable for a wetlaid process, and fiber lengths of 20 to 80 mm for a carding process.

Bevorzugt enthält Viskose/CMC-Mischfaser ein weiteres flammhemmendes Additiv. Dieses weitere Additiv kann insbesondere aus der Gruppe bestehend aus halogenhaltigen Additiven, phosphorhaltigen Additiven, Aluminium- und Magnesiumsalzen und Polykieselsäuren ausgewählt ist. Das weitere Additiv kann in an sich bekannter Weise durch Einspinnen in die Viskosespinnmasse in der Faser inkorporiert sein (z.B. im Fall von phosphorhältigen Additiven wie z.B. Exolit® 5060) oder nachträglich auf die Faser aufgebracht werden (wie z.B. im Fall von alkalischen Lösungen eines Aluminiumsalzes).Viscose / CMC blended fiber preferably contains another flame retardant additive. This further additive may in particular be selected from the group consisting of halogen-containing additives, phosphorus-containing additives, aluminum and magnesium salts and polysilicic acids. The other additive may in manner known per se by one spinning in the viscose spinning in fiber incorporated (eg in the case of phosphorus containing additives such as Exolit ® 5060) or be subsequently applied to the fiber (such as in the case of alkaline solutions of an aluminum salt) ,

Die erfindungsgemäß eingesetzten Viskose/CMC-Mischfasern, bzw. Textilien oder Vliesstoffe, welche diese enthalten, brennen im Unterschied zu Viskose-Fasern bzw. Produkten aus reinen Viskose-Fasern nach dem Entzünden nicht weiter. Vielmehr verlöscht die Flamme unmittelbar und die Faser glimmt lediglich weiter. Besonders ausgeprägt ist dieser Effekt ab einer Einlagerung ab 20 Gew.% CMC bezogen auf underivatisierte Cellulose.The viscose / CMC mixed fibers used according to the invention, or textiles or nonwovens which contain them, in contrast to viscose fibers or products made of pure viscose fibers do not burn after ignition. Rather, the flame extinguishes immediately and the fiber just continues to glow. This effect is particularly pronounced from a storage from 20 wt.% CMC based on underivatized cellulose.

Die erfindungsgemäß eingesetzten Viskose/CMC-Mischfasern Fasern unterscheiden sich aber - im Unterschied zu einigen vorbekannten flammgehemmten Viskosefasern - in ihrenThe viscose / CMC blended fibers used according to the invention, however, differ in their properties - in contrast to some previously known flame-retardant viscose fibers

Festigkeits- und Dehnungswerten und auch ihrer Elastizität nicht wesentlich von herkömmlichen Viskosefasern und lassen sich somit genauso verarbeiten wie diese.Strength and elongation values and also their elasticity are not significantly different from conventional viscose fibers and can therefore be processed just like these.

Das für die erfindungsgemäßen Fasern eingesetzte Additiv (CMC) ist gesundheitlich unbedenklich und wird sogar als Lebensmitteladditiv verwendet. Eine Versprödung und Versteifung der Fasern findet nicht statt. Der flammhemmende Effekt ist unbegrenzt waschbeständig.The additive used for the fibers according to the invention (CMC) is harmless to health and is even used as a food additive. Embrittlement and stiffening of the fibers does not take place. The flame-retardant effect is indefinitely washable.

Dementsprechend betrifft die vorliegende Erfindung auch ein flammhemmendes Produkt, enthaltend eine regenerierte Cellulosefaser, in welcher Carboxymethylcellulose inkorporiert ist.Accordingly, the present invention also relates to a flame retardant product containing a regenerated cellulose fiber in which carboxymethyl cellulose is incorporated.

Das erfindungsgemäße flammhemmende Produkt ist bevorzugt dadurch gekennzeichnet, dass der Anteil an inkorporierter Carboxymethylcellulose in der Cellulosefaser 5 Gew.% bis 50 Gew.%, bevorzugt 15 Gew.% bis 40 Gew.%, besonders bevorzugt 20 Gew.% bis 30 Gew.%, bezogen auf underivatisierte Cellulose beträgt.The flame retardant product according to the invention is preferably characterized in that the proportion of incorporated carboxymethylcellulose in the cellulose fiber is 5% by weight to 50% by weight, preferably 15% by weight to 40% by weight, particularly preferably 20% by weight to 30% by weight. , based on underivatized cellulose.

Das erfindungsgemäße flammhemmende Produkt kann bevorzugt die Viskose/CMC-Mischfaser in einem Anteil von 10% - 100% enthalten.The flame retardant product according to the invention may preferably contain the viscose / CMC mixed fiber in a proportion of 10% to 100%.

Das erfindungsgemäße flammhemmende Produkt ist bevorzugt aus der Gruppe bestehend aus Bekleidung, insbesondere Schutzbekleidung, Heimtextilien, insbesondere Matratzen, Automobiltextilien, Filtermaterialien und Isolationsmaterial für den Bau- und Automobilbereich ausgewählt.The flame-retardant product according to the invention is preferably selected from the group consisting of clothing, in particular protective clothing, home textiles, in particular mattresses, automotive textiles, filter materials and insulation material for the construction and automotive sector.

