EP0877788B1 - Solid, waterless preparations - Google Patents

Solid, waterless preparations Download PDF

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Publication number
EP0877788B1
EP0877788B1 EP97903271A EP97903271A EP0877788B1 EP 0877788 B1 EP0877788 B1 EP 0877788B1 EP 97903271 A EP97903271 A EP 97903271A EP 97903271 A EP97903271 A EP 97903271A EP 0877788 B1 EP0877788 B1 EP 0877788B1
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EP
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Prior art keywords
weight
fabric
cotton fabric
fatty alcohol
preparations
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EP97903271A
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German (de)
French (fr)
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EP0877788A1 (en
Inventor
Teresa Copete Vidal
Emili Brau Balague
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BASF Personal Care and Nutrition GmbH
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Cognis Deutschland GmbH and Co KG
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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/38Products with no well-defined composition, e.g. natural products
    • C11D3/386Preparations containing enzymes, e.g. protease or amylase
    • C11D3/38645Preparations containing enzymes, e.g. protease or amylase containing cellulase
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/72Ethers of polyoxyalkylene glycols
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/2075Carboxylic acids-salts thereof
    • C11D3/2086Hydroxy carboxylic acids-salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P5/00Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
    • D06P5/15Locally discharging the dyes
    • D06P5/151Locally discharging the dyes with acids or bases
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P5/00Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
    • D06P5/15Locally discharging the dyes
    • D06P5/158Locally discharging the dyes with other compounds

Definitions

  • the invention relates to solid preparations with a defined content of acidic cellulases, selected Fatty alcohol polyglycol ether and buffer salts, a process for producing a "stonewash” - Effect on dyed cotton fabric using the preparations mentioned and their Use as a means of producing dyed cotton fabrics with a "stonewash” effect.
  • EP-A2 0307564 and EP-A1 0665324 Ecolab
  • processes for creating differently colored areas of textiles made of cellulose by treatment with an aqueous liquor which, in addition to cellulases, contain nonionic surfactants of the fatty alcohol ethoxylate type with up to 20 ethylene oxide units can contain per mole of fatty alcohol.
  • Cellulases (1,4- ⁇ -D-glucan-4-glucanohydrolases; EC 3.2.1.4.) are enzyme complexes that are involved in the breakdown of native cellulose.
  • the acidic cellulases to be used according to the invention are enzymes which are preferably prepared from cultures of Aspergillus or Trichoderma species and which have an optimum activity at acidic pH values in the range from 4 to 6. Acidic cellulases, which are sold by Novo Nordisk under the Celluzyme® brand and are produced by submerged fermentation of the Humicola insolens fungus, are particularly preferred. Overviews of the interaction of cellulases with cellulose are, for example, from E.Hoshino in J. Biochem. 114 , 230; 236 (1994), ibid. 115 , 837 (1994) and J. Ferment. Bioeng. 77 , 496 (1994) .
  • Fatty alcohol polyglycol ethers are known nonionic surfactants which are obtained on an industrial scale by alkoxylating fatty alcohols with ethylene oxide and / or propylene oxide in the presence of homogeneous or heterogeneous alkaline catalysts. With regard to the parameters of enzyme stabilization, activity and dust-binding capacity, the selection of these components has proven to be critical. Fatty alcohol polyglycol ethers which form component (b) and which are to be used particularly advantageously therefore follow the formula (I) in which R 1 is a linear alkyl radical having 16 to 22 carbon atoms and n is preferably a number from 50 to 80. Typical examples are addition products of an average of 40 to 100 and in particular 50 to 60 moles of ethylene oxide in technical terms tallow fatty alcohols with 16 to 18 carbon atoms.
  • the choice of the inorganic or organic salts is in itself not very critical. In terms of stabilization the cellulases and the dust-binding capacity, however, have alkali and / or alkaline earth sulfates, -carbonates, -phosphates and -citrates especially proven. Typical examples are sodium sulfate, Potassium sulfate, calcium carbonate, sodium phosphate and sodium citrate. Although it goes without saying citric acid can also be considered.
  • the preparations according to the invention are used in amounts of customary 0.1 to 10 and preferably 1 to 5 wt .-% - based on the cotton fabric - used.
  • the liquor weight ratio of cotton fabric to water is usually in the range of 1: 10 to 1: 100.
  • a fleet consisting of about 3 to 5 kg of denim and 50 to 80 is preferred kg of water is prepared, which is 30 to 200 and preferably 50 to 100 g of the preparations according to the invention adds. It is recommended to use the procedure at a pH in the range of 4.5 to 5.5 and at a temperature in the range of 50 to 65, preferably 55 to 60 ° C. If If desired, conventional fabric softener can be used together with the preparations.
  • the preparations according to the invention impart colored cotton fabrics, in particular blue ones Denim not only a typical "stonewash” effect, but also a pleasant soft touch, she thus also improve comfort.
  • Another object of the invention therefore relates the use of the solid preparations according to the invention to achieve a "stonewash" effect on dyed cotton fabric.
  • Example 1 A pair of brand-new blue jeans were placed in a Siemens Siewamat 3573 washing machine with a capacity of 5.5 kg of laundry and about 60 l of water. The jeans were prewashed once at 40 ° C with a conventional detergent containing amylase. 50 g of a preparation consisting of: 15% by weight of Celluzyme, 15% by weight tallow fatty alcohol + 50 EO and 70% by weight sodium citrate / citric acid (1: 1) added. The dust development during filling was assessed as “dust-free” (+) or “not dust-free” (-). The liquor was treated at 55 ° C. for 60 min and then rinsed clear twice. The "stonewash" effect and the soft feel were assessed subjectively by a panel consisting of 6 trained people on a scale from 1 (very clear or very soft) to 6 (hardly noticeable or hard). The result is summarized in Table 1.
  • Example 1 was repeated, but instead of the tallow fatty alcohol + 50 EO a tallow fatty alcohol + 20EO was used and the treatment was carried out over a period of 60 min at a temperature of 55 ° C. The results are summarized in Table 1.
  • Comparative example V2 Comparative example V2. Comparative example V1 was repeated, but the treatment was carried out over a period of 90 minutes, not over a period of 60 minutes. The results are summarized in Table 1.
  • Comparative Example V3 Comparative Example V3. Comparative example V2 was repeated, but the treatment was carried out not at a temperature of 55, but 40 ° C. The results are summarized in Table 1
  • the example and the comparative examples show that only when the preparations according to the invention are used dyed cotton fabrics are obtained, which are characterized both by an optimal "stonewash” effect as well as a pleasant soft feel.
  • the preparations according to the invention are practical when decanting dust free.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Textile Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Detergent Compositions (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Description

