EP0904444A1 - Process for treating cellulose fibres and structures made of those fibres - Google Patents

Process for treating cellulose fibres and structures made of those fibres

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Publication number
EP0904444A1
EP0904444A1 EP97926908A EP97926908A EP0904444A1 EP 0904444 A1 EP0904444 A1 EP 0904444A1 EP 97926908 A EP97926908 A EP 97926908A EP 97926908 A EP97926908 A EP 97926908A EP 0904444 A1 EP0904444 A1 EP 0904444A1
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EP
European Patent Office
Prior art keywords
fibers
textile
carbon atoms
lyocell
general formula
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP97926908A
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German (de)
French (fr)
Other versions
EP0904444B1 (en
Inventor
Markus Eibl
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Lenzing AG
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Lenzing AG
Chemiefaser Lenzing AG
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Publication of EP0904444A1 publication Critical patent/EP0904444A1/en
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Publication of EP0904444B1 publication Critical patent/EP0904444B1/en
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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 process for treatment of cellulosic fibers and structures made from these cellulose fibers, in which method the fibers or the fiber structure are contacted with a textile auxiliary agent in contact 'to impart to the fibers of improved properties.
  • the invention further relates to new fiber structures, such as yarns and textile surfaces, which are obtainable by this process.
  • a tertiary amine oxide in particular N-methylmorpholine-N-oxide (NMMO)
  • NMMO N-methylmorpholine-N-oxide
  • WO 92/07124 describes a method for producing a fiber with a reduced tendency to fibrillation, according to which the freshly spun, that is to say not yet dried, fiber is treated with a cationic polymer.
  • a polymer with imidazole and azetidine groups is mentioned as such a polymer.
  • treatment with an emulsifiable polymer e.g. Polyethylene or polyvinyl acetate, or crosslinking with glyoxal.
  • EP-A-0 538 977 and WO 94/09191 describe a process of the type mentioned at the outset in which fibers of the Lyocell genus are brought into contact with a textile auxiliary in order to reduce the tendency to fibrillation.
  • WO 94/24343 describes a process for the production of cellulose fibers with reduced tendency to fibrillation, in which Process spun a solution of cellulose in a tertiary amine oxide into fibers and the freshly spun fibers are brought into contact with a textile auxiliary which carries at least two reactive groups and are washed with an aqueous buffer, glyoxal not being used as the textile auxiliary. According to this previously known method, the freshly spun fibers are best brought into contact with the textile auxiliary in an alkaline environment.
  • fiber structures made from fibers of the Lyocell genus can be crosslinked with methylol compounds in order to produce washable fabrics and knitted fabrics.
  • methylol compounds it has been shown that it is not possible to prevent the formation of abrasive edges during the coloring when using these compounds. For this, the crosslinking would have to take place before the dyeing or at least during the dyeing.
  • methylol compounds and the other classic finishing agents are hardly suitable for this.
  • Another disadvantage of methylol compounds is the formation of formaldehyde, which leads to stress in the workplace.
  • the invention has for its object to provide a process for the treatment of cellulose fibers of the Lyocell genus and of structures made of these fibers, which can be carried out in a simple manner and which enables the treated fibers to have a reduced tendency to fibrillation or treated fiber structures or fiber structures containing treated fibers 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
  • X is halogen, alkoxy with 1-4 carbon atoms, amino, alkylamino with 1-4 carbon atoms, hydroxysulfonyl, or 1-nicotinyl; Y the general formula
  • n is the number 1 or 2;
  • R is hydrogen, alkyl of 1-4 carbon atoms or phenyl;
  • R 2 and R3 are hydrogen, hydroxysulfonyl, hydroxyl, halogen, alkyl of 1-4 carbon atoms or carboxyl;
  • A is vinyl or -C-H.B, wherein B is a group which can be split off under alkaline conditions; and
  • Z is Y or X.
  • An expedient embodiment of the method according to the invention is characterized in that fibers of the Lyocell genus are brought into contact with the textile auxiliary used according to the invention in an alkaline environment.
  • Crosslinkers acting in an alkaline environment can be used during reactive dyeing.
