EP0904444B1 - Process for treating cellulose fibres and structures made of those fibres - Google Patents

Process for treating cellulose fibres and structures made of those fibres Download PDF

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Publication number
EP0904444B1
EP0904444B1 EP97926908A EP97926908A EP0904444B1 EP 0904444 B1 EP0904444 B1 EP 0904444B1 EP 97926908 A EP97926908 A EP 97926908A EP 97926908 A EP97926908 A EP 97926908A EP 0904444 B1 EP0904444 B1 EP 0904444B1
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Prior art keywords
fibres
textile
carbon atoms
fibers
auxiliary agent
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German (de)
French (fr)
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EP0904444A1 (en
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Markus Eibl
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Lenzing AG
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Lenzing AG
Chemiefaser 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
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/35—Heterocyclic compounds
    • D06M13/355—Heterocyclic compounds having six-membered heterocyclic rings
    • D06M13/358—Triazines
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/0004—General aspects of dyeing
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/64—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
    • D06P1/642—Compounds containing nitrogen
    • D06P1/6426—Heterocyclic compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/58—Material containing hydroxyl groups
    • D06P3/60—Natural or regenerated cellulose
    • D06P3/66—Natural or regenerated cellulose using reactive dyes

Definitions

  • the invention relates to a method for the treatment of Cellulose fibers and of structures made from these cellulose fibers which process the fibers or the fiber structures with a Textile auxiliaries are brought into contact with the fibers to give improved properties.
  • the invention relates also new fiber structures, e.g. Yarns and textile surfaces, which can be obtained using this procedure.
  • WO 92/07124 describes a method for producing a Fiber with reduced tendency to fibrillation, according to which the fresh spun, i.e. not yet dried, fiber with one cationic polymer is treated.
  • a polymer with imidazole and azetidine groups As such a polymer called a polymer with imidazole and azetidine groups.
  • treatment with an emulsifiable Polymer e.g. Polyethylene or polyvinyl acetate, or also crosslinking with glyoxal.
  • EP-A - 0 538 977 and WO 94/09191 describe a method of the type mentioned, in which fibers of the genus Lyocell to reduce the tendency to fibrillation with a Textile auxiliaries are brought into contact.
  • WO 94/24343 describes a process for the production of Cellulose fibers with reduced tendency to fibrillation, in which Process a solution of cellulose in a tertiary amine oxide spun into fibers and the freshly spun fibers with one Textile auxiliaries carrying at least two reactive groups, contacted and washed with an aqueous buffer be used as a textile auxiliary not glyoxal becomes. According to this previously known method, the fresh spun fibers with the textile auxiliary is best in one alkaline environment.
  • the invention has for its object a method for Treatment of cellulose fibers of the Lyocell genus and Formed from these fibers to provide that on can be carried out in a simple manner and that enables the treated fibers have a reduced tendency to fibrillation or treated fiber structures or treated fibers Fiber structures have improved abrasion and pilling values.
  • the process according to the invention for the treatment of cellulose fibers, in which the fibers are brought into contact with a textile auxiliary, is characterized in that a compound having the general formula is used as the textile auxiliary or their alkali salt is used, where X is halogen, alkoxy with 1-4 carbon atoms, amino, alkylamino with 1-4 carbon atoms, hydroxysulfonyl, or 1-nicotinyl; Y the general formula in which n is the number 1 or 2; R 1 is hydrogen, alkyl of 1-4 carbon atoms or phenyl; R 2 and R 3 are hydrogen, hydroxysulfonyl, hydroxyl, halogen, alkyl of 1-4 carbon atoms or carboxyl; A is vinyl or -C 2 H 4 B, wherein B is a group which can be split off under alkaline conditions; and Z is Y or X.
  • the preparation of the above compounds is from the DE-A 37 40 650 and from Ullmann's Encyclopedia of Industrial Chemistry, 5th edition, Vol. A22, pp. 652-654 and from Ullmanns Encyclopedia of Technical Chemistry, 4th Edition, Vol. 20, p. 114-117 known. Some of the compounds are described in DE-OS 37 40 650 described as fiber-reactive, non-chromophoric amines.
  • An expedient embodiment of the invention The method is characterized in that fibers of the genus Lyocell with the textile auxiliary used according to the invention in be brought into contact with an alkaline environment.
  • crosslinking agents acting in an alkaline environment can be used during the Reactive staining can be used.
  • a preferred embodiment of the method according to the invention is that the compound as a textile auxiliary or their alkali salt is used.
  • a preparation of this compound is known from Example 9 of DE-A-37 40 650.
  • the process consists of leaving the fibers in an undyed state be used or that the treatment is carried out the fibers are dyed simultaneously, or that the Fibers are present as fiber structures.
  • the present invention further relates to the use of a compound of the general formula where X, Y and Z have the meaning given above, or their alkali metal salt, as textile auxiliaries for the treatment of fibers of the Lyocell genus or for the treatment of structures made of fibers of the Lyocell genus, a yarn or textile surface being best used as the fiber structure .
  • a woven, knitted or knitted fabric is particularly suitable as a textile surface.
  • the invention further relates to the use of the above Compound of general formula (I) for improving the Pilling behavior, to reduce the formation of pills and Improvement of the white abrasion behavior of the textile surface.
  • the present invention further relates to fibers of the type Lyocell, which can be obtained by the process according to the invention are, or yarns and fiber structures that contain these fibers.
  • the samples obtained in Examples 1 to 3 were after the Coloring washed 10 times at 60 ° C and tumble dried (according to DIN 53920 or ISO 6330, DIN 26330 without prewash).
  • the Assessment of pills and whitening was done after the fifth and after the tenth wash.
  • the Pilling during washing shows the behavior in the wet Status.
  • Table 1 shows that both the pills and also the white abrasion in those treated with substance I. Samples after 5 and 10 washes are greatly reduced.
  • This example is analogous to example 1, but instead of Single jersey the following fabric is used: 100% Lyocell, 1.7 dtex, twill, weft and chain Nm 50, 150 cm long and 30 cm wide.
  • Example 2 This example is analogous to Example 2, but instead of Single jersey the following fabric is used: 100% Lyocell, 1.7 dtex, twill, weft and chain Nm 50, 150 cm long and 30 cm wide.
  • Example 3 is analogous to Example 3, but instead of Single jersey the following fabric is used: 100% Lyocell, 1.7 dtex, twill, weft and chain Nm 50, 150 cm long and 30 cm wide.
  • Example 6 shows clear brightening due to abrasive edges, whereas the fabrics of Examples 4 and 5 are streak-free.
  • the fabrics are with 1 ml / l plasticizer (Basosoft, Avivan GSA) at 60 ° C and paraffinated.
  • the yarn thus obtained becomes a single jersey and socks knitted.
  • the fabrics are with 1 ml / l plasticizer (Basosoft, Avivan GSA) at 60 ° C and paraffinated.
  • Socks are knitted from the yarn thus obtained.
  • Example 7 The single jersey from Example 7 and a single jersey the same, untreated yarn are put together in the laboratory jet (Mathis, nozzle 40 mm, 1 revolution / minute) according to the above Dyeing instructions dyed, the fabrics receiving 9a and 9b become.
  • the dyed single jersey 9a shows no streaks or Chafe marks. In contrast, the Single Jersey 9b Abrasive edges and graying clearly visible.
  • the pilling test is carried out in a dry state in accordance with SN 198525.
  • Pill 125 Pill 500 Pill 2000 Example 9a 4.5 4.0 4.0 Example 9b 3.5 2.5 1.0
  • a Lyocell fabric dyed with reactive dyes (twill, 1.7 dtex, Nm 50) is impregnated with a liquor on the pad (liquor absorption: 80%), which contains 10 g / l crosslinker and 3 ml wetting agent (Leonil SR).
  • the fabric is then dried at 60 ° C and impregnated again with a liquor (liquor absorption: 80%) which contains 10 g / l crosslinking agent (substance I or TAHT), 3 ml wetting agent (Leonil SR), 10 g / l plasticizer ( Sandolub NV), 10 g / l Na 2 CO 3 and 1 ml / l NaOH contains.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Coloring (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)