Gebiet der ErfindungField of the Invention

Die Erfindung betrifft feste Zubereitungen mit einem definierten Gehalt an sauren Cellulasen, ausgewählten Fettalkoholpolyglycolethem und Puffersalzen, ein Verfahren zur Erzeugung eines "stonewash"- Effektes auf gefärbtem Baumwollgewebe unter Einsatz der genannten Zubereitungen sowie deren Verwendung als Mittel zur Herstellung von gefärbten Baumwollgewebe mit "stonewash"-Effekt.The invention relates to solid preparations with a defined content of acidic cellulases, selected Fatty alcohol polyglycol ether and buffer salts, a process for producing a "stonewash" - Effect on dyed cotton fabric using the preparations mentioned and their Use as a means of producing dyed cotton fabrics with a "stonewash" effect.

Stand der TechnikState of the art

Die Weltproduktion von Jeans beträgt jährlich mehrere Millionen Stück. Ein guter Teil dieser Menge wird einem künstlichen Alterungsprozeß unterzogen, bei dem man die Jeans zusammen mit Steinen in einer Waschflotte behandelt und dabei zwar einerseits abnutzt, gleichzeitig aber auch den Weichgriff verbessert und somit den Tragekomfort steigert. Die mit der Abnutzung verbundene statistische Auswaschung von Farbe wird im übrigen vom Verbraucher häufig gewünscht ("stonewash"-Eftekt).The world production of jeans is several million pieces annually. A good part of that amount is subjected to an artificial aging process, in which the jeans are put together with stones in treated with a wash liquor, which on the one hand wears out, but at the same time also softens the handle improved and thus increases comfort. The statistical washout associated with wear Color is otherwise often desired by the consumer ("stonewash" effect).