  • a preferred embodiment of the method according to the invention is that the compound as a textile auxiliary
  • Further preferred embodiments of the method according to the invention consist in that the fibers are used in the undyed state, or that the treatment is carried out, the fibers being dyed at the same time, or that the fibers are present as fiber structures.
  • the present invention further relates to the use of a compound of the general formula
  • 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 a 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) to improve the Pilling behavior, to reduce the formation of pills and to improve the chafing behavior of the textile surface.
  • the present invention further relates to fibers of the Lyocell genus which can be obtained by the process according to the invention, or to yarns and fiber structures which contain these fibers.
  • Cellulose fibers of the Lyocell genus were produced in accordance with the process described in EP-A-0 356 419 and WO 93/19230. 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”.
  • the textile is impregnated with a liquor ratio of 1:20 with 6% reactive dye (Remazol Brilliantblau BB or Remazol Schwarz B) in 40 minutes at 40 * c.
  • the dye bath contains 0.3 ml / 1 of an anti-wrinkle (e.g. Biavin 109).
  • 50 g / 1 Na-SO. added in portions.
  • 5 g / l Na_C0 are added and the mixture is heated to 60'C.
  • 0.25 ml / 1 NaOH are added and staining 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.
  • the Textiles with 1 ml / 1 softener Basosoft, Avivan GSA
  • Example 2 This example is analogous to Example 1, except that the following fabric is used instead of the single jersey: 100% Lyocell, 1.7 dtex, twill, weft and chain Nm 50, 150 cm long and 30 cm wide.
  • Example 5 This example is analogous to Example 2, but the following fabric is used instead of the single jersey: 100% Lyocell, 1.7 dtex, twill, weft and chain Nm 50, 150 cm long and 30 cm wide.
  • Example 3 This example is analogous to Example 3, except that the following fabric is used instead of the single jersey: 100% Lyocell, 1.7 dtex, twill, weft and chain Nm 50, 150 cm long and 30 cm wide.
  • the fabrics obtained in Examples 4, 5 and 6 are sewn together and dyed on the laboratory jet (Mathis, 40 mm nozzle, 1 revolution / minute) according to the above dyeing instructions.
  • Example 6 shows clear brightening due to abrasive edges, whereas the fabrics of Examples 4 and 5 are streak-free.
  • the fabrics of Examples 4 and 5 also show significantly better values than the fabric piece of Example 6 with regard to pill formation and whitening.
  • the tissues are treated with 1 ml / 1 plasticizer (Basosoft, Avivan GSA) at 60'C and waxed.
  • 1 ml / 1 plasticizer Basosoft, Avivan GSA
  • a single jersey and socks are knitted from the yarn thus obtained.
  • the tissues are treated with 1 ml / 1 plasticizer (Basosoft, Avivan GSA) at 60'C and waxed. Socks are knitted from the yarn thus obtained.
  • 1 ml / 1 plasticizer Basosoft, Avivan GSA
  • the single jersey from Example 7 and a single jersey made from the same, untreated yarn are dyed together in the laboratory jet (Mathis, nozzle 40 mm, 1 revolution / minute) according to the above dyeing instructions, the fabrics 9a and 9b being obtained.
  • the dyed single jersey 9a shows no streaks or chafing. In contrast, the single jersey 9b abrasive edges and graying are clearly visible.
  • 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.
  • the pilling test is carried out in a dry state in accordance with SN 198525.
  • 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.
  • “Pill 125”, “Pill 500” and “Pill 2000” means pilling after 125, 500 and 2000 cycles, respectively.
  • 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 / 1 crosslinker and 3 ml wetting agent (Leonil SR). Then the fabric is dried at 60 ° C and impregnated again with a liquor (liquor absorption: 80%) which contains 10 g / 1 crosslinking agent (substance I or TAHT), 3 ml wetting agent (Leonil SR), 10 g / 1 plasticizer ( Sandolub NV), 10 g / 1 Na 2 CO 3 and 1 ml / 1 NaOH contains.
  • 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.

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

Verfahren zur Behandlung von Cellulosefasern und von Gebilden aus diesen FasernProcess for treating cellulose fibers and structures made from these fibers
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 process for treatment of cellulosic fibers and structures made from these cellulose fibers, in which method the fibers or the fiber structure are contacted with a textile auxiliary agent in contact 'to impart to the fibers of improved properties. The invention further relates to new fiber structures, such as yarns and textile surfaces, which are obtainable by this process.
