EP0984084B1 - Verfahren zur Herstellung von Cellulosefasern - Google Patents

Verfahren zur Herstellung von Cellulosefasern Download PDF

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Publication number
EP0984084B1
EP0984084B1 EP99123392A EP99123392A EP0984084B1 EP 0984084 B1 EP0984084 B1 EP 0984084B1 EP 99123392 A EP99123392 A EP 99123392A EP 99123392 A EP99123392 A EP 99123392A EP 0984084 B1 EP0984084 B1 EP 0984084B1
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Prior art keywords
fiber
compounds
treatment
cellulose
alkyl
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French (fr)
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EP0984084A3 (de
EP0984084A2 (de
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Wolfgang Dr. Schrott
Wolfram Badura
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BASF SE
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BASF SE
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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
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins
    • 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
    • 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
    • D06M13/395—Isocyanates
    • 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
    • D06M13/402—Amides imides, sulfamic acids
    • D06M13/419—Amides having nitrogen atoms of amide groups substituted by hydroxyalkyl or by etherified or esterified hydroxyalkyl groups
    • 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
    • D06M13/402—Amides imides, sulfamic acids
    • D06M13/432—Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
    • 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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
    • D06M15/423—Amino-aldehyde resins
    • 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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
    • 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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
    • D06M15/568—Reaction products of isocyanates with polyethers
    • 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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
    • D06M15/572—Reaction products of isocyanates with polyesters or polyesteramides
    • 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
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
    • 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
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/35—Abrasion, pilling or fibrillation resistance