Natürlich stellt die Beladung von Waschmaschinen mit Steinen einen Vorgang dar, der hohe Anforderungen an den Werkstoff stellt. Auch der Umstand, daß pro Waschvorgang nur eine begrenzte Zahl von Jeans so behandelt werden können und ein nicht unbeträchtlicher Teil von ihnen bei dieser Prozedur so stark geschädigt wird, daß er für den Verkauf nicht mehr in Frage kommt, ließen es geboten erscheinen, den Vorgang statt auf mechanischem auf chemischem Wege durchzuführen. Aus dem Stand der Technik war bereits bekannt, daß Cellulasen über die Eigenschaft verfügen, blauen Indigofarbstoff von Denimfasem abzulösen. Eine Übersicht hierzu ist von N.K.Lange in C.R. 2.TRICEL Symposium, Espoo, Finnland, 1993, S. 263 erschienen.Of course, loading washing machines with stones is a process that places high demands on the material. The fact that only a limited number of jeans can be treated per washing process and that a not inconsiderable part of them are so badly damaged during this procedure that it is no longer suitable for sale made the process seem necessary instead of performing it mechanically by chemical means. It was already known from the prior art that cellulases have the property of detaching blue indigo dye from denim fibers. An overview of this has been published by NKLange in CR 2.TRICEL Symposium, Espoo, Finland, 1993, p. 263 .

In der Weiterentwicklung dieser Erkenntnis schlägt die Europäische Patentschrift EP-B1 0452393 (Cayla) ein Verfahren zum heterogenen Vorwaschen von Baumwolltextilien vor, das unter Verwendung bestimmter Cellulasen bei pH-Werten unterhalb von pH = 6 durchgeführt wird. Aus den beiden Europäischen Patentanmeldung EP-A2 0307564 und EP-A1 0665324 (Ecolab) sind Verfahren zum Schaffen unterschiedlich gefärbter Bereiche von Textilien aus Cellulose durch Behandeln mit einer wäßrigen Flotte bekannt, die neben Cellulasen nichtionische Tenside vom Typ der Fettalkoholethoxylate mit bis zu 20 Ethylenoxideinheiten pro Mol Fettalkohol enthalten können.In the further development of this knowledge, the European patent EP-B1 0452393 (Cayla) proposes a process for the heterogeneous prewashing of cotton textiles, which is carried out using certain cellulases at pH values below pH = 6. From the two European patent applications EP-A2 0307564 and EP-A1 0665324 (Ecolab), processes for creating differently colored areas of textiles made of cellulose by treatment with an aqueous liquor are known which, in addition to cellulases, contain nonionic surfactants of the fatty alcohol ethoxylate type with up to 20 ethylene oxide units can contain per mole of fatty alcohol.

Auch wenn es möglich ist, unter Einsatz von Produkten des Stands der Technik "stonewashed"-Jeans herzustellen, die denen nach konventioneller mechanischer Behandlung erhältlichen optisch kaum nachstehen, bleiben doch eine Reihe von Problemen ungelöst. So lassen beispielsweise die Enzymstabilisierung und insbesondere das Staubbindevermögen von Produkten gemäß des Stands der Technik zu wünschen übrig. Die Aufgabe der Erfindung hat somit darin bestanden, hochaktive Zubereitungen zur Erzielung eines "stonewash"-Effektes auf gefärbtem Baumwollgewebe hervorzurufen, die sich gleichzeitig noch durch ein hohes Staubbindevermögen auszeichnen und den behandelten Geweben einen angenehmen Weichgriff verleihen.Even if it is possible to use stonewashed jeans using state-of-the-art products to produce the optically hardly available to those available after conventional mechanical treatment inferior, a number of problems remain unsolved. For example, enzyme stabilization and in particular the dust-binding capacity of products according to the prior art to be desired. The object of the invention was therefore to provide highly active preparations to achieve a "stonewash" effect on dyed cotton fabric that evokes at the same time characterized by a high dust-binding capacity and the treated fabrics give a pleasant soft feel.