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, a number of processes have been described in recent years in which cellulose is dissolved in an organic solvent, a combination of an organic solvent with an inorganic salt or in aqueous salt solutions without the formation of a derivative. Cellulose fibers made from such solutions were given the generic name Lyocell by BISFA (The International Bureau for the Standardization of man made Fibers). BISFA defines a cellulose fiber as Lyocell, which is obtained from an organic solvent by a spinning process. BISFA understands "organic solvent" as a mixture of an organic chemical and water. "Solvent spinning" is intended to mean dissolving and spinning 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 Schiingenfestigkeit auszeichnen.To date, however, only a single process for the production of a cellulose fiber of the Lyocell type has prevailed until industrial implementation. In this process, a tertiary amine oxide, in particular N-methylmorpholine-N-oxide (NMMO), is used as the solvent. Such a method is e.g. in US-A-4,246,221 and provides fibers which are characterized by high strength, a high wet modulus and 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 usability of fabrics, such as fabrics, made from the fibers mentioned, is, however, by the pronounced The tendency of these fibers to fibrillate when wet is severely restricted. Fibrillation is understood to mean breaking open the wet fiber in the longitudinal direction under mechanical stress in the wet state, as a result of which the fiber is given a hairy, furry appearance. A fabric made and dyed from these fibers loses its color intensity over the course of a few washes. In addition, there are bright stripes on the scuffed and crease edges. The reason for the fibrillation is assumed to be that the fiber consists of fibrils arranged in the direction of the fibers, between which there is only a small amount of crosslinking.
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.Furthermore, streaking can also occur during the dyeing of the fibers in strand form. In textile surfaces, dry friction can lead to the formation of nodules, which property is 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. Polyerhylen oder Polyvinylacetat, oder auch eine Vernetzung mit Glyoxal erfolgen.WO 92/07124 describes a method for producing a fiber with a reduced tendency to fibrillation, according to which the freshly spun, that is to say not yet dried, fiber is treated with a cationic polymer. A polymer with imidazole and azetidine groups is mentioned as such a polymer. In addition, treatment with an emulsifiable polymer, e.g. Polyethylene or polyvinyl acetate, or 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 a lecture given by S. Mortimer at the 1993 CELLUCON conference in Lund, Sweden, it was mentioned that the tendency to fibrillation increased 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 process of the type mentioned at the outset in which fibers of the Lyocell genus are brought into contact with a textile auxiliary in order to reduce the tendency to fibrillation.
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 spun a solution of cellulose in a tertiary amine oxide into fibers and the freshly spun fibers are brought into contact with a textile auxiliary which carries at least two reactive groups and are washed with an aqueous buffer, glyoxal not being used as the textile auxiliary. According to this previously known method, the freshly spun fibers are best brought into contact with the textile auxiliary in an 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 made from fibers of the Lyocell genus can be crosslinked with methylol compounds in order to produce washable fabrics and knitted fabrics. However, it has been shown that it is not possible to prevent the formation of abrasive edges during the coloring when using these compounds. For this, the crosslinking would have to take place before the dyeing or at least during the dyeing. However, methylol compounds and the other classic finishing agents are hardly suitable for this. Another disadvantage of methylol compounds is the formation of formaldehyde, which leads to stress in 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 to provide a process for the treatment of cellulose fibers of the Lyocell genus and of structures made of these fibers, which can be carried out in a simple manner and which enables the treated fibers to have a reduced tendency to fibrillation or treated fiber structures or fiber structures containing treated fibers 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 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