Abstract

A process for the treatment of cellulose fibers of the Lyocell type, wherein said fibers are contacted with a textile auxiliary agent, characterized in that as said textile auxiliary agent a compound of the general formula or its alkaline metal salt is employed, wherein X is halogen, alkoxy having 1-4 carbon atoms, amino, alkylamino having 1-4 carbon atoms, hydroxysulphonyl or 1-nicotinyl; Y having the general formula wherein n is the number 1 or 2; R1 is hydrogen, alkyl having 1-4 carbon atoms or phenyl; R2 and R3 are hydrogen, hydroxysulphonyl, hydroxyl, halogen, alkyl having 1-4 carbon atoms or carboxyl; A is vinyl or -C2H4B, wherein B is a group capable of being cleaved under alkaline conditions; and Z is Y or X.

Description

Die Erfindung betrifft ein Verfahren zur Behandlung von Cellulosefasern und von Gebilden aus diesen Cellulosefasern, bei welchem Verfahren die Fasern bzw. die Fasergebilde mit einem Textilhilfsmittel in Kontakt gebracht werden, um den Fasern verbesserte Eigenschaften zu verleihen. Die Erfindung betrifft ferner neue Fasergebilde, wie z.B. Garne und textile Flächen, die nach diesem Verfahren erhältlich sind.The invention relates to a method for the treatment of Cellulose fibers and of structures made from these cellulose fibers which process the fibers or the fiber structures with a Textile auxiliaries are brought into contact with the fibers to give improved properties. The invention relates also new fiber structures, e.g. Yarns and textile surfaces, which can be obtained using this procedure.

Als Alternative zum Viskoseverfahren wurden in den letzten Jahren eine Reihe von Verfahren beschrieben, bei denen Cellulose ohne Bildung eines Derivats in einem organischen Lösungsmittel, einer Kombination eines organischen Lösungsmittels mit einem anorganischen Salz oder in wässerigen Salzlösungen gelöst wird. Cellulosefasern, die aus solchen Lösungen hergestellt werden, erhielten von der BISFA (The International Bureau for the Standardisation of man made Fibres) den Gattungsnamen Lyocell. Als Lyocell wird von der BISFA eine Cellulosefaser definiert, die durch ein Spinnverfahren aus einem organischen Lösungsmittel erhalten wird. Unter "organisches Lösungsmittel" wird von der BISFA ein Gemisch aus einer organischen Chemikalie und Wasser verstanden. "Lösungsmittelspinnen" soll Auflösen und Spinnen ohne Derivatisierung bedeuten.As an alternative to the viscose process, the last Years have described a number of processes in which cellulose without the formation of a derivative in an organic solvent, a combination of an organic solvent with a inorganic salt or dissolved in aqueous salt solutions. Cellulose fibers made from such solutions received from BISFA (The International Bureau for the Standardization of man made fibers) the generic name Lyocell. BISFA defines a cellulose fiber as Lyocell, by an organic solvent spinning process is obtained. Under "organic solvent" is the BISFA a mixture of an organic chemical and water Understood. "Solvent spinning" is meant to dissolve and spin mean without derivatization.

Bis heute hat sich jedoch nur ein einziges Verfahren zur Herstellung einer Cellulosefaser der Gattung Lyocell bis zur industriellen Realisierung durchgesetzt. Bei diesem Verfahren wird als Lösungsmittel ein tertiäres Aminoxid, insbesondere N-Methylmorpholin-N-oxid (NMMO), verwendet. Ein solches Verfahren ist z.B. in der US-A - 4,246,221 beschrieben und liefert Fasern, die sich durch eine hohe Festigkeit, einen hohen Naßmodul und durch eine hohe Schlingenfestigkeit auszeichnen.To date, however, only one method has been used Production of a cellulose fiber of the Lyocell genus up to industrial implementation. With this procedure is a tertiary amine oxide, in particular as a solvent N-methylmorpholine-N-oxide (NMMO). Such one The procedure is e.g. in US-A-4,246,221 and provides fibers that are characterized by high strength, high Wet module and characterized by a high loop strength.

Die Brauchbarkeit von Flächengebilden, z.B. Geweben, hergestellt aus den genannten Fasern, wird jedoch durch die ausgeprägte Neigung dieser Fasern, im nassen Zustand zu fibrillieren, stark eingeschränkt. Unter Fibrillierung wird das Aufbrechen der nassen Faser in Längsrichtung bei mechanischer Beanspruchung im nassen Zustand verstanden, wodurch die Faser ein haariges, pelziges Aussehen erhält. Ein aus diesen Fasern hergestelltes und gefärbtes Gewebe verliert im Laufe einiger Wäschen stark an Farbintensität. Dazu kommt noch, daß sich an Scheuer- und Knitterkanten helle Streifen ausbilden. Als Ursache für die Fibrillierung wird angenommen, daß die Faser aus in Faserrichtung angeordneten Fibrillen besteht, zwischen denen nur in geringem Ausmaß eine Quervernetzung vorhanden ist.The utility of fabrics, e.g. Fabrics made from the fibers mentioned, but is pronounced by the These fibers tend to fibrillate when wet limited. Fibrillation is the breaking up of the wet fiber in the longitudinal direction with mechanical stress in understood wet condition, which gives the fiber a hairy, furry appearance. One made from these fibers and dyed fabric loses heavily over the course of a few washes Color intensity. In addition, there are abrasive and Form crease edges with light stripes. As the cause of that Fibrillation is believed to consist of fiber in Fibrils arranged in the direction of the fiber exist between which only there is little cross-linking.