Beschreibung der ErfindungDescription of the invention

Gegenstand der Erfindung sind feste, wasserfreie Zubereitungen, bestehend aus

  • (a) 5 bis 50 Gew.-% sauren Cellulasen,
  • (b) 10 bis 20 Gew.-% Fettalkoholpolyglycolethem der Formel (I), R1O(CH2CH2O)nH in der R1 für einen linearen Alkylrest mit 16 bis 22 Kohlenstoffatomen und n für Zahlen von 40 bis 100 steht, und
  • (c) ad 100 Gew.-% Citronensäure, anorganischen und/oder organischen Salzen.
  • The invention relates to solid, anhydrous preparations consisting of
  • (a) 5 to 50% by weight of acidic cellulases,
  • (b) 10 to 20% by weight of fatty alcohol polyglycol ether of the formula (I) , R 1 O (CH 2 CH 2 O) n H in which R 1 is a linear alkyl radical having 16 to 22 carbon atoms and n is a number from 40 to 100, and
  • (c) ad 100% by weight of citric acid, inorganic and / or organic salts.
  • Überraschenderweise wurde gefunden, daß sich Zubereitungen der genannten Art in besonderer Weise eignen, um auf gefärbtem Jeansstoff einen "stonewash"-Effekt hervorzurufen. Die Erfindung schließt die Erkenntnis ein, daß ein besonders vorteilhafter Effekt bei Temperaturen oberhalb von 50 und vorzugsweise bei 55 bis 65°C erreicht wird, also durchaus oberhalb des Aktivitätsoptimums der sauren Celluasen. Gegenüber Produkten des Stands der Technik, die als Tenside niedrigethoxylierte Fettalkoholpolyglycolether enthalten, wird eine verbesserte Enzymstabilisierung und damit eine höhere Aktivität und ein höheres Staubbindevermögen beobachtet, was es nicht nur möglich macht, den Prozeß mit einer niedrigeren Cellulasekonzentration durchzuführen, sondern auch Vorteile im Hinblick auf die Arbeitssicherheit und die Abwasserbelastung bietet. Surprisingly, it was found that preparations of the type mentioned are in a special way are suitable to create a "stonewash" effect on dyed denim. The invention closes the finding that a particularly advantageous effect at temperatures above 50 and preferably is reached at 55 to 65 ° C, well above the optimum activity of the acid Celluases. Compared to products of the prior art which, as surfactants, have low-ethoxylated fatty alcohol polyglycol ethers will contain an improved enzyme stabilization and thus a higher Activity and a higher dust-binding capacity are observed, which not only makes the process possible perform with a lower cellulase concentration, but also benefits in terms of offers occupational safety and wastewater pollution.

    Ein weiterer Gegenstand der Erfindung betrifft ein Verfahren zur Herstellung von Baumwollgewebe mit "stonewash"-Effekt, bei dem man eine wäßrige Flotte, enthaltend gefärbtes Baumwollgewebe mit einer festen, praktisch Zubereitung, bestehend aus

  • (a) 5 bis 50 Gew.-% sauren Cellulasen,
  • (b) 10 bis 20 Gew.-% Fettalkoholpolyglycolethem der Formel (I), R1O(CH2CH2O)nH in der R1 für einen linearen Alkylrest mit 16 bis 22 Kohlenstoffatomen und n für Zahlen von 40 bis 100 steht, und
  • (c) ad 100 Gew.-% Citronensäure, anorganischen und/oder organischen Salzen
  • behandelt.Another object of the invention relates to a process for the production of cotton fabric with a "stonewash" effect, in which an aqueous liquor containing dyed cotton fabric with a solid, practical preparation consisting of
  • (a) 5 to 50% by weight of acidic cellulases,
  • (b) 10 to 20% by weight of fatty alcohol polyglycol ether of the formula (I) , R 1 O (CH 2 CH 2 O) n H in which R 1 is a linear alkyl radical having 16 to 22 carbon atoms and n is a number from 40 to 100, and
  • (c) ad 100% by weight of citric acid, inorganic and / or organic salts
  • treated.