Definitions

  • the present invention relates to a new method of manufacture of cellulose fibers spun from solvents reduced tendency to fibrillate by treating the fibers with certain reactive compounds.
  • GB-A-2 043 525 describes the production of cellulose fibers by spinning a cellulose solution in a suitable solvent, e.g. an N-oxide of a tertiary amine, such as N-methylmorpholine-N-oxide, known. In such a spinning process the Cellulose solution extruded through a suitable nozzle and the resulting fiber precursor washed in water and then dried. Such fibers are called “solvent spun Fibers ".
  • Such cellulose fibers spun from solvents offer many technical advantages, but tend to fibrillate. This means the splicing of the finest fiber fibrils, the processing of cellulose fibers in textile production can lead to problems.
  • WO-A-92/07124 recommends the to solve this problem Treatment of the cellulose fibers with an aqueous solution or Dispersion of a polymer that is cationic ionizable over a variety Groups, e.g. a polyvinylimidazoline.
  • EP-A-538 977 teaches the use of compounds which have 2 to 6 functional groups with cellulose can react, e.g. Products based on dichlorotriazine, for this purpose.
  • the object of the present invention was to develop a new method for the production of cellulose fibers spun from solvents with reduced tendency to fibrillate, that comes from other chemical defibrillation reagents.
  • cyclic hydroxy or alkoxyethylene ureas of the general formula VI are used in which R 4 and R 5 are hydrogen or C 1 -C 3 alkyl with the proviso that at least one of the radicals R 4 and R 5 is a C 1 -C 3 alkyl group, and R 6 and R 7 are hydrogen or C 1 -C 4 alkyl.
  • Cyclic hydroxy or alkoxyethylene ureas are used as crosslinkers in the textile field the formaldehyde-free finishing (upgrading) of cellulose-containing known textile materials.
  • the compounds (VI) can be used in the process according to the invention Production of cellulose fibers generally in an aqueous system, preferably in aqueous solution or emulsion, for use arrive, the aqueous system in general, based by weight of the aqueous system, 0.1 to 20% by weight, preferably 0.5 to 10 wt .-%, which has compounds (VI).
  • the preferred solvent in stage 1 is N-methylmorpholine-N-oxide used.
  • the wet fiber obtained in Step 3 is called undried Fiber is usually referred to and referred to the dry weight of the fiber, 120 to 150 wt .-% water.
  • the water content of the dried fiber is generally based on the dry weight of the fiber, 60 to 80 wt .-%.
  • the treatment according to the invention with the compounds (VI) can either on the wet fiber (during or after level 3) or on the dried fiber (after step 4). It is but also a treatment in the fiber production stage (Level 2), e.g. in a precipitation bath, possible.
  • the treatment can for example by adding the aqueous system of the compounds (VI) happen to a circulating bath that is the fiber precursor contains.
  • the fiber precursor can e.g. exist as staple fiber.
  • the treatment is done on the dried fiber, it can these e.g. as staple fiber, fleece, yarn, knitwear or fabric available.
  • the treatment of the fibers in this case can e.g. in aqueous liquor.
  • Treatment is usually at a temperature of 20 to 200 ° C, preferably 40 to 180 ° C, made.
  • the duration of treatment is usually 1 second to 20 minutes, preferably 5 to 60 seconds and in particular 5 to 30 seconds.
  • the treatment can be carried out both at room temperature (20 ° C) with subsequent drying up to 100 ° C as well Condensation at temperatures up to 200 ° C, in particular at 150 to 180 ° C.
  • the treatment of the moist or dried fiber can be 0.1 up to 10% by weight, preferably 0.2 to 5% by weight, in particular 0.2 up to 2% by weight, based in each case on the dry weight of the fiber, of the compounds (VI). In some cases, however, it can also be advantageous to increase the amounts mentioned, e.g. up to approx. 20% by weight.
  • anti-migration agents for example based on oxethylation products, to mention.
  • the reactivity of these agents can be increased by adding catalytic amounts of Lewis acids such as MgCl 2 , ZnCl 2 , AlCl 3 , BF 3 or systems such as MgCl 2 / NaBF 4 or MgSO 4 / NaBF 4 / LiCl or of inorganic or organic acids or corresponding acidic salts, for example HCl, H 2 SO 4 , H 3 PO 4 , p-toluenesulfonic acid, methanesulfonic acid, NaHSO 4 , NaH 2 PO 4 , (NH) 4 HSO 4 or trialkylamine hydrochloride, or of other crosslinking inorganic salts, for example nitrates or teraalkylammonium salts, adapted to the process requirements, ie generally increased.
  • Lewis acids such as MgCl 2 , ZnCl 2 , AlCl 3 , BF 3 or systems
  • the compounds (VI) can be compared the compounds described in EP-A-538 977 purely thermal (without alkali) can be fixed, which makes them optimal in the fiber production process let integrated.
  • the dyeability of the fibers treated in this way with all the usual cellulose fiber dyes, reactive dyes are also generally possible.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Polyurethanes Or Polyureas (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Artificial Filaments (AREA)