bzw. ihr Alkalisalz eingesetzt wird, wobei X Halogen, Alkoxy mit 1-4 Kohlenstoffatomen, Amino, Alkylamino mit 1-4 Kohlenεtoffatomen, Hydroxysulfonyl, oder 1-Nicotinyl ist; Y die allgemeine Formelor 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
besitzt, worin n die Zahl 1 oder 2 ist; R Wasserstoff, Alkyl mit 1-4 Kohlenstoffatomen oder Phenyl ist; R 2 und R3 Wasserstoff, Hydroxysulfonyl, Hydroxyl, Halogen, Alkyl mit 1-4 Kohlenstoffatomen oder Carboxyl sind; A Vinyl oder -C-H.B ist, worin B eine unter alkalischen Bedingungen abspaltbare Gruppe ist; und Z gleich Y oder X ist.in which n is the number 1 or 2; R is hydrogen, alkyl of 1-4 carbon atoms or phenyl; R 2 and R3 are hydrogen, hydroxysulfonyl, hydroxyl, halogen, alkyl of 1-4 carbon atoms or carboxyl; A is vinyl or -C-H.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-OS 37 40 650 und aus Ulimann'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-mentioned compounds is known from DE-OS 37 40 650 and from Ulimann's Encyclopedia of Industrial Chemistry, 5th edition, Vol. A22, pp. 652-654 and from Ullmanns Encyclopedia of Industrial Chemistry, 4th edition, Vol. 20, pp. 114-117. Some of the compounds are described in DE-OS 37 40 650 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. Eine bevorzugte Ausführungsform des erfindungsgemäßen Verfahrens besteht darin, daß als Textilhilfsmittel die VerbindungAn expedient embodiment of the method according to the invention is characterized in that fibers of the Lyocell genus are brought into contact with the textile auxiliary used according to the invention in an alkaline environment. Crosslinkers acting in an alkaline environment can be used during reactive dyeing. A preferred embodiment of the method according to the invention is that the compound as a textile auxiliary
bzw. ihr Alkalisalz eingesetzt wird. Eine Herstellung dieser Verbindung ist aus Beispiel 9 der DE-OS - 37 40 650 bekannt.or their alkali salt is used. A preparation of this compound is known from Example 9 of DE-OS - 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 method according to the invention consist in that the fibers are used in the undyed state, or that the treatment is carried out, the fibers being dyed at the same time, or that the fibers are present as fiber structures.
Die vorliegende Erfindung betrifft ferner die Verwendung einer Verbindung der allgemeinen FormelThe present invention further relates to the use of a compound of the general formula
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.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 a 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) to improve the Pilling behavior, to reduce the formation of pills and to improve the chafing 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 Lyocell genus which can be obtained by the process according to the invention, or to yarns and fiber structures which 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.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) Herstellung der Cellulosefasern1) Production of the cellulose fibers
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.Cellulose fibers of the Lyocell genus were produced in accordance with the process described in EP-A-0 356 419 and WO 93/19230. 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) Allgemeine Färbevorschrift2) General staining instructions
Das Textil wird bei einem Flottenverhältnis von 1:20 mit 6% Reaktivfarbstoff (Remazol Brilliantblau BB oder Remazol Schwarz B) ιo Minuten bei 40*c imprägniert. Das Färbebad enthält 0,3 ml/1 eines Lauffaltenverhinderers (z.B. Biavin 109). Anschließend werden innerhalb von 20 Minuten 50 g/1 Na-SO. portionsweise zugegeben. Anschließend werden 5g/l Na_C0, zugesetzt und wird auf 60'C erwärmt. Nach weiteren 15 Minuten werden 0,25 ml/1 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/1 Weichmacher (Basosoft, Avivan GSA) bei 60'C aviviert.The textile is impregnated with a liquor ratio of 1:20 with 6% reactive dye (Remazol Brilliantblau BB or Remazol Schwarz B) in 40 minutes at 40 * c. The dye bath contains 0.3 ml / 1 of an anti-wrinkle (e.g. Biavin 109). Then 50 g / 1 Na-SO. added in portions. Then 5 g / l Na_C0, are added and the mixture is heated to 60'C. After a further 15 minutes, 0.25 ml / 1 NaOH are added and staining 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 with 1 ml / 1 softener (Basosoft, Avivan GSA) at 60'C.