Ferner kann es auch bei der Färbung der Fasern in Strangform zur Streifenbildung kommen. In textilen Flächen kann es durch Reibung im Trockenen zur Bildung von Knötchen kommen, welche Eigenschaft als "Pilling" bekannt ist.It can also be used for dyeing the fibers in strand form Banding come. In textile surfaces, it can Dry friction leads to the formation of nodules, which Property known as "pilling".

Die WO 92/07124 beschreibt ein Verfahren zur Herstellung einer Faser mit verringerter Fibrillierneigung, gemäß dem die frisch gesponnene, also noch nicht getrocknete Faser mit einem kationischen Polymer behandelt wird. Als derartiges Polymer wird ein Polymer mit Imidazol- und Azetidin-Gruppen genannt. Zusätzlich kann noch eine Behandlung mit einem emulgierbaren Polymer, wie z.B. Polyethylen oder Polyvinylacetat, oder auch eine Vernetzung mit Glyoxal erfolgen.WO 92/07124 describes a method for producing a Fiber with reduced tendency to fibrillation, according to which the fresh spun, i.e. not yet dried, fiber with one cationic polymer is treated. As such a polymer called a polymer with imidazole and azetidine groups. In addition, treatment with an emulsifiable Polymer, e.g. Polyethylene or polyvinyl acetate, or also crosslinking with glyoxal.

In einem bei der CELLUCON-Konferenz 1993 in Lund, Schweden, von S. Mortimer gehaltenen Vortrag wurde erwähnt, daß die Fibrillierneigung mit zunehmender Verstreckung ansteigt.In one at the CELLUCON conference 1993 in Lund, Sweden, by S. Mortimer lecture was mentioned that the The tendency to fibrillation increases with increasing stretching.

EP-A - 0 538 977 und die WO 94/09191 beschreiben ein Verfahren der eingangs erwähnten Art, bei welchem Fasern der Gattung Lyocell zur Verringerung der Fibrillierneigung mit einem Textilhilfsmittel in Kontakt gebracht werden.EP-A - 0 538 977 and WO 94/09191 describe a method of the type mentioned, in which fibers of the genus Lyocell to reduce the tendency to fibrillation with a Textile auxiliaries are brought into contact.

Die WO 94/24343 beschreibt ein Verfahren zur Herstellung von Cellulosefasern mit verringerter Fibrillierneigung, bei welchem Verfahren eine Lösung von Cellulose in einem tertiären Aminoxid zu Fasern versponnen und die frisch gesponnenen Fasern mit einem Textilhilfsmittel, das mindestens zwei reaktive Gruppen trägt, in Kontakt gebracht und mit einem wässerigen Puffer gewaschen werden, wobei als Textilhilfsmittel nicht Glyoxal eingesetzt wird. Gemäß diesem vorbekannten Verfahren werden die frisch gesponnenen Fasern mit dem Textilhilfsmittel am besten in einem alkalischem Milieu in Kontakt gebracht.WO 94/24343 describes a process for the production of Cellulose fibers with reduced tendency to fibrillation, in which Process a solution of cellulose in a tertiary amine oxide spun into fibers and the freshly spun fibers with one Textile auxiliaries carrying at least two reactive groups, contacted and washed with an aqueous buffer be used as a textile auxiliary not glyoxal becomes. According to this previously known method, the fresh spun fibers with the textile auxiliary is best in one alkaline environment.

Es ist ferner bekannt, daß Fasergebilde aus Fasern der Gattung Lyocell mit Methylolverbindungen vernetzt werden können, um waschstabile Gewebe und Gestricke herzustellen. Es hat sich jedoch gezeigt, daß es nicht möglich ist, bei Verwendung dieser Verbindungen die Bildung von Scheuerkanten bei der Färbung zu verhindern. Dazu müßte die Vernetzung vor der Färbung oder zumindest während der Färbung erfolgen. Methylolverbindungen und auch die anderen klassischen Hochveredelungsmittel sind dazu jedoch kaum geeignet. Ein weiterer Nachteil der Methylolverbindungen ist die Bildung von Formaldehyd, die zu einer Belastung am Arbeitsplatz führt.It is also known that fiber structures from fibers of the genus Lyocell can be cross-linked with methylol compounds manufacture washable fabrics and knitted fabrics. It has however demonstrated that it is not possible using this Connections to the formation of abrasive edges during staining prevent. To do this, the networking would have to be done before coloring or at least during the coloring. Methylol compounds and the other classic finishing agents are also included however hardly suitable. Another disadvantage of Methylol compounds is the formation of formaldehyde, too leads to stress at the workplace.

Die Erfindung stellt sich die Aufgabe, ein Verfahren zur Behandlung von Cellulosefasern der Gattung Lyocell und von Gebilden aus diesen Fasern zu Verfügung zu stellen, das auf einfache Weise durchgeführt werden kann und das ermöglicht, daß die behandelten Fasern eine verringerte Fibrillierneigung bzw. behandelte Fasergebilde oder behandelte Fasern enthaltende Fasergebilde verbesserte Scheuer- und Pillingwerte aufweisen.The invention has for its object a method for Treatment of cellulose fibers of the Lyocell genus and Formed from these fibers to provide that on can be carried out in a simple manner and that enables the treated fibers have a reduced tendency to fibrillation or treated fiber structures or treated fibers Fiber structures have improved abrasion and pilling values.