Description

Die vorliegende Erfindung betrifft ein neues Verfahren zur Herstellung von aus Lösungsmitteln gesponnenen Cellulosefasern mit verringerter Neigung zum Fibrillieren durch Behandlung der Fasern mit bestimmten reaktiven Verbindungen.
Aus der GB-A-2 043 525 ist die Herstellung von Cellulosefasern durch Spinnen einer Celluloselösung in einem geeigneten Lösungsmittel, z.B. einem N-Oxid eines tertiären Amins, wie N-Methylmorpholin-N-oxid, bekannt. In einem solchen Spinnprozeß wird die Celluloselösung durch eine geeignete Düse extrudiert und die resultierende Faservorstufe in Wasser gewaschen und danach getrocknet. Solche Fasern werden als "aus Lösungsmittel gesponnene Fasern" bezeichnet.
Solche aus Lösungsmitteln gesponnenen Cellulosefasern bieten viele anwendungstechnische Vorteile, neigen aber zum Fibrillieren. Darunter versteht man das Abspleißen feinster Faserfibrillen, die bei der Verarbeitung der Cellulosefasern in der Textilherstellung zu Problemen führen können.
Die WO-A-92/07124 empfiehlt zur Lösung dieses Problems die Behandlung der Cellulosefasern mit einer wäßrigen Lösung oder Dispersion eines Polymers, das über eine Vielzahl kationisch ionisierbarer Gruppen verfügt, z.B. ein Polyvinylimidazolin.
Weiterhin lehrt die EP-A-538 977 die Verwendung von Verbindungen, die 2 bis 6 funktionelle Gruppen aufweisen, die mit Cellulose reagieren können, z.B. Produkte auf Basis von Dichlortriazin, für diesen Zweck.
Aufgabe der vorliegenden Erfindung war es, ein neues Verfahren zur Herstellung von aus Lösungsmitteln gesponnenen Cellulosefasern mit verringerter Neigung zum Fibrillieren bereitzustellen, das von anderen chemischen Defibrillierungsreagenzien ausgeht.
Es wurde nun gefunden, daß die Herstellung von aus Lösungsmitteln gesponnenen Cellulosefasern mit verringerter Neigung zum Fibrillieren vorteilhaft gelingt, wenn man die Fasern mit einer oder mehreren Verbindungen aus der Gruppe der cyclischen Hydoxy- oder Alkoxyethylenharnstoffen der allgemeinen Formel VI,
Figure 00020001
behandelt, in der R4 und R5 Wasserstoff oder C1-C3-Alkyl mit der Maßgabe bedeuten, daß mindestens einer der Reste R4 und R5 eine C1-C3-Alkylgruppe ist, und R6 und R7 für Wasserstoff oder C1-C4-Alkyl stehen, ein.
Erfindungsgemäß setzt man cyclische Hydroxy- oder Alkoxyethylenharnstoffe der allgemeinen Formel VI
Figure 00030001
in der R4 und R5 Wasserstoff oder C1-C3-Alkyl mit der Maßgabe bedeuten, daß mindestens einer der Reste R4 und R5 eine C1-C3-Alkylgruppe ist, und R6 und R7 für Wasserstoff oder C1-C4-Alkyl stehen, ein.
Verbindungen aus der Gruppe der durch eine oder mehrere Alkylgruppen N-substituierten cyclischen Hydroxy-oder Alkoxyethylenharnstoffe sind auf dem Textilgebiet als Vernetzer bei der formaldehydfreien Ausrüstung (Hochveredlung) von cellulosehaltigen textilen Materialien bekannt.
Die Verbindungen (VI) können beim erfindungsgemäßen Verfahren zur Herstellung von Cellulosefasern generell in einem wäßrigen System, vorzugsweise in wäßriger Lösung oder Emulsion, zur Anwendung gelangen, wobei das wäßrige System im allgemeinen, bezogen auf das Gewicht des wäßrigen Systems, 0,1 bis 20 Gew.-%, vorzugsweise 0,5 bis 10 Gew.-%, der Verbindungen (VI) aufweist.
Die Herstellverfahren für aus Lösungsmittel gesponnene Cellulosefasern laufen in der Regel in 4 Stufen ab.
Stufe 1:
Lösen der Cellulose in einem mit Wasser mischbaren Lösungsmittel
Stufe 2:
Extrudieren der Lösung durch eine Düse unter Bildung der Faservorstufe
Stufe 3:
Behandlung der Faservorstufe mit Wasser um Lösungsmittel zu entfernen und die Cellulosefaser auszubilden
Stufe 4:
Trocknung der Faser
Als Lösungsmittel in Stufe 1 wird vorzugsweise N-Methylmorpholin-N-oxid verwendet.