BEISPIELE:EXAMPLES:

Es wurden auf an sich bekannte Weise Viskose/CMC-Mischstapelfasern mit einem Anteil von 0% (Nullmuster), 12 Gew.%, 20 Gew.% und 30 Gew.% CMC bezogen auf underivatisierte Cellulose hergestellt. Die Fasern wurden auf eine Stapellänge von 40 mm geschnitten.Viscose / CMC mixed staple fibers with a proportion of 0% (zero pattern), 12% by weight, 20% by weight and 30% by weight of CMC based on underivatized cellulose were prepared in a manner known per se. The fibers were cut to a staple length of 40 mm.

Aus den Faserproben wurden Rotorringe zu je 10g hergestellt. Die Rotorringe wurden anschließend geöffnet und durch einen Tamponkalander verpresst. Die hergestellten Bänder haben ein Flächengewicht von ca. 238g/m2 (206 - 260 g/m2) bei einer Dicke von ca. 5mm. Für die Brandtests wurden Prüflinge der Größe 8 x 2 cm geschnitten. Die Prüfkörper wurden horizontal oder vertikal eingespannt und das freie Ende der Probe mit einem Bunsenbrenner für einen definierten Zeitraum beflammt.Rotor rings of 10g each were made from the fiber samples. The rotor rings were then opened and pressed through a tampon calender. The produced tapes have a surface weight of about 238 g / m 2 (206-260 g / m 2 ) at a thickness of about 5 mm. For the fire tests specimens of size 8 x 2 cm were cut. The specimens were clamped horizontally or vertically and the free end of the sample was ignited with a Bunsen burner for a defined period of time.

Ergebnisse:Results:

Herkömmliche Viskosefaser (0% CMC):Conventional viscose fiber (0% CMC):

Die Muster entzündeten sich bereits bei 1 s Beflammzeit und brannten anschließend mit lebhafter Flamme bis zur vollständigen Verbrennung weiter.The patterns were already inflamed at 1 s flame time and then burned with a lively flame until complete combustion.

Viskosefasern mit 12% bzw. 20% CMC (erfindungsgemäß):Viscose fibers with 12% or 20% CMC (according to the invention):

Der Prüfkörper verbrennt bei direktem Kontakt mit der Brennerflamme. Bei Wegnahme der Flamme verlöscht die Probe aber sofort ("selbstverlöschend"). In einigen Fällen brannten nach Wegnahme der Flamme noch locker aus dem Prüfkörper herausstehend Einzelfasern an der Oberfläche ab.The test piece burns in direct contact with the burner flame. If the flame is removed, the sample will extinguish immediately ("self-extinguishing"). In some cases, after removal of the flame, individual fibers protruding loosely from the test piece burned off the surface.

Die Beflammzeit wurde von 1s - 10s variiert. Alle Proben verlöschten unmittelbar nach Wegnahme der Flamme. Es erhöhte sich lediglich der verbrannte Anteil durch längeren Kontakt mit der Brennerflamme.The flame time was varied from 1s - 10s. All samples quenched immediately after removal of the flame. It only increased the proportion burned by prolonged contact with the burner flame.

Alle Proben glimmten nach dem Verlöschen nach. So kam es in allen Fällen zu einer langsamen vollständigen Veraschung der Prüfkörper.All samples smoldered after extinguishing. Thus, in all cases, slow complete ashing of the specimens occurred.

Claims (10)