Das erfindungsgemäße Verfahren zur Behandlung von Cellulosefasern, bei welchem die Fasern mit einem Textilhilfsmittel in Kontakt gebracht werden, ist dadurch gekennzeichnet, daß als Textilhilfsmittel eine Verbindung mit der allgemeinen Formel

Figure 00040001
bzw. ihr Alkalisalz eingesetzt wird, wobei X Halogen, Alkoxy mit 1-4 Kohlenstoffatomen, Amino, Alkylamino mit 1-4 Kohlenstoffatomen, Hydroxysulfonyl, oder 1-Nicotinyl ist; Y die allgemeine Formel
Figure 00040002
besitzt, worin n die Zahl 1 oder 2 ist; R1 Wasserstoff, Alkyl mit 1-4 Kohlenstoffatomen oder Phenyl ist; R2 und R3 Wasserstoff, Hydroxysulfonyl, Hydroxyl, Halogen, Alkyl mit 1-4 Kohlenstoffatomen oder Carboxyl sind; A Vinyl oder -C2H4B ist, worin B eine unter alkalischen Bedingungen abspaltbare Gruppe ist; und
Z gleich Y oder X ist.The process according to the invention for the treatment of cellulose fibers, in which the fibers are brought into contact with a textile auxiliary, is characterized in that a compound having the general formula is used as the textile auxiliary
Figure 00040001
or their alkali salt is used, where X is halogen, alkoxy with 1-4 carbon atoms, amino, alkylamino with 1-4 carbon atoms, hydroxysulfonyl, or 1-nicotinyl; Y the general formula
Figure 00040002
in which n is the number 1 or 2; R 1 is hydrogen, alkyl of 1-4 carbon atoms or phenyl; R 2 and R 3 are hydrogen, hydroxysulfonyl, hydroxyl, halogen, alkyl of 1-4 carbon atoms or carboxyl; A is vinyl or -C 2 H 4 B, wherein B is a group which can be split off under alkaline conditions; and
Z is Y or X.

Die Herstellung der oben genannten Verbindungen ist aus der DE-A 37 40 650 und aus Ullmann's Encyclopedia of Industrial Chemistry, 5. Auflage, Vol. A22, S. 652-654 sowie aus Ullmanns Encyclopädie der technischen Chemie, 4. Auflage, Vol. 20, S. 114-117 bekannt. Einige der Verbindungen werden in der DE-OS 37 40 650 als faserreaktive, nicht-chromophore Amine beschrieben.The preparation of the above compounds is from the DE-A 37 40 650 and from Ullmann's Encyclopedia of Industrial Chemistry, 5th edition, Vol. A22, pp. 652-654 and from Ullmanns Encyclopedia of Technical Chemistry, 4th Edition, Vol. 20, p. 114-117 known. Some of the compounds are described in DE-OS 37 40 650 described as fiber-reactive, non-chromophoric amines.

Eine zweckmäßige Ausführungsform des erfindungsgemäßen Verfahrens ist dadurch gekennzeichnet, daß Fasern der Gattung Lyocell mit dem erfindungsgemäß verwendeten Textilhilfsmittel in einem alkalischem Milieu in Kontakt gebracht werden. In alkalischem Milieu wirkende Vernetzer können während der Reaktivfärbung eingesetzt werden. An expedient embodiment of the invention The method is characterized in that fibers of the genus Lyocell with the textile auxiliary used according to the invention in be brought into contact with an alkaline environment. In crosslinking agents acting in an alkaline environment can be used during the Reactive staining can be used.

Eine bevorzugte Ausführungsform des erfindungsgemäßen Verfahrens besteht darin, daß als Textilhilfsmittel die Verbindung

Figure 00050001
bzw. ihr Alkalisalz eingesetzt wird. Eine Herstellung dieser Verbindung ist aus Beispiel 9 der DE-A- 37 40 650 bekannt.A preferred embodiment of the method according to the invention is that the compound as a textile auxiliary
Figure 00050001
or their alkali salt is used. A preparation of this compound is known from Example 9 of DE-A-37 40 650.

Weitere bevorzugte Ausführungsformen des erfindungsgemäßen Verfahrens bestehen darin, daß die Fasern in ungefärbtem Zustand eingesetzt werden, oder daß die Behandlung durchgeführt wird, wobei die Fasern gleichzeitig gefärbt werden, oder daß die Fasern als Fasergebilde vorliegen.Further preferred embodiments of the invention The process consists of leaving the fibers in an undyed state be used or that the treatment is carried out the fibers are dyed simultaneously, or that the Fibers are present as fiber structures.

Die vorliegende Erfindung betrifft ferner die Verwendung einer Verbindung der allgemeinen Formel

Figure 00050002
wobei X, Y und Z die oben angegebene Bedeutung haben, bzw. ihres Alkalisalzes, als Textilhilfsmittel zur Behandlung von Fasern der Gattung Lyocell oder zur Behandlung von Gebilden aus Fasern der Gattung Lyocell, wobei als Fasergebilde am besten ein Garn oder eine textile Fläche eingesetzt wird. Als textile Fläche eignen sich insbesondere ein Gewebe, ein Gestricke oder ein Gewirke.The present invention further relates to the use of a compound of the general formula
Figure 00050002
where X, Y and Z have the meaning given above, or their alkali metal salt, as textile auxiliaries for the treatment of fibers of the Lyocell genus or for the treatment of structures made of fibers of the Lyocell genus, a yarn or textile surface being best used as the fiber structure . A woven, knitted or knitted fabric is particularly suitable as a textile surface.

Die Erfindung betrifft ferner die Verwendung der obigen Verbindung der allgemeinen Formel (I) zur Verbesserung des Pillingverhaltens, zur Verringerung der Pillsbildung und zur Verbesserung des Weißscheuerverhaltens der textilen Fläche.The invention further relates to the use of the above Compound of general formula (I) for improving the Pilling behavior, to reduce the formation of pills and Improvement of the white abrasion behavior of the textile surface.

Die vorliegende Erfindung betrifft weiters Fasern der Gattung Lyocell, die nach dem erfindungsgemäßen Verfahren erhältlich sind, bzw. Garne und Fasergebilde, die diese Fasern enthalten.The present invention further relates to fibers of the type Lyocell, which can be obtained by the process according to the invention are, or yarns and fiber structures that contain these fibers.

Die erfindungsgemäße Behandlung mit den oben genannten Verbindungen kann vor, während oder nach der Färbung und an der Faser, dem Garn und am Fasergebilde vorgenommen werden. Eine bevorzugte Ausführungsform der Erfindung, bei welcher die obige Verbindung der Formel (III) eingesetzt wird, wird mit den folgenden Beispielen noch näher erläutert. Alle %-Angaben sind als Masse% zu verstehen.