Die feuchte Faser, die in Stufe 3 erhalten wird, wird als nichtgetrocknete Faser bezeichnet und weist in der Regel, bezogen auf das Trockengewicht der Faser, 120 bis 150 Gew.-% Wasser auf.
Der Wassergehalt der getrockneten Faser beträgt im allgemeinen, bezogen auf das Trockengewicht der Faser, 60 bis 80 Gew.-%.
Die erfindungsgemäße Behandlung mit den Verbindungen (VI) kann entweder an der feuchten Faser (während oder nach Stufe 3) oder an der getrockneten Faser (nach Stufe 4) erfolgen. Es ist aber auch eine Behandlung im Stadium der Faserherstellung (Stufe 2), z.B. in einem Fällbad, möglich.
Wenn die Behandlung an der feuchten Faser erfolgt, so kann dies beispielsweise durch Zugabe des wäßrigen Systems der Verbindungen (VI) zu einem zirkulierenden Bad geschehen, das die Faservorstufe enthält. Die Faservorstufe kann dabei z.B. als Stapelfaser vorliegen.
Wenn die Behandlung an der getrockneten Faser erfolgt, so kann diese z.B. als Stapelfaser, Vlies, Garn, Maschenware oder Gewebe vorliegen. Die Behandlung der Fasern in diesem Fall kann z.B. in wäßriger Flotte erfolgen.
Im Gegensatz zu der in der EP-A-538 977 beschriebenen Methode kann im erfindungsgemäßen Verfahren auf die Anwesenheit von Alkali verzichtet werden.
Die Behandlung wird in der Regel bei einer Temperatur von 20 bis 200°C, vorzugsweise 40 bis 180°C, vorgenommen. Dabei erfolgt eine chemische Reaktion der Verbindungen (VI) mit den Hydroxygruppen der Cellulose, wobei auch eine chemische Verknüpfung zwischen Hydroxygruppen verschiedener Cellulose-Fibrillen möglich ist. Dadurch wird die Stabilität der Faser erhöht.
Die Zeitdauer der Behandlung beträgt üblicherweise 1 Sekunde bis 20 Minuten, vorzugsweise 5 bis 60 Sekunden und insbesondere 5 bis 30 Sekunden.
Beim Imprägnierverfahren kann die Behandlung sowohl bei Raumtemperatur (20°C) mit anschließender Trocknung bis 100°C als auch bei Durchführung von Kondensationen bei Temperaturen bis zu 200°C, insbesondere bei 150 bis 180°C, erfolgen.
Die Behandlung der feuchten oder getrockneten Faser kann mit 0,1 bis 10 Gew.-%, vorzugsweise 0,2 bis 5 Gew.-%, insbesondere 0,2 bis 2 Gew.-%, jeweils bezogen auf das Trockengewicht der Faser, der Verbindungen (VI) erfolgen. In manchen Fällen kann es jedoch auch vorteilhaft sein, die genannten Mengen noch zu erhöhen, z.B. bis auf ca. 20 Gew.-%.
Bei der Behandlung können weitere hierbei übliche Hilfsmittel in den hierfür üblichen Mengen mitverwendet werden. Insbesondere sind hier Antimigrationsmittel, beispielsweise auf Basis von Oxethylierungsprodukten, zu erwähnen.
Bei der erfindungsgemäßen Verwendung der Verbindungen (VI) kann die Reaktivität dieser Mittel durch Zusatz katalytischer Mengen von Lewis-Säuren wie MgCl2, ZnCl2, AlCl3, BF3 oder Systemen wie MgCl2/NaBF4 oder MgSO4/NaBF4/LiCl oder von anorganischen oder organischen Säuren oder entsprechenden sauren Salzen, z.B. HCl, H2SO4, H3PO4, p-Toluolsulfonsäure, Methansulfonsäure, NaHSO4, NaH2PO4, (NH)4HSO4 oder Trialkylamin-Hydrochlorid, oder von anderen vernetzend wirkenden anorganischen Salzen, z.B. Nitraten oder Teraalkylammoniumsalzen, den Prozeßerfordernissen angepaßt, d.h. in der Regel erhöht werden.
Wie bereits ausgeführt, können die Verbindungen (VI) gegenüber den in der EP-A-538 977 beschriebenen Verbindungen rein thermisch (ohne Alkali) fixiert werden, wodurch sie sich optimal in den Faserherstellungsprozeß integrieren lassen. Die Anfärbbarkeit der so behandelten Fasern mit allen üblichen Cellulosefaserfarbstoffen, auch Reaktivfarbstoffen, ist in der Regel möglich.
Unter Anwendung der in der EP-A-538 977 beschriebenen Testmethoden, auf die hier ausdrücklich Bezug genommen wird, können vorteilhafte Ergebnisse erzielt werden.