    Saure CellulasenAcid cellulases

    Cellulasen (1,4-β-D-Glucan-4-glucanohydrolasen; EC 3.2.1.4.) stellen Enzymkomplexe dar, die am Abbau nativer Cellulose beteiligt sind. Bei den erfindungsgemäß einzusetzenden sauren Cellulasen handelt es sich um Enzyme, die vorzugsweise aus Kulturen von Aspergillus- oder Trichoderma-Arten hergestellt werden und ein Aktivitätsoptimum bei sauren pH-Werten im Bereich von 4 bis 6 aufweisen. Besonders bevorzugt sind saure Cellulasen, die unter der Marke Celluzyme® von der Novo Nordisk vertrieben und durch submerse Fermentation des Pilzes Humicola insolens hergestellt werden. Übersichten zur Wechselwirkung von Cellulasen mit Cellulose sind beispielsweise von E.Hoshino in J. Biochem. 114, 230; 236 (1994), ibid. 115, 837 (1994) sowie J. Ferment. Bioeng. 77, 496 (1994) zu finden.Cellulases (1,4-β-D-glucan-4-glucanohydrolases; EC 3.2.1.4.) Are enzyme complexes that are involved in the breakdown of native cellulose. The acidic cellulases to be used according to the invention are enzymes which are preferably prepared from cultures of Aspergillus or Trichoderma species and which have an optimum activity at acidic pH values in the range from 4 to 6. Acidic cellulases, which are sold by Novo Nordisk under the Celluzyme® brand and are produced by submerged fermentation of the Humicola insolens fungus, are particularly preferred. Overviews of the interaction of cellulases with cellulose are, for example, from E.Hoshino in J. Biochem. 114 , 230; 236 (1994), ibid. 115 , 837 (1994) and J. Ferment. Bioeng. 77 , 496 (1994) .

    FettalkoholpolyglycoletherFatty alcohol polyglycol ether

    Fettalkoholpolyglycolether stellen bekannte nichtionische Tenside dar, die man großtechnisch durch Alkoxylierung von Fettalkoholen mit Ethylenoxid und/oder Propylenoxid in Gegenwart homogener oder heterogener alkalischer Katalysatoren erhält. Im Hinblick auf die Parameter Enzymstabilisierung, Aktivität und Staubbindevermögen hat sich die Auswahl dieser Komponenten als kritisch erwiesen. Besonders vorteilhaft einzusetzende Fettalkoholpolyglycolether, die die Komponente (b) bilden, folgen daher der Formel (I), in der R1 für einen linearen Alkylrest mit 16 bis 22 Kohlenstoffatomen und n vorzugsweise für Zahlen von 50 bis 80 steht. Typische Beispiele sind Anlagerungsprodukte von durchschnittlich 40 bis 100 und insbesondere 50 bis 60 Mol Ethylenoxid dn technisch Talgfettalkohole mit 16 bis 18 Külilenstoffatomen.Fatty alcohol polyglycol ethers are known nonionic surfactants which are obtained on an industrial scale by alkoxylating fatty alcohols with ethylene oxide and / or propylene oxide in the presence of homogeneous or heterogeneous alkaline catalysts. With regard to the parameters of enzyme stabilization, activity and dust-binding capacity, the selection of these components has proven to be critical. Fatty alcohol polyglycol ethers which form component (b) and which are to be used particularly advantageously therefore follow the formula (I) in which R 1 is a linear alkyl radical having 16 to 22 carbon atoms and n is preferably a number from 50 to 80. Typical examples are addition products of an average of 40 to 100 and in particular 50 to 60 moles of ethylene oxide in technical terms tallow fatty alcohols with 16 to 18 carbon atoms.

    SalzeSalts

    Die Wahl der anorganischen bzw. organischen Salze ist an sich wenig kritisch. Im Hinblick auf die Stabilisierung der Cellulasen und das Staubbindevermögen haben sich jedoch Alkali- und/oder Erdalkalisulfate, -carbonate, -phosphate und -citrate besonders bewährt. Typische Beispiele sind Natriumsulfat, Kaliumsulfat, Calciumcarbonat, Natriumphosphat und Nathumcitrat. Obschon es sich selbstverständlich nicht um ein Salz handelt, kommt zudem auch Citronensäure in Betracht.The choice of the inorganic or organic salts is in itself not very critical. In terms of stabilization the cellulases and the dust-binding capacity, however, have alkali and / or alkaline earth sulfates, -carbonates, -phosphates and -citrates especially proven. Typical examples are sodium sulfate, Potassium sulfate, calcium carbonate, sodium phosphate and sodium citrate. Although it goes without saying citric acid can also be considered.