  • 1) Herstellung der Cellulosefasern Gemäß dem in der EP-A - 0 356 419 und der WO 93/19230 beschriebenen Verfahren wurden Cellulosefasern der Gattung Lyocell hergestellt. Diese Fasern wurden in bekannter Weise zu einem Textil weiterverarbeitet. Die Behandlung der Fasern wird mit der Verbindung der Formel (III) vorgenommen. Diese Verbindung wird im folgenden als "Substanz I" bezeichnet.
  • 2) Allgemeine Färbevorschrift Das Textil wird bei einem Flottenverhältnis von 1:20 mit 6% Reaktivfarbstoff (Remazol Brilliantblau BB oder Remazol Schwarz B) 10 Minuten bei 40°C imprägniert. Das Färbebad enthält 0,3 ml/l eines Lauffaltenverhinderers (z.B. Biavin 109). Anschließend werden innerhalb von 20 Minuten 50 g/l Na2SO4 portionsweise zugegeben. Anschließend werden 5g/l Na2CO3 zugesetzt und wird auf 60°C erwärmt. Nach weiteren 15 Minuten werden 0,25 ml/l NaOH zugegeben und wird weitere 20 Minuten lang gefärbt. Anschließend wird warm gespült, mit Essigsäure auf pH 5,5 gebracht und kalt, kochend und schließlich wieder kalt gespült. Wenn im folgenden nicht anders angegeben, werden die Textilien mit 1 ml/l Weichmacher (Basosoft, Avivan GSA) bei 60°C aviviert.
    • The treatment according to the invention with the abovementioned compounds can be carried out before, during or after the dyeing and on the fiber, the yarn and on the fiber structure. A preferred embodiment of the invention, in which the above compound of formula (III) is used, is explained in more detail with the following examples. All% figures are to be understood as mass%.
  • 1) Production of the cellulose fibers According to the method described in EP-A - 0 356 419 and WO 93/19230, cellulose fibers of the Lyocell genus were produced. These fibers were processed into a textile in a known manner. The treatment of the fibers is carried out with the compound of formula (III). This compound is referred to below as "substance I".
  • 2) General dyeing instructions The textile is impregnated with a liquor ratio of 1:20 with 6% reactive dye (Remazol Brilliantblau BB or Remazol Schwarz B) for 10 minutes at 40 ° C. The dye bath contains 0.3 ml / l of an anti-wrinkle (e.g. Biavin 109). 50 g / l Na 2 SO 4 are then added in portions within 20 minutes. 5 g / l Na 2 CO 3 are then added and the mixture is heated to 60.degree. After a further 15 minutes, 0.25 ml / l NaOH are added and the dyeing is continued for a further 20 minutes. It is then rinsed warm, brought to pH 5.5 with acetic acid and rinsed cold, boiling and finally cold again. Unless otherwise stated below, the textiles are finished with 1 ml / l plasticizer (Basosoft, Avivan GSA) at 60 ° C.

    • Beispiel 1example 1

    4 Lfm Single Jersey (100% Lyocell, 1,7 dtex, Nm 50) werden mit 1 g/l eines Waschmittels (Kiralon Jet), 2 g/l Na2CO3 10 Minuten bei 30°C behandelt (Flottenverhältnis 1:15). Anschließend werden 3% (bezogen auf das Warengewicht) Substanz I zugegeben. Nach weiteren 10 Minuten erfolgt die Zugabe von 20 g/l Na2SO4 und eine Erhöhung der Temperatur auf 40°C. Nach weiteren 10 Minuten wird die Konzentration an Na2CO3 auf insgesamt 5 g/l erhöht und auf 80°C erwärmt. Nach 15 Minuten wird kalt und warm gespült und gemäß obiger Vorschrift gefärbt.4 running meters of single jersey (100% Lyocell, 1.7 dtex, Nm 50) are treated with 1 g / l of a detergent (Kiralon Jet), 2 g / l Na 2 CO 3 for 10 minutes at 30 ° C (liquor ratio 1:15 ). Then 3% (based on the weight of the goods) of substance I are added. After a further 10 minutes, 20 g / l Na 2 SO 4 are added and the temperature is increased to 40 ° C. After a further 10 minutes, the concentration of Na 2 CO 3 is increased to a total of 5 g / l and heated to 80 ° C. After 15 minutes, it is rinsed cold and warm and dyed according to the above instructions.

    Beispiel 2Example 2

    4 Lfm Single Jersey (100% Lyocell, 1,7 dtex, Nm 50) werden mit 1 g/l eines Waschmittels (Kiralon Jet), 2 g/l Na2CO3 10 Minuten bei 30°C behandelt (Flottenverhältnis 1:15). Anschließend werden 3% (bezogen auf das Warengewicht) Substanz I zugegeben. Nach weiteren 10 Minuten erfolgt eine Erhöhung der Temperatur auf 40°C. Nach weiteren 10 Minuten wird die Konzentration an Na2CO3 auf insgesamt 5 g/l erhöht und auf 80°C erwärmt. Nach 15 Minuten wird kalt und warm gespült und gemäß obiger Vorschrift gefärbt.4 running meters of single jersey (100% Lyocell, 1.7 dtex, Nm 50) are treated with 1 g / l of a detergent (Kiralon Jet), 2 g / l Na 2 CO 3 for 10 minutes at 30 ° C (liquor ratio 1:15 ). Then 3% (based on the weight of the goods) of substance I are added. After a further 10 minutes, the temperature is increased to 40 ° C. After a further 10 minutes, the concentration of Na 2 CO 3 is increased to a total of 5 g / l and heated to 80 ° C. After 15 minutes, it is rinsed cold and warm and dyed according to the above instructions.

    Beispiel 3 (Vergleich)Example 3 (comparison)

    4 Lfm Single Jersey (100% Lyocell, 1,7 dtex, Nm 50) werden mit 1 g/l eines Waschmittels (Kiralon Jet), 2 g/l Na2CO3 10 Minuten bei 30°C behandelt (Flottenverhältnis 1:15). Nach weiteren 10 Minuten erfolgt eine Erhöhung der Temperatur auf 80°C. Nach 30 Minuten wird kalt und warm gespült und gemäß obiger Vorschrift gefärbt. 4 running meters of single jersey (100% Lyocell, 1.7 dtex, Nm 50) are treated with 1 g / l of a detergent (Kiralon Jet), 2 g / l Na 2 CO 3 for 10 minutes at 30 ° C (liquor ratio 1:15 ). After a further 10 minutes, the temperature is increased to 80 ° C. After 30 minutes, it is rinsed cold and warm and dyed according to the above instructions.