Claims (3)

  1. Verfahren zur Herstellung von aus Lösungsmitteln gesponnenen Cellulosefasern mit verringerter Neigung zum Fibrillieren, dadurch gekennzeichnet, daß man die Fasern mit einer oder mehreren Verbindungen aus der Gruppe der
    cyclischen Hydroxy- oder Alkoxyethylenharnstoffe der allgemeinen Formel VI
    Figure 00070001
    behandelt, in der R4 und R5 Wasserstoff oder C1-C3-Alkyl mit der Maßgabe bedeuten, daß mindestens einer der Reste R4 und R5 eine C1-C3-Alkylgruppe ist, und R6 und R7 für Wasserstoff oder C1-C4-Alkyl stehen, einsetzt.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß man die Fasern mit 0,1 bis 10 Gew.-%, bezogen auf das Trockengewicht der Fasern, der Verbindungen (B) behandelt.
  3. Verfahren nach den Ansprüchen 1 oder 2, dadurch gekennzeichnet, daß man die Behandlung bei einer Temperatur von 20 bis 200°C vornimmt.
EP99123392A 1994-09-06 1995-08-22 Verfahren zur Herstellung von Cellulosefasern Expired - Lifetime EP0984084B1 (de)

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DE4431635 1994-09-06
DE4431635A DE4431635A1 (de) 1994-09-06 1994-09-06 Verfahren zur Herstellung von Cellulosefasern
EP95931179A EP0779942B1 (de) 1994-09-06 1995-08-22 Verfahren zur herstellung von cellulosefasern

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EP0984084A2 EP0984084A2 (de) 2000-03-08
EP0984084A3 EP0984084A3 (de) 2000-04-19
EP0984084B1 true EP0984084B1 (de) 2003-01-02

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EP99123391A Expired - Lifetime EP0985747B1 (de) 1994-09-06 1995-08-22 Verfahren zur Herstellung von Cellulosefasern
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US (1) US5776394A (de)
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CN1886427B (zh) 2003-11-28 2012-05-23 伊士曼化工公司 纤维素共聚体和氧化方法
US9416494B2 (en) 2012-12-26 2016-08-16 Kimberly-Clark Worldwide, Inc. Modified cellulosic fibers having reduced hydrogen bonding
US9410292B2 (en) 2012-12-26 2016-08-09 Kimberly-Clark Worldwide, Inc. Multilayered tissue having reduced hydrogen bonding
US8980054B2 (en) 2012-12-26 2015-03-17 Kimberly-Clark Worldwide, Inc. Soft tissue having reduced hydrogen bonding
KR102440861B1 (ko) * 2020-05-26 2022-09-05 오영세 라이오셀 섬유의 제조방법 및 이로부터 제조된 라이오셀 섬유
CN116926971B (zh) * 2023-06-30 2024-07-12 广东德美精细化工集团股份有限公司 一种抗原纤化组合物及在莱赛尔织物上的应用

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EP0531820A1 (de) * 1991-09-10 1993-03-17 Bayer Ag Polyisocyanatgemische, ein Verfahren zu ihrer Herstellung und ihre Verwendung
EP0538977A1 (de) * 1991-10-21 1993-04-28 Courtaulds Plc Faserbehandlung
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DK0779942T3 (da) 2000-08-28
EP0984084A3 (de) 2000-04-19
EP0779942A1 (de) 1997-06-25
DE59510523D1 (de) 2003-02-06
EP0985747B1 (de) 2002-10-30
EP0984084A2 (de) 2000-03-08
EP0779942B1 (de) 2000-06-21
JPH10505389A (ja) 1998-05-26
WO1996007780A1 (de) 1996-03-14
DE59508498D1 (de) 2000-07-27
ES2148552T3 (es) 2000-10-16
ES2190169T3 (es) 2003-07-16
ATE226985T1 (de) 2002-11-15
US5776394A (en) 1998-07-07
ATE230447T1 (de) 2003-01-15
DE4431635A1 (de) 1996-03-07
DE59510440D1 (de) 2002-12-05
ATE194018T1 (de) 2000-07-15
EP0985747A3 (de) 2000-04-19

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