    Durchführung des VerfahrensExecution of the procedure

    Zur Durchführung des Verfahrens werden die erfindungsgemäßen Zubereitungen in Mengen von üblicherweise 0,1 bis 10 und vorzugsweise 1 bis 5 Gew.-% - bezogen auf das Baumwollgewebe - eingesetzt. Das Flottengewichtsverhältnis Baumwollgewebe zu Wasser liegt in der Regel im Bereich von 1 : 10 bis 1 : 100. Vorzugsweise wird eine Flotte bestehend aus etwa 3 bis 5 kg Jeansstoff und 50 bis 80 kg Wasser hergestellt, der man 30 bis 200 und vorzugsweise 50 bis 100 g der erfindungsgemäßen Zubereitungen zusetzt. Es empfiehlt sich, das Verfahren bei einem pH-Wert im Bereich von 4,5 bis 5,5 und bei einer Temperatur im Bereich von 50 bis 65, vorzugsweise 55 bis 60°C durchzuführen. Falls gewünscht, kann man zusammen mit den Zubereitungen konventionelle Wäscheweichspülmittel einsetzen.To carry out the process, the preparations according to the invention are used in amounts of customary 0.1 to 10 and preferably 1 to 5 wt .-% - based on the cotton fabric - used. The liquor weight ratio of cotton fabric to water is usually in the range of 1: 10 to 1: 100. A fleet consisting of about 3 to 5 kg of denim and 50 to 80 is preferred kg of water is prepared, which is 30 to 200 and preferably 50 to 100 g of the preparations according to the invention adds. It is recommended to use the procedure at a pH in the range of 4.5 to 5.5 and at a temperature in the range of 50 to 65, preferably 55 to 60 ° C. If If desired, conventional fabric softener can be used together with the preparations.

    Gewerbliche AnwendbarkeitIndustrial applicability

    Die erfindungsgemäßen Zubereitungen verleihen gefärbtem Baumwollgewebe, insbesondere blauem Denim nicht nur einen typischen "stonewash"-Effekt, sondern auch einen angenehmen Weichgriff, sie verbessern zudem also auch den Tragekomfort. Ein weiterer Gegenstand der Erfindung betrifft daher die Verwendung der erfindungsgemäßen festen Zubereitungen zur Erzielung eines "stonewash"-Effektes auf gefärbtem Baumwollgewebe. The preparations according to the invention impart colored cotton fabrics, in particular blue ones Denim not only a typical "stonewash" effect, but also a pleasant soft touch, she thus also improve comfort. Another object of the invention therefore relates the use of the solid preparations according to the invention to achieve a "stonewash" effect on dyed cotton fabric.