    Ergebnis der Beispiele 1 bis 3Result of Examples 1 to 3 Waschtest:Washing test:

    Die in den Beispielen 1 bis 3 erhaltenen Proben wurden nach der Färbung 10 Mal bei 60°C gewaschen und im Tumbler getrocknet (gemäß DIN 53920 bzw. ISO 6330, DIN 26330 ohne Vorwäsche). Die Beurteilung hinsichtlich Pillsbildung und Weißscheuerung erfolgte nach der fünften und nach der zehnten Wäsche. Die Pillsbildung bei der Wäsche zeigt das Verhalten im nassen Zustand.The samples obtained in Examples 1 to 3 were after the Coloring washed 10 times at 60 ° C and tumble dried (according to DIN 53920 or ISO 6330, DIN 26330 without prewash). The Assessment of pills and whitening was done after the fifth and after the tenth wash. The Pilling during washing shows the behavior in the wet Status.

    Die Benotung erfolgt nach EMPA-Fotovorlagen und erstreckt sich von 1 (= stark vorhanden; d.h. schlecht) bis 5 (=nicht vorhanden; d.h. gut) und ist in der nachfolgenden Tabelle zusammengefaßt: Beisp. 1 Beisp. 2 Beisp. 3 Pillsbildung nach 5 Wäschen 4,5 4,5 4,5 Pillsbildung nach 10 Wäschen 3,5 3,0 1,5 Weißscheuerung nach 5 Wäschen 5,0 5,0 3,0 Weißscheuerung nach 10 Wäschen 5,0 4,0 2,0 The grading is based on EMPA photo templates and extends from 1 (= strong; i.e. bad) to 5 (= not available; ie good) and is summarized in the following table: Ex. 1 Ex. 2 Ex. 3 Pills after 5 washes 4.5 4.5 4.5 Pills after 10 washes 3.5 3.0 1.5 White scrubbing after 5 washes 5.0 5.0 3.0 White scrubbing after 10 washes 5.0 4.0 2.0

    Der Tabelle 1 ist zu entnehmen, daß sowohl die Pillsbildung als auch die Weißscheuerung bei den mit der Substanz I behandelten Proben nach 5 und 10 Wäschen stark vermindert ist.Table 1 shows that both the pills and also the white abrasion in those treated with substance I. Samples after 5 and 10 washes are greatly reduced.

    Beispiel 4Example 4

    Dieses Beispiel ist analog Beispiel 1, wobei jedoch statt des Single Jersey folgendes Gewebe verwendet wird: 100% Lyocell, 1,7 dtex, Köper, Schuß und Kette Nm 50, 150 cm lang und 30 cm breit.This example is analogous to example 1, but instead of Single jersey the following fabric is used: 100% Lyocell, 1.7 dtex, twill, weft and chain Nm 50, 150 cm long and 30 cm wide.

    Beispiel 5Example 5

    Dieses Beispiel ist analog Beispiel 2, wobei jedoch statt des Single Jersey folgendes Gewebe verwendet wird: 100% Lyocell, 1,7 dtex, Köper, Schuß und Kette Nm 50, 150 cm lang und 30 cm breit.This example is analogous to Example 2, but instead of Single jersey the following fabric is used: 100% Lyocell, 1.7 dtex, twill, weft and chain Nm 50, 150 cm long and 30 cm wide.

    Beispiel 6 (Vergleich)Example 6 (comparison)

    Dieses Beispiel ist analog Beispiel 3, wobei jedoch statt des Single Jersey folgendes Gewebe verwendet wird: 100% Lyocell, 1,7 dtex, Köper, Schuß und Kette Nm 50, 150 cm lang und 30 cm breit.This example is analogous to Example 3, but instead of Single jersey the following fabric is used: 100% Lyocell, 1.7 dtex, twill, weft and chain Nm 50, 150 cm long and 30 cm wide.

    Die in den Beispielen 4, 5 und 6 erhaltenen Gewebe werden zusammengenäht und am Laborjet (Mathis, Düse 40 mm, 1 Umlauf/Minute) nach obiger Färbevorschrift gefärbt.The fabrics obtained in Examples 4, 5 and 6 are sewn together and on the laboratory jet (Mathis, nozzle 40 mm, 1 Circulation / minute) dyed according to the above dyeing instructions.

    Das Gewebe von Beispiel 6 zeigt deutliche Aufhellungen aufgrund von Scheuerkanten, wogegen die Gewebe der Beispiele 4 und 5 streifenfrei sind.The fabric of Example 6 shows clear brightening due to abrasive edges, whereas the fabrics of Examples 4 and 5 are streak-free.

    Auch hinsichtlich Pillsbildung und Weißscheuerung zeigen die Gewebe der Beispiele 4 und 5 deutlich bessere Werte als das Gewebestück von Beispiel 6.They also show in terms of pills and whitening Fabrics of Examples 4 and 5 significantly better values than that Tissue piece from example 6.

    Beispiel 7Example 7

    4 kg Garn (100% Lyocell, 1,7 dtex, Nm 50) werden mit 2 g/l Waschmittel (Kiralon OLB), 2 g/l Na2CO3 30 Minuten bei 95°C in einem Garnfärbeapparat behandelt (wechselweises Pumpen: 4 Minuten von innen nach außen; 6 Minuten von außen nach innen). Anschließend wird heiß und kalt gespült. Während des letzten Spülbades wird mit Essigsäure auf pH 6,0 gebracht.4 kg of yarn (100% Lyocell, 1.7 dtex, Nm 50) are treated with 2 g / l detergent (Kiralon OLB), 2 g / l Na 2 CO 3 for 30 minutes at 95 ° C in a yarn dyeing machine (alternate pumping: 4 minutes from the inside out; 6 minutes from the outside in). Then it is rinsed hot and cold. During the last rinsing bath, the pH is brought to 6.0 with acetic acid.

    Anschließend wird mit 10% Substanz I (bezogen auf das Gewebegewicht) 15 Minuten lang bei 30°C imprägniert. Dann werden 6% Reaktivfarbstoff (Remazol Schwarz B) zugegeben. Es wird auf 50°C erwärmt, und innerhalb von 55 Minuten werden 50 g/l Na2SO4 portionsweise zugegeben. Dann werden 2,5 g/l Na2CO3 zugesetzt und wird auf 60°C erwärmt. Nach weiteren 15 Minuten werden weitere 7,5 g/l Na2CO3 zugegeben. Nach 15 Minuten erfolgt die Zugabe von 0,25 ml/l NaOH, und es wird weitere 30 Minuten gefärbt. Anschließend wird warm gespült, mit Essigsäure auf pH 5,5 gebracht und gespült (kalt, kochend und schließlich wieder kalt).It is then impregnated with 10% of substance I (based on the weight of the fabric) at 30 ° C. for 15 minutes. Then 6% reactive dye (Remazol Black B) is added. The mixture is heated to 50 ° C. and 50 g / l Na 2 SO 4 are added in portions over the course of 55 minutes. Then 2.5 g / l Na 2 CO 3 are added and the mixture is heated to 60.degree. After a further 15 minutes, a further 7.5 g / l Na 2 CO 3 are added. After 15 minutes, 0.25 ml / l NaOH is added and the dyeing is continued for a further 30 minutes. It is then rinsed warm, brought to pH 5.5 with acetic acid and rinsed (cold, boiling and finally cold again).