Beispiel 1example 1
4 Lfm Single Jersey (100% Lyocell, 1,7 dtex, Nm 50) werden mit l g/1 eines Waschmittels (Kiralon Jet), 2 g/1 Na2C0_ 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/1 Na-SO. und eine Erhöhung der Temperatur auf 40"C. Nach weiteren 10 Minuten wird die Konzentration an Na~C0 auf insgesamt 5 g/1 erhöht und auf 80°C erwärmt. Nach 15 Minuten wird kalt und warm gespült und gemäß obiger Vorschrift gefärbt.4 Lfm single jersey (100% Lyocell, 1.7 dtex, Nm 50) with lg / 1 of a detergent (Kiralon Jet), 2 g / 1 Na 2 C0_ 10 minutes at 30 * C treated (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 / 1 Na-SO are added. and an increase in the temperature to 40 "C. After a further 10 minutes, the concentration of Na ~ CO is increased to a total of 5 g / 1 and warmed 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 l g/1 eines Waschmittels (Kiralon Jet), 2 g/1 Na2C03 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 Na2C03 auf insgesamt 5 g/1 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 / 1 of a detergent (Kiralon Jet), 2 g / 1 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 / 1 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/1 eines Waschmittels (Kiralon Jet), 2 g/1 Na CO. 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. Ergebnis der Beispiele l bis 34 linear meters of single jersey (100% Lyocell, 1.7 dtex, Nm 50) are mixed with 1 g / 1 of a detergent (Kiralon Jet), 2 g / 1 Na CO. Treated 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, rinsing is carried out cold and warm and dyeing is carried out according to the above instructions. Result 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 washed 10 times at 60 ° C. after dyeing and dried in a tumbler (in accordance with DIN 53920 or ISO 6330, DIN 26330 without prewash). The assessment of pills and whitening was carried out after the fifth and after the tenth wash. The pill formation during washing shows the behavior when wet.
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:The grading is based on EMPA photo templates and ranges from 1 (= strong; i.e. poor) to 5 (= not available; i.e. good) and is summarized in the following table:
Tabelle 1Table 1
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 2,0Ex. 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 l 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.It can be seen from Table 1 that both the pill formation and the white scrubbing in the samples treated with substance I are greatly reduced after 5 and 10 washes.
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, except that the following fabric is used instead of the single jersey: 100% Lyocell, 1.7 dtex, twill, weft and chain Nm 50, 150 cm long and 30 cm wide.
Beispiel 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.Example 5 This example is analogous to Example 2, but the following fabric is used instead of the single jersey: 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, except that the following fabric is used instead of the single jersey: 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, l Umlauf/Minute) nach obiger Färbevorschrift gefärbt.The fabrics obtained in Examples 4, 5 and 6 are sewn together and dyed on the laboratory jet (Mathis, 40 mm nozzle, 1 revolution / minute) 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.The fabrics of Examples 4 and 5 also show significantly better values than the fabric piece of Example 6 with regard to pill formation and whitening.
Beispiel 7Example 7
4 kg Garn (100% Lyocell, 1,7 dtex, Nm 50) werden mit 2 g/1 Waschmittel (Kiralon OLB), 2 g/1 Na2CO- 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 / 1 detergent (Kiralon OLB), 2 g / 1 Na 2 CO 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/1 Na_S04 portionsweise zugegeben. Dann werden 2,5 g/1 Na-CO, zugesetzt und wird auf 60'C erwärmt. Nach weiteren 15 Minuten werden weitere 7,5 g/1 Na2C03 zugegeben. Nach 15 Minuten erfolgt die Zugabe von 0,25 ml/1 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. It is heated to 50 ° C., and 50 g / 1 Na_S0 4 are added in portions over the course of 55 minutes. Then 2.5 g / 1 Na-CO are added and is heated to 60'C. After a further 15 minutes, a further 7.5 g / 1 Na 2 CO 3 are added. After 15 minutes, 0.25 ml / 1 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/1 Weichmacher (Basosoft, Avivan GSA) bei 60'C aviviert und paraffiniert.Unless otherwise stated below, the tissues are treated with 1 ml / 1 plasticizer (Basosoft, Avivan GSA) at 60'C and waxed.
Aus dem so erhaltenen Garn werden ein Single Jersey und Socken gestrickt.A single jersey and socks are knitted from the yarn thus obtained.