    BeispieleExamples

    Beispiel 1. Ein Paar fabrikneuer Blue Jeans wurden in eine Waschmaschine des Typs Siemens Siewamat 3573 mit einem Fassungsvermögen von 5,5 kg Wäsche und ca. 60 1 Wasser gegeben. Die Jeans wurden mit einem konventionellen, amylasehaltigen Vollwaschmittel einmal bei 40°C vorgewaschen. Anschließend wurden über den Waschmittelzulauf 50 g einer Zubereitung bestehend aus
    15 Gew.-% Celluzyme,
    15 Gew.-% Talgfettalkohol+50 EO und
    70 Gew.-% Natriumcitrat/Citronensäure (1:1) zugegeben. Dabei wurde die Staubentwicklung beim Einfüllen mit "staubfrei" (+) oder "nicht staubfrei" (-) beurteilt. Die Flotte wurde 60 min bei 55°C behandelt und anschließend zweimal klargespült. Der "stonewash"-Effekt und der Weichgriff wurden subjektiv von einem Panel bestehend aus 6 geschulten Personen auf einer Skala von 1 (sehr deutlich bzw. sehr weich) bis 6 (kaum feststellbar bzw. hart) beurteilt. Das Ergebnis ist in Tabelle 1 zusammengefaßt.
    Example 1. A pair of brand-new blue jeans were placed in a Siemens Siewamat 3573 washing machine with a capacity of 5.5 kg of laundry and about 60 l of water. The jeans were prewashed once at 40 ° C with a conventional detergent containing amylase. 50 g of a preparation consisting of:
    15% by weight of Celluzyme,
    15% by weight tallow fatty alcohol + 50 EO and
    70% by weight sodium citrate / citric acid (1: 1) added. The dust development during filling was assessed as "dust-free" (+) or "not dust-free" (-). The liquor was treated at 55 ° C. for 60 min and then rinsed clear twice. The "stonewash" effect and the soft feel were assessed subjectively by a panel consisting of 6 trained people on a scale from 1 (very clear or very soft) to 6 (hardly noticeable or hard). The result is summarized in Table 1.

    Vergleichsbeispiel V1. Beispiel 1 wurde wiederholt, jedoch anstelle des Talgfettalkohol+50 EO ein Talgfettalkohol+20EO eingesetzt und die Behandlung über einen Zeitraum von 60 min bei einer Temperatur von 55°C durchgeführt. Die Ergebnisse sind in Tabelle 1 zusammengefaßt. Comparative Example V1. Example 1 was repeated, but instead of the tallow fatty alcohol + 50 EO a tallow fatty alcohol + 20EO was used and the treatment was carried out over a period of 60 min at a temperature of 55 ° C. The results are summarized in Table 1.

    Vergleichsbeispiel V2. Vergleichsbeispiel V1 wurde wiederholt, die Behandlung jedoch nicht über einen Zeitraum von 60, sondern von 90 min durchgeführt. Die Ergebnisse sind in Tabelle 1 zusammengefaßt. Comparative example V2. Comparative example V1 was repeated, but the treatment was carried out over a period of 90 minutes, not over a period of 60 minutes. The results are summarized in Table 1.

    Vergleichsbeispiel V3. Vergleichsbeispiel V2 wurde wiederholt, die Behandlung jedoch nicht bei einer Temperatur von 55, sondern 40°C durchgeführt. Die Ergebnisse sind in Tabelle 1 zusammengefaßt

    Figure 00060001
    Comparative Example V3. Comparative example V2 was repeated, but the treatment was carried out not at a temperature of 55, but 40 ° C. The results are summarized in Table 1
    Figure 00060001

    Das Beispiel und die Vergleichsbeispiele zeigen, daß nur bei Einsatz der erfindungsgemäßen Zubereitungen gefärbte Baumwollgewebe erhalten werden, die sich sowohl durch einen optimalen "stonewash"-Effekt als auch durch einen angenehmen Weichgriff auszeichnen. Im Gegensatz zu den Produkten des Stands der Technik sind die erfindungsgemäßen Zubereitungen beim Umfüllen praktisch staubfrei.The example and the comparative examples show that only when the preparations according to the invention are used dyed cotton fabrics are obtained, which are characterized both by an optimal "stonewash" effect as well as a pleasant soft feel. In contrast to the products In the prior art, the preparations according to the invention are practical when decanting dust free.

    Claims (10)