    Wenn im folgenden nicht anders angegeben, werden die Gewebe mit 1 ml/l Weichmacher (Basosoft, Avivan GSA) bei 60°C aviviert und paraffiniert.Unless otherwise stated below, the fabrics are with 1 ml / l plasticizer (Basosoft, Avivan GSA) at 60 ° C and paraffinated.

    Aus dem so erhaltenen Garn werden ein Single Jersey und Socken gestrickt.The yarn thus obtained becomes a single jersey and socks knitted.

    Beispiel 8 (Vergleich)Example 8 (comparison)

    4 kg Garn (100% Lyocell, 1,7 dtex, Nm 50) werden mit 2 g/l Waschmittel (Kiralon OLB), 2 g/l Na2CO3 30 Minuten bei 95°C in einem Garnfärbeapparat behandelt (wechselweises Pumpen: 4 Minuten von innen nach außen; 6 Minuten von außen nach innen). Anschließend wird heiß und kalt gespült. Während des letzten Spülbades wird mit Essigsäure auf pH 6,0 gebracht.4 kg of yarn (100% Lyocell, 1.7 dtex, Nm 50) are treated with 2 g / l detergent (Kiralon OLB), 2 g / l Na 2 CO 3 for 30 minutes at 95 ° C in a yarn dyeing machine (alternate pumping: 4 minutes from the inside out; 6 minutes from the outside in). Then it is rinsed hot and cold. During the last rinsing bath, the pH is brought to 6.0 with acetic acid.

    Anschließend wird mit 6% Reaktivfarbstoff (Remazol Schwarz B) 15 Minuten lang bei 30°C imprägniert. Es wird auf 50°C erwärmt, und innerhalb von 55 Minuten werden 50 g/l Na2SO4 portionsweise zugegeben. Dann werden 2,5 g/l Na2CO3 zugesetzt und wird auf 60°C erwärmt. Nach weiteren 15 Minuten werden weitere 7,5 g/l Na2CO3 zugegeben. Nach 15 Minuten erfolgt die zugabe von 0,25 ml/l NaOH, und es wird weitere 30 Minuten gefärbt. Anschließend wird warm gespült, mit Essigsäure auf pH 5,5 gebracht und gespült (kalt, kochend und schließlich wieder kalt).It is then impregnated with 6% reactive dye (Remazol Black B) for 15 minutes at 30 ° C. The mixture is heated to 50 ° C. and 50 g / l Na 2 SO 4 are added in portions over the course of 55 minutes. Then 2.5 g / l Na 2 CO 3 are added and the mixture is heated to 60.degree. After a further 15 minutes, a further 7.5 g / l Na 2 CO 3 are added. After 15 minutes, 0.25 ml / l NaOH is added and the dyeing is continued for a further 30 minutes. It is then rinsed warm, brought to pH 5.5 with acetic acid and rinsed (cold, boiling and finally cold again).

    Wenn im folgenden nicht anders angegeben, werden die Gewebe mit 1 ml/l Weichmacher (Basosoft, Avivan GSA) bei 60°C aviviert und paraffiniert. Unless otherwise stated below, the fabrics are with 1 ml / l plasticizer (Basosoft, Avivan GSA) at 60 ° C and paraffinated.

    Aus dem so erhaltenen Garn werden Socken gestrickt.Socks are knitted from the yarn thus obtained.

    Beispiel 9Example 9

    Der Single Jersey von Beispiel 7 und ein Single Jersey aus demselben, unbehandelten Garn werden gemeinsam im Laborjet (Mathis, Düse 40 mm, 1 Umlauf/Minute) nach obiger Färbevorschrift gefärbt, wobei die Gewebe 9a bzw. 9b erhalten werden.The single jersey from Example 7 and a single jersey the same, untreated yarn are put together in the laboratory jet (Mathis, nozzle 40 mm, 1 revolution / minute) according to the above Dyeing instructions dyed, the fabrics receiving 9a and 9b become.

    Der gefärbte Single Jersey 9a zeigt keine Streifen oder Scheuerstellen. Im Gegensatz dazu sind beim Single Jersey 9b Scheuerkanten und auch eine Vergrauung deutlich zu erkennen.The dyed single jersey 9a shows no streaks or Chafe marks. In contrast, the Single Jersey 9b Abrasive edges and graying clearly visible.

    Die Socken werden bei 40°C wiederholt gewaschen. Die Trocknung erfolgt jeweils im Tumbler. Schon nach 5 Waschzyklen sind die Socken aus dem Garn von Beispiel 8 stark vergraut. Die Socken aus dem Garn von Beispiel 7 hingegen weisen keinerlei Vergrauung bzw. Scheuerkanten auf. Beisp. 7 Beisp. 8 Pillsbildung nach 5 Wäschen 4,5 2,0 Weißscheuerung nach 5 Wäschen 5,0 1,0 The socks are washed repeatedly at 40 ° C. Drying takes place in the tumbler. After 5 washing cycles, the socks made from the yarn of Example 8 are grayed out. The socks made from the yarn of Example 7, on the other hand, have no graying or abrasive edges. Ex. 7 Ex. 8 Pills after 5 washes 4.5 2.0 White scrubbing after 5 washes 5.0 1.0

    Auch nach 20 Wäschen zeigen die Socken von Beispiel 7 eine Pillsbildung von 4,5 und eine Weißscheuerung von 5 auf.Even after 20 washes, the socks from Example 7 show one Pills formation of 4.5 and white chafing of 5.

    Prüfung auf PillingPilling test

    Die Pillingprüfung erfolgt gemäß SN 198525 im trockenen Zustand.The pilling test is carried out in a dry state in accordance with SN 198525.