Beispiel 8 (Vergleich)Example 8 (comparison)
4 kg Garn (100% Lyocell, 1,7 dtex, Nm 50) werden mit 2 g/1 Waschmittel (Kiralon OLB), 2 g/1 Na.CO. 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 mixed with 2 g / 1 detergent (Kiralon OLB), 2 g / 1 Na.CO. Treated in a yarn dyeing machine for 30 minutes at 95 * C (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/1 Na SO. portionsweise zugegeben. Dann werden 2,5 g/1 Na_C0 zugesetzt und wird auf 60'C erwärmt. Nach weiteren 15 Minuten werden weitere 7,5 g/1 Na2C03 zugegeben. Nach 15 Minuten erfolgt die Zugabe von 0,25 ml/1 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 / 1 Na 2 SO 4 are added in portions over the course of 55 minutes. Then 2.5 g / 1 Na 2 CO are added and the mixture is heated to 60 ° C. After a further 15 minutes, a further 7 5 g / 1 Na 2 CO 3 are added, after 15 minutes 0.25 ml / 1 NaOH is added and the mixture is stained for a further 30 minutes, after which it is 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/1 Weichmacher (Basosoft, Avivan GSA) bei 60'C aviviert und paraffiniert. Aus dem so erhaltenen Garn werden Socken gestrickt.Unless otherwise stated below, the tissues are treated with 1 ml / 1 plasticizer (Basosoft, Avivan GSA) at 60'C and waxed. 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, l Umlauf/Minute) nach obiger Färbevorschrift gefärbt, wobei die Gewebe 9a bzw. 9b erhalten werden.The single jersey from Example 7 and a single jersey made from the same, untreated yarn are dyed together in the laboratory jet (Mathis, nozzle 40 mm, 1 revolution / minute) according to the above dyeing instructions, the fabrics 9a and 9b being obtained.
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 chafing. In contrast, the single jersey 9b abrasive edges and graying are 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.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.
Tabelle 2Table 2
Beisp. 7 Beisp. 8 Pillsbildung nach 5 Wäschen 4,5 2,0 Weißscheuerung nach 5 Wäschen 5,0 1,0Ex. 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 of Example 7 showed a pilling of 4.5 and a white abrasion 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 l 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. Tabelle 3The 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. Table 3
Pill 125 Pill 500 Pill 2000Pill 125 Pill 500 Pill 2000
Beispiel 9a 4,5 4,0 4,0Example 9a 4.5 4.0 4.0
Beispiel 9b 3,5 2,5 1,0Example 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/1 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/1 Vernetzer (Substanz I bzw. TAHT), 3 ml Netzmittel (Leonil SR), 10 g/1 Weichmacher (Sandolub NV), 10 g/1 Na2C03 und 1 ml/1 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 / 1 crosslinker and 3 ml wetting agent (Leonil SR). Then the fabric is dried at 60 ° C and impregnated again with a liquor (liquor absorption: 80%) which contains 10 g / 1 crosslinking agent (substance I or TAHT), 3 ml wetting agent (Leonil SR), 10 g / 1 plasticizer ( Sandolub NV), 10 g / 1 Na 2 CO 3 and 1 ml / 1 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.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.
Tabelle IVTable IV
Vernetzer Weißscheuerung nach 3 Wäschen nach 5 WäschenCrosslinker white abrasion after 3 washes after 5 washes
TAHT 1,0 1,0TAHT 1.0 1.0
Substanz I 3,0 2,0 Substance I 3.0 2.0

Claims

Patentansprüche:Claims:
l. Verfahren zur Behandlung von Cellulosefasern der Gattungl. Process for the treatment of cellulose fibers of the genus
Lyocell, bei welchem die Fasern mit einem Textilhilfsmittel in Kontakt gebracht werden, dadurch gekennzeichnet, daß als Textilhilfsmittel eine Verbindung mit der allgemeinen FormelLyocell, in which the fibers are brought into contact with a textile auxiliary, characterized in that a compound with the general formula is used as textile auxiliary
bzw. ihr Alkalisalz eingesetzt wird, wobeior their alkali salt is used, wherein
X Halogen, Alkoxy mit 1-4 Kohlenstoffatomen, Amino,X halogen, alkoxy with 1-4 carbon atoms, amino,
Alkylamino mit 1-4 Kohlenstoffatomen, Hydroxysulfonyl, oderAlkylamino with 1-4 carbon atoms, hydroxysulfonyl, or
1-Nicotinyl ist;Is 1-nicotinyl;
Y die allgemeine FormelY the general formula
besitzt, worin n die Zahl 1 oder 2 ist; R Wasserstoff,in which n is the number 1 or 2; R is hydrogen,
2 32 3
Alkyl mit 1-4 Kohlenstoffatomen oder Phenyl ist; R und RIs alkyl of 1-4 carbon atoms or phenyl; R and R
Wasserstoff, Hydroxysulfonyl, Hydroxyl, Halogen, Alkyl mit 1-4 Kohlenstoffatomen oder Carboxyl sind; A Vinyl oder -C2H.B ist, worin B eine unter alkalischen Bedingungen abspaltbare Gruppe ist; und Z gleich Y oder X ist. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß als Textilhilfsmittel die VerbindungAre hydrogen, hydroxysulfonyl, hydroxyl, halogen, alkyl of 1-4 carbon atoms or carboxyl; A is vinyl or -C 2 HB, wherein B is a group which can be split off under alkaline conditions; and Z is Y or X. 2. The method according to claim 1, characterized in that the compound as a textile auxiliary
o O
bzw. ihr Alkalisalz eingesetzt wird.or their alkali salt is used.