    1. Solid water-free preparations consisting of
      (a) 5 to 50% by weight of acidic cellulases,
      (b) 10 to 20% by weight of fatty alcohol polyglycol ethers corresponding to formula (I): R1O(CH2CH2O)nH    in which R1 is a linear alkyl group containing 16 to 22 carbon atoms and n is a number of 40 to 100, and
      (c) to 100% by weight citric acid, inorganic and/or organic salts.
    2. A process for the production of "stonewash" effect cotton fabric in which an aqueous liquor containing dyed cotton fabric is treated with a solid water-free preparation consisting of
      (a) 5 to 50% by weight of acidic cellulases,
      (b) 10 to 20% by weight of fatty alcohol polyglycol ethers corresponding to formula (I): R1O(CH2CH2O)nH    in which R1 is a linear alkyl group containing 16 to 22 carbon atoms and n is a number of 40 to 100, and
      (c) to 100% by weight citric acid, inorganic and/or organic salts.
    3. A process as claimed in claim 2, characterized in that acidic cellulases with optimum activity at a pH value of 4.5 to 5 are used.
    4. A process as claimed in claim(s) 2 and/or 3, characterized in that fatty alcohol polyglycol ethers corresponding to formula (I), in which R1 is a linear alkyl group containing 16 to 22 carbon atoms and n is a number of 50 to 80, are used.
    5. A process as claimed in at least one of claims 2 to 4, characterized in that buffer salts selected from the group consisting of alkali metal and/or alkaline earth metal sulfates, phosphates and citrates are used.
    6. A process as claimed in at least one of claims 2 to 5, characterized in that the water-free preparations are used in quantities of 0.1 to 10% by weight, based on the cotton fabric.
    7. A process as claimed in at least one of claims 2 to 6, characterized in that the fabric is treated with a liquor ratio by weight of cotton fabric to water of 1:10 to 1:100.
    8. A process as claimed in at least one of claims 2 to 7, characterized in that the treatment of the fabric is carried out at a pH value of 4.5 to 5.5.
    9. A process as claimed in at least one of claims 2 to 8, characterized in that the treatment of the fabric is carried out at a temperature of 50 to 65°C.
    10. The use of the solid preparations claimed in claim 1 as a means of obtaining a "stonewash" effect on dyed cotton fabric.
    EP97903271A 1996-02-22 1997-02-13 Solid, waterless preparations Expired - Lifetime EP0877788B1 (en)

    Applications Claiming Priority (3)

    Application Number Priority Date Filing Date Title
    DE1996106619 DE19606619A1 (en) 1996-02-22 1996-02-22 Solid, practically water-free preparations
    DE19606619 1996-02-22
    PCT/EP1997/000668 WO1997031089A1 (en) 1996-02-22 1997-02-13 Solid, virtually waterless preparatios

    Publications (2)

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    EP0877788A1 EP0877788A1 (en) 1998-11-18
    EP0877788B1 true EP0877788B1 (en) 2000-05-24

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    ES2217918B1 (en) * 2001-06-21 2005-11-01 Cognis Iberia S.L. FINISHED PRODUCTS FOR TEXTILE TREATMENT.
    DE10358097A1 (en) 2003-12-10 2005-07-14 Sasol Germany Gmbh A method for preventing or minimizing color edging using polyesters
    DE102015201702A1 (en) 2015-01-30 2016-08-04 Henkel Ag & Co. Kgaa Acid liquid compact detergent containing hydroxycarboxylic acid, nonionic surfactant and enzyme
    CN112048400B (en) * 2020-07-30 2021-08-24 宁波职业技术学院 Acidic cellulase complex and preparation method thereof

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    DE3166233D1 (en) * 1980-02-05 1984-10-31 Procter & Gamble Liquid detergent composition
    US4832864A (en) * 1987-09-15 1989-05-23 Ecolab Inc. Compositions and methods that introduce variations in color density into cellulosic fabrics, particularly indigo dyed denim
    FR2641555B1 (en) * 1989-01-09 1992-03-27 Cayla PROCESS FOR HETEROGENEOUS WASHING OF DYED COTTON-BASED ARTICLES USING CELLULASES IN AN AQUEOUS MEDIUM
    DK145090D0 (en) * 1990-06-14 1990-06-14 Novo Nordisk As CELLULASE PREPARATIONS AND APPLICATIONS THEREOF
    DE4407801A1 (en) * 1993-03-15 1994-09-22 Sandoz Ag Treatment of textiles
    CA2104921C (en) * 1993-06-09 2003-12-30 Paul Stoner Sr. Methods and compositions for treating denim fabric and the fabric produced thereby
    IL113714A0 (en) * 1994-06-22 1995-08-31 Ivax Ind Inc Method of treating dyed cellulosic fabric

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    EP0877788A1 (en) 1998-11-18
    WO1997031089A1 (en) 1997-08-28
    DE19606619A1 (en) 1997-08-28

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