EP2000583A1 - Procédé de traitement de textile contenant de la cellulose - Google Patents

Procédé de traitement de textile contenant de la cellulose Download PDF

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Publication number
EP2000583A1
EP2000583A1 EP08009672A EP08009672A EP2000583A1 EP 2000583 A1 EP2000583 A1 EP 2000583A1 EP 08009672 A EP08009672 A EP 08009672A EP 08009672 A EP08009672 A EP 08009672A EP 2000583 A1 EP2000583 A1 EP 2000583A1
Authority
EP
European Patent Office
Prior art keywords
textile
treatment
alkaline
solution
alkaline substance
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
EP08009672A
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German (de)
English (en)
Other versions
EP2000583B1 (fr
Inventor
Christian Schimper
Constanta Ibanescu
Thomas Bechtold
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Universität Innsbruck
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Universität Innsbruck
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Publication of EP2000583A1 publication Critical patent/EP2000583A1/fr
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Publication of EP2000583B1 publication Critical patent/EP2000583B1/fr
Not-in-force legal-status Critical Current
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    • 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
    • D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
    • D06M23/16—Processes for the non-uniform application of treating agents, e.g. one-sided treatment; Differential treatment
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/38—Products with no well-defined composition, e.g. natural products
    • C11D3/386—Preparations containing enzymes, e.g. protease or amylase
    • C11D3/38645—Preparations containing enzymes, e.g. protease or amylase containing cellulase
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/02—Inorganic compounds
    • C11D7/04—Water-soluble compounds
    • C11D7/06—Hydroxides
    • 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
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • 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
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
    • 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
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
    • 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
    • D06M13/10—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 oxygen
    • D06M13/144—Alcohols; Metal alcoholates
    • D06M13/148—Polyalcohols, e.g. glycerol or glucose
    • 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
    • D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • D06M16/003—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic with enzymes or microorganisms
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
    • C11D2111/10—Objects to be cleaned
    • C11D2111/12—Soft surfaces, e.g. textile
    • 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