3. Verfahren nach einem der Ansprüche l oder 2, dadurch gekennzeichnet, daß die Fasern in ungefärbtem Zustand eingesetzt werden.3. The method according to any one of claims l or 2, characterized in that the fibers are used in the undyed state.
4. Verfahren nach einem der Ansprüche 1 oder 2, dadurch gekennzeichnet, daß die Behandlung durchgeführt wird, wobei die Fasern gleichzeitig gefärbt werden.4. The method according to any one of claims 1 or 2, characterized in that the treatment is carried out, the fibers being dyed simultaneously.
5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß die Fasern als Fasergebilde vorliegen,5. The method according to any one of claims 1 to 4, characterized in that the fibers are present as fiber structures,
6. Verwendung einer Verbindung der allgemeinen Formel6. Use of a compound of the general formula
wobei X, Y und Z die in Anspruch 1 angegebene Bedeutung haben, bzw. ihres Alkalisalzes, als Textilhilfsmittel zur Behandlung von Fasern der Gattung Lyocell. where X, Y and Z have the meaning given in claim 1, or their alkali metal salt, as textile auxiliaries for the treatment of fibers of the Lyocell genus.
7. Verwendung einer Verbindung der allgemeinen Formel7. Use of a compound of the general formula
wobei X, Y und Z die in Anspruch 1 angegebene Bedeutung haben, bzw. ihres Alkalisalzes, als Textilhilfsmittel zur Behandlung von Gebilden aus Fasern der Gattung Lyocell.where X, Y and Z have the meaning given in claim 1, or their alkali metal salt, as textile auxiliaries for the treatment of structures made of fibers of the Lyocell genus.
8. Verwendung nach Anspruch 7, dadurch gekennzeichnet, daß als Fasergebilde ein Garn oder eine textile Fläche eingesetzt wird.8. Use according to claim 7, characterized in that a yarn or a textile surface is used as the fiber structure.
9. Verwendung nach Anspruch 8, dadurch gekennzeichnet, daß als textile Fläche ein Gewebe, Gestricke oder Gewirke eingesetzt wird.9. Use according to claim 8, characterized in that a woven, knitted or knitted fabric is used as the textile surface.
10. Verwendung nach Anspruch 9 zur Verbesserung des Pillingverhaltens der textilen Fläche.10. Use according to claim 9 to improve the pilling behavior of the textile surface.
11. Verwendung nach Anspruch 9 zur Verringerung der Pillsbildung der textilen Fläche.11. Use according to claim 9 to reduce the formation of pills in the textile surface.
12. Verwendung nach Anspruch 9 zur Verbesserung des Weißscheuerverhaltens der textilen Fläche.12. Use according to claim 9 to improve the white abrasion behavior of the textile surface.
13. Fasern der Gattung Lyocell, erhältlich nach einem Verfahren gemäß einem der Ansprüche 1 bis 5. 13. Fibers of the Lyocell genus, obtainable by a process according to one of claims 1 to 5.