Verwendung einer regenerierten Cellulosefaser, in welche Carboxymethylcellulose inkorporiert ist, in einem flammhemmenden Produkt.Use of a regenerated cellulose fiber incorporating carboxymethyl cellulose in a flame retardant product. Verwendung gemäß Anspruch 1, dadurch gekennzeichnet, dass der Anteil an inkorporierter Carboxymethylcellulose in der Cellulosefaser 5 Gew.% bis 50 Gew.%, bevorzugt 15 Gew.% bis 40 Gew.%, besonders bevorzugt 20 Gew.% bis 30 Gew.%, bezogen auf underivatisierte Cellulose beträgt.Use according to claim 1, characterized in that the proportion of incorporated carboxymethylcellulose in the cellulose fiber 5 wt.% To 50 wt.%, Preferably 15 wt.% To 40 wt.%, Particularly preferably 20 wt.% To 30 wt.%, based on underivatized cellulose. Verwendung gemäß Anspruch 1 oder 2, dadurch gekennzeichnet dass der Fasertiter der Cellulosefaser zwischen 0,5 dtex und 8 dtex, bevorzugt zwischen 1,3 und 6 dtex liegt.Use according to claim 1 or 2, characterized in that the fiber titer of the cellulose fiber is between 0.5 dtex and 8 dtex, preferably between 1.3 and 6 dtex. Verwendung gemäß einem der vorhergehenden Ansprüche, dadurch gekennzeichnet dass die Faserlänge der Cellulosefaser von 2 mm bis 80 mm beträgt.Use according to one of the preceding claims, characterized in that the fiber length of the cellulose fiber of 2 mm to 80 mm. Verwendung gemäß einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Faser ein weiteres flammhemmendes Additiv enthält.Use according to one of the preceding claims, characterized in that the fiber contains a further flame-retardant additive. Verwendung gemäß Anspruch 5, dadurch gekennzeichnet, dass das weitere flammhemmende Additiv aus der Gruppe bestehend aus halogenhaltigen Additiven, phosphorhaltigen Additiven, Aluminium- und Magnesiumsalzen und Polykieselsäuren ausgewählt ist.Use according to claim 5, characterized in that the further flame-retardant additive is selected from the group consisting of halogen-containing additives, phosphorus-containing additives, aluminum and magnesium salts and polysilicic acids. Flammhemmendes Produkt, enthaltend eine regenerierte Cellulosefaser, in welcher Carboxymethylcellulose inkorporiert ist.A flame-retardant product containing a regenerated cellulose fiber in which carboxymethylcellulose is incorporated. Flammhemmendes Produkt gemäß Anspruch 7, dadurch gekennzeichnet, dass der Anteil an inkorporierter Carboxymethylcellulose in der Cellulosefaser 5 Gew.% bis 50 Gew.%, bevorzugt 15 Gew.% bis 40 Gew.%, besonders bevorzugt 20 Gew.% bis 30 Gew.%, bezogen auf underivatisierte Cellulose beträgt.Flame retardant product according to claim 7, characterized in that the proportion of incorporated carboxymethyl cellulose in the cellulose fiber 5 wt.% To 50 wt.%, Preferably 15 wt.% To 40 wt.%, Particularly preferably 20 wt.% To 30 wt.% , based on underivatized cellulose. Flammhemmendes Produkt gemäß einem der Ansprüche 7 oder 8, dadurch gekennzeichnet, dass es die regenerierte Cellulosefaser in einem Anteil von 10% - 100% enthält.Flame retardant product according to one of claims 7 or 8, characterized in that it contains the regenerated cellulose fiber in a proportion of 10% - 100%. Flammhemmendes Produkt gemäß einem der Ansprüche 7 bis 9, ausgewählt aus der Gruppe bestehend aus Bekleidung, insbesondere Schutzbekleidung, Heimtextilien, insbesondere Matratzen, Automobiltextilien, Filtermaterialien und Isolationsmaterial für den Bau- und Automobilbereich.Flame retardant product according to one of claims 7 to 9, selected from the group consisting of clothing, in particular protective clothing, home textiles, in particular mattresses, automotive textiles, filter materials and insulation material for the construction and automotive sector.
EP20090450141 2009-07-31 2009-07-31 Use of a regenerated cellulose fibre in a flame-retarded product Withdrawn EP2280100A1 (en)

Priority Applications (8)

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EP20090450141 EP2280100A1 (en) 2009-07-31 2009-07-31 Use of a regenerated cellulose fibre in a flame-retarded product
PCT/EP2010/059867 WO2011012422A1 (en) 2009-07-31 2010-07-09 Use of a regenerated cellulose fibre in a flame-retardant product
US13/387,270 US20120219784A1 (en) 2009-07-31 2010-07-09 Use of a regenerated cellulose fiber in a flame-retardant product
JP2012522073A JP2013501150A (en) 2009-07-31 2010-07-09 Use of regenerated cellulose fiber
CN2010800341913A CN102639768A (en) 2009-07-31 2010-07-09 Use of a regenerated cellulose fibre in a flame-retardant product
EP10729914A EP2459783A1 (en) 2009-07-31 2010-07-09 Use of a regenerated cellulose fibre in a flame-retardant product
KR20127005141A KR20120065339A (en) 2009-07-31 2010-07-09 Use of a regenerated cellulose fibre in a flame-retardant product
CA 2767932 CA2767932A1 (en) 2009-07-31 2010-07-09 Use of a regenerated cellulose fibre

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DE102011101321A1 (en) * 2011-05-12 2012-11-15 Glanzstoff Bohemia S.R.O. Flame-retardant cellulose regenerated filament fibers and process for its preparation
CN104357935B (en) * 2014-11-13 2016-04-06 山西瑞赛格纺织科技有限公司 A kind of composite flame-retardant agent slurry for regenerated celulose fibre
CN105603555B (en) * 2016-02-02 2017-11-10 九江消防装备有限公司 A kind of bio-based composite flame-proof material and preparation method and application
CN111172615A (en) * 2020-01-20 2020-05-19 天津科技大学 Flame-retardant nano-cellulose composite fiber prepared by wet spinning and preparation process thereof

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US3974251A (en) * 1973-03-07 1976-08-10 Hoechst Aktiengesellschaft Production of flameproof fibers of regenerated cellulose
US4199367A (en) 1975-11-07 1980-04-22 Avtex Fibers Inc. Alloy rayon
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KR20120065339A (en) 2012-06-20
US20120219784A1 (en) 2012-08-30
EP2459783A1 (en) 2012-06-06
WO2011012422A1 (en) 2011-02-03
CN102639768A (en) 2012-08-15
CA2767932A1 (en) 2011-02-03

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