Definitions

  • the invention relates to a process for the enzymatic treatment of cellulose-containing textile by means of a solution comprising at least one kind of cellulase.
  • cellulose-splitting enzymes have become very important in the textile-chemical treatment of cellulose fiber-containing materials.
  • the technically most commonly used "total crude” cellulases are a mixture of microbiologically produced erido-, exocellullases and cellobiohydrolases.
  • the object of the cellulases is the hydrolytic degradation of the cellulose by selective cleavage of the ⁇ -1,4-glycosidic bond, whereby soluble fragments are removed from the polymers and taken up by the treatment solution, where a further hydrolysis to glucose takes place.
  • Object of the present invention is therefore to provide a method of the type mentioned, in which the textile loses imperceptible to mechanical resistance.
  • Such a method of the type mentioned is characterized in that prior to treatment with the cellulase-containing solution, an alkaline substance, preferably an alkaline solution, is applied only in regions on the textile.
  • a textile comprises both textile fibers, semi-finished and finished textile products such as yarn or textile fabrics and textile finished goods such as textile clothing etc. It is essential to the invention that the textile comprises cellulose (eg blended fabric) - but the textile does not have to consist of it.
  • the textile for example the textile fiber
  • the textile fiber is pretreated on the surface with an alkaline substance such that the alkaline substance penetrates only slightly into the textile or the textile fiber.
  • the alkaline substance preferably alkaline solution
  • the alkaline substance is applied to the surface of the textile fiber or textile such that it remains substantially on the surface of the textile.
  • substantially remaining on the surface of the textile fiber is meant that the alkaline substance can not penetrate to the core of the textile fiber or the textile, but under 20 to 30% of the thickness of the textile fiber, preferably less than 10% of the thickness of the textile fiber in the textile fiber penetrates.
  • the alkaline substance is applied by spraying and / or patting and / or doctoring and / or printing.
  • the textile fiber or the flat textile obtained from a textile fiber is provided with patterns which, on the one hand, can have a different color ("stone-wash effect"), on the other hand a more pleasant or altered feel.
  • the textile fibers are present in a flat textile, preferably textile fabric, it is possible to apply individual patterns to the textile which can be predetermined, in particular by printing a predefinable printing pattern.
  • the alkaline substance is applied at least partially on one side of the flat textile.
  • a different treatment of the two sides of the textile fabric is of interest in order to achieve advantages in terms of functional properties (water transport, absorbency, smoothness, etc.).
  • the invention is based on the fact that in the areas where an alkaline substance has been applied, an increased rate of degradation can be achieved, since the cellulase has a higher reaction rate at these points. It is favorable if the alkaline substance comprises an aqueous solution of at least one metal hydroxide, preferably an alkaline earth metal hydroxide and / or alkali metal hydroxide, wherein it is preferably provided that the metal hydroxide is NaOH.
  • the rate of reaction of the fiber-enzyme reaction depends on the fiber type presented (cotton, viscose fibers, lyocell fibers, etc.) as well as the concentration and activity of the enzymes used. Depending on the processing stage in the textile finishing process, the fiber changes in its reactivity. For example, it is known in the prior art that cotton textiles after treatment in concentrated caustic soda show an increased degradation rate by cellulases, which is mainly due to reduced crystallinity and increased accessibility of the fiber.
  • the alkaline solution has a thickening agent.
  • the alkaline substance is a humectant wherein it is particularly preferred that the humectant comprises glycerin.
  • Alkaline treatment solutions known in the art may contain alkali ions (Li, Na, K ions), as well as, for example, alkaline earth hydroxides and quaternary ammonium hydroxides.
  • the treatment in Nahsmlttelsystemen (alcoholic solutions of Banlmittein) has been described in the prior art.
  • the present invention is therefore based on the idea to make the activation of the fiber only localized and thus to limit the rate of hydrolytic degradation of the cellulase on certain areas of the textile structure.
  • the application of the activating alkali solution can be carried out by spraying, paddling, knife coating, and minimal application techniques on one or both sides of the product by the usual methods, in a particularly advantageous embodiment, printing techniques (stencil printing, foam printing) are mentioned.
  • printing techniques stencil printing, foam printing
  • Alkali solutions may be alkali hydroxides, alkaline earth hydroxides, quaternary ammonium bases as well as amines or other basic compounds known to those of ordinary skill in the art.
  • concentrations of the application solutions are in the range of 0.5 to 10 mol / l of alkali solution, the concentration due to the desired activation effect, the textile substrate to be treated and optionally provided intermediate drying is determined.
  • intermediate drying a concentration of the non-volatile alkali takes place on the surface; so that higher concentrations are achieved here compared to the applied application solution.
  • concentration range for a desired result will be easy to determine with knowledge of the invention, even for the average expert by series experiments.
  • the applied solution beforehand admixed with humectants such as glycerin to prevent complete drying and hardening.
  • Textile structures can be, for example, woven fabrics, knitted fabrics, nonwovens, films, etc., with no restrictions with regard to the material form to be treated.
  • Cellulosic substrates may preferably consist of cotton, bast fibers, viscose, modal, lyocell fibers or mixtures thereof with other fibers of cellulose or other fibrous materials, in particular synthetic materials.
  • dyed textiles of cotton or other cellulosic fibers, or their blends are treated with synthetic fibers (such as Lycra, polyester fibers, polyamide), in a particularly preferred embodiment, indigo dyed denim webs of cellulosic fibers are treated.
  • Suitable cellulase treatment methods may be selected from the methods proposed in the prior art.
  • indigo ring-dyed denim fabric is activated, which has the advantage which provides faster detachment of the indigo dye from the tissue surface.
  • a drying step takes place, preferably by heating the textile.
  • the textile is at least partially dyed, preferably indigo-dyed, wherein it is particularly preferred that the textile comprises textile fibers which are woven into a fabric, preferably denim fabric, or the alkaline substance in ready-made textiles before a washing treatment.
  • woven textile fibers woven into a textile fabric in the form of a textile fabric 1 are shown schematically.
  • On the textile fabric 1 is partially applied to the checkered areas 2 an alkaline substance.
  • the white areas 3 are untreated.
  • the alkaline paste was washed with water, rinsed three times with cold water and neutralized at 40 ° C with 1% acetic acid.
  • the enzyme treatment was then carried out in a laboratory dyeing plant (Pretema Multicolor laboratory dyeing unit type MC 360, Caromatic, Switzerland), a "total crude cellulose” Genencor, USA, was used with a concentration of 3.0 IU / mg tissue (30 mUL treatment bath).
  • the solution was adjusted to pH 4.8 by a 50 mM acetate buffer.
  • the liquor ratio was 1 g of tissue: 25 ml of treatment bath.
  • Treatment of material I was 1.5 hours, material II, 0.75 hours at a temperature of 55 ° C.
  • the enzymatic hydrolysis was stopped by raising the temperature to 75 ° C. and raising the pH to 10 and treating for 10 minutes.
  • the samples were rinsed and air dried.
  • Table 1 compares the results of the untreated and activated tissues. The increased brightness due to the increased degradation on the surface of the materials is clearly visible. The total color difference ⁇ E is also calculated and shown. The ⁇ E values above 6 clearly show the increased color loss on the alkaline pretreated areas.
  • Example 2 shows the increase in the rate of degradation by alkaline pretreatment using the example of regenerated fibers
  • Viscose fabric (staple fiber yarn 38 mm, 1.3 dtex) was used as a substrate. Plain weave warp 20 tex, weft, 24 tex, twist 19 rounds / inch, 143 g / m 2 , 37/29 fd / cm was used.
  • the treatment solution was prepared by diluting a 50% (w / w) sodium hydroxide solution with water (1.04, 2.20, 3.48 and 4.91 mol / L NaOH).
  • the fabric was pretensioned in different alkali solutions for 1 minute at a liquor ratio of 1: 3.
  • the concentration of the