14. Fasergebilde, erhältlich nach einem Verfahren gemäß Anspruch 5. 14. Fiber structures obtainable by 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)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
AT0110796A AT409144B (en) 1996-06-21 1996-06-21 METHOD FOR TREATING CELLULOSE FIBERS AND FORMS OF THESE FIBERS
AT1107/96 1996-06-21
AT110796 1996-06-21
PCT/AT1997/000132 WO1997049856A1 (en) 1996-06-21 1997-06-19 Process for treating cellulose fibres and structures made of those fibres

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EP0904444A1 true EP0904444A1 (en) 1999-03-31
EP0904444B1 EP0904444B1 (en) 1999-11-24

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EP97926908A Expired - Lifetime EP0904444B1 (en) 1996-06-21 1997-06-19 Process for treating cellulose fibres and structures made of those fibres

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US (1) US6022378A (en)
EP (1) EP0904444B1 (en)
JP (1) JP2000513412A (en)
CN (1) CN1146684C (en)
AT (2) AT409144B (en)
AU (1) AU721876B2 (en)
BR (1) BR9709916A (en)
CA (1) CA2258500A1 (en)
DE (1) DE59700768D1 (en)
ES (1) ES2142167T3 (en)
GR (1) GR3032485T3 (en)
ID (1) ID17073A (en)
NO (1) NO985955L (en)
TW (1) TW336966B (en)
WO (1) WO1997049856A1 (en)

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EP0903434B1 (en) * 1997-09-17 2002-11-27 Lenzing Aktiengesellschaft Process for the treatment of cellulosic fibres
AT2256U1 (en) 1997-10-15 1998-07-27 Chemiefaser Lenzing Ag METHOD FOR TREATING CELLULOSIC MOLDED BODIES
GB2373784A (en) * 2001-03-30 2002-10-02 Tencel Ltd Lyocell fibre and treatment to reduce fibrillation
AT411863B (en) * 2002-09-16 2004-07-26 Chemiefaser Lenzing Ag BLANKET, PREFERABLY QUILTED BLANKET
US7575599B2 (en) * 2004-07-30 2009-08-18 Spinalmotion, Inc. Intervertebral prosthetic disc with metallic core
US7574126B2 (en) * 2003-12-09 2009-08-11 Panasonic Corporation Lens driving apparatus, imaging apparatus, and lens barrel and camera main body used for this
ATA1332004A (en) * 2004-01-30 2005-10-15 Chemiefaser Lenzing Ag METHOD FOR THE TREATMENT OF SOLVENT-SPUN CELLULOSIC FIBERS
AT507051B1 (en) 2008-06-27 2015-05-15 Chemiefaser Lenzing Ag CELLULOSE FIBER AND METHOD FOR THE PRODUCTION THEREOF
US9416494B2 (en) * 2012-12-26 2016-08-16 Kimberly-Clark Worldwide, Inc. Modified cellulosic fibers having reduced hydrogen bonding
US8980054B2 (en) * 2012-12-26 2015-03-17 Kimberly-Clark Worldwide, Inc. Soft tissue having reduced hydrogen bonding
MX2017014154A (en) * 2015-05-04 2018-07-06 Carbtex Tech Inc Articles of ignition resistant cotton fibers.
EP3771755A1 (en) 2019-08-02 2021-02-03 Lenzing Aktiengesellschaft Method for the preparation of lyocell staple fibres

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Also Published As

Publication number Publication date
WO1997049856A1 (en) 1997-12-31
CN1228131A (en) 1999-09-08
US6022378A (en) 2000-02-08
ATA110796A (en) 2001-10-15
NO985955L (en) 1999-02-03
JP2000513412A (en) 2000-10-10
TW336966B (en) 1998-07-21
GR3032485T3 (en) 2000-05-31
ATE186961T1 (en) 1999-12-15
CN1146684C (en) 2004-04-21
NO985955D0 (en) 1998-12-18
ES2142167T3 (en) 2000-04-01
ID17073A (en) 1997-12-04
AU721876B2 (en) 2000-07-13
AU3159497A (en) 1998-01-14
DE59700768D1 (en) 1999-12-30
CA2258500A1 (en) 1997-12-31
EP0904444B1 (en) 1999-11-24
AT409144B (en) 2002-05-27
BR9709916A (en) 1999-08-10

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