    Die Beurteilung erfolgt gemäß der Norm visuell mit Hilfe von Vergleichsbildern. Die Note 5 bedeutet ein geringes Pilling, während die Note 1 ein extremes Pilling bedeutet. In der nachfolgenden Tabelle 3 bedeutet "Pill 125", "Pill 500" und "Pill 2000" das Pilling nach 125, 500 bzw. 2000 Zyklen. Pill 125 Pill 500 Pill 2000 Beispiel 9a 4,5 4,0 4,0 Beispiel 9b 3,5 2,5 1,0 The assessment is carried out visually according to the standard with the help of comparison images. The grade 5 means a low pilling, while the grade 1 means an extreme pilling. In Table 3 below, "Pill 125", "Pill 500" and "Pill 2000" means pilling after 125, 500 and 2000 cycles, respectively. Pill 125 Pill 500 Pill 2000 Example 9a 4.5 4.0 4.0 Example 9b 3.5 2.5 1.0

    Beispiel 10 (Vergleich mit Triacryloylhexahydrotriazin (TAHT))Example 10 (Comparison with Triacryloylhexahydrotriazine (TAHT))

    Ein mit Reaktivfarbstoffen gefärbtes Lyocell-Gewebe (Köper, 1,7 dtex, Nm 50) wird mit einer Flotte am Foulard imprägniert (Flottenaufnahme: 80%), welche 10 g/l Vernetzer und 3 ml Netzmittel (Leonil SR) enthält. Dann wird das Gewebe bei 60°C getrocknet und erneut mit einer Flotte imprägniert (Flottenaufnahme: 80%), welche 10 g/l Vernetzer (Substanz I bzw. TAHT), 3 ml Netzmittel (Leonil SR), 10 g/l Weichmacher (Sandolub NV), 10 g/l Na2CO3 und 1 ml/l NaOH enthält.A Lyocell fabric dyed with reactive dyes (twill, 1.7 dtex, Nm 50) is impregnated with a liquor on the pad (liquor absorption: 80%), which contains 10 g / l crosslinker and 3 ml wetting agent (Leonil SR). The fabric is then dried at 60 ° C and impregnated again with a liquor (liquor absorption: 80%) which contains 10 g / l crosslinking agent (substance I or TAHT), 3 ml wetting agent (Leonil SR), 10 g / l plasticizer ( Sandolub NV), 10 g / l Na 2 CO 3 and 1 ml / l NaOH contains.

    Anschließend läßt man das Gewebe 16 Stunden bei 70°C in einer Folie eingeschweißt ruhen. Dann wird gespült (kalt, warm und schließlich kochend), mit Essigsäure versetzt und bei 60°C getrocknet. Das Ergebnis hinsichtlich Weißscheuerung ist in der Tabelle IV angegeben. Vernetzer Weißscheuerung nach 3 Wäschen nach 5 Wäschen TAHT 1,0 1,0 Substanz I 3,0 2,0 The fabric is then left to rest sealed in a film at 70 ° C. for 16 hours. Then it is rinsed (cold, warm and finally boiling), mixed with acetic acid and dried at 60 ° C. The result regarding whitening is shown in Table IV. Crosslinker Whitening after 3 washes after 5 washes TAHT 1.0 1.0 Substance I 3.0 2.0

    Claims (14)

    1. A process for the treatment of cellulose fibres of the Lyocell type, wherein the fibres are contacted with a textile auxiliary agent, characterized in that as said textile auxiliary agent a compound of the general formula
      Figure 00170001
      or its alkaline metal salt is employed, wherein X is halogen, alkoxy having 1-4 carbon atoms, amino, alkylamino having 1-4 carbon atoms, hydroxysulphonyl or 1-nicotinyl; Y has the general formula
      Figure 00170002
      wherein n is an integer of 1 or 2; R1 is hydrogen, alkyl having 1-4 carbon atoms or phenyl; R2 and R3 are hydrogen, hydroxysulphonyl, hydroxyl, halogen, alkyl having 1-4 carbon atoms or carboxyl; A is vinyl or -C2H4B, wherein B is a group capable of being cleaved under alkaline conditions; and Z is Y or X.
    2. A process according to Claim 1, characterized in that as said textile auxiliary agent the compound
      Figure 00170003
      or its alkaline metal salt is employed.
    3. A process according to one of the Claims 1 or 2, characterized in that said fibers are employed in a non-dyed state.
    4. A process according to one of the Claims 1 or 2, characterized in that said treatment is carried out while said fibres are simultaneously being dyed.
    5. A process according to one of the Claims 1 to 4, characterized in that said fibres are present as fibre assemblies.
    6. The use of a compound of the general formula
      Figure 00180001
      wherein X, Y and Z have the meaning indicated in Claim 1, or its alkaline metal salt as a textile auxiliary agent for the treatment of fibres of the Lyocell type.
    7. The use of a compound of the general formula
      Figure 00180002
      wherein X, Y and Z have the meaning indicated in Claim 1, or its alkaline metal salt as a textile auxiliary agent for the treatment of assemblies of fibres of the Lyocell type.
    8. The use according to Claim 7, characterized in that as said fibre assembly a yarn or a plane textile assembly is employed.
    9. The use according to Claim 8, characterized in that as said plane textile assembly a woven or a knitted fabric is employed.
    10. The use according to Claim 9 to improve the pilling behaviour of said plane textile assembly.
    11. The use according to Claim 9 to reduce the pill formation of said plane textile assembly.
    12. The use according to Claim 9 to improve the white abrasion behaviour of said plane textile assembly.
    13. Fibres of the Lyocell type obtainable according to a process according to one of the Claims 1 to 5.
    14. Fibre assembly of fibres of the Lyocell type obtainable according to a process according to Claim 5.
    EP97926908A 1996-06-21 1997-06-19 Process for treating cellulose fibres and structures made of those fibres Expired - Lifetime EP0904444B1 (en)

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    WO1997049856A1 (en) 1997-12-31
    AU3159497A (en) 1998-01-14
    EP0904444A1 (en) 1999-03-31
    CN1228131A (en) 1999-09-08
    AU721876B2 (en) 2000-07-13
    ES2142167T3 (en) 2000-04-01
    ATE186961T1 (en) 1999-12-15
    GR3032485T3 (en) 2000-05-31
    BR9709916A (en) 1999-08-10
    AT409144B (en) 2002-05-27
    DE59700768D1 (en) 1999-12-30
    ID17073A (en) 1997-12-04
    ATA110796A (en) 2001-10-15
    CN1146684C (en) 2004-04-21
    US6022378A (en) 2000-02-08
    NO985955L (en) 1999-02-03
    TW336966B (en) 1998-07-21
    JP2000513412A (en) 2000-10-10
    NO985955D0 (en) 1998-12-18
    CA2258500A1 (en) 1997-12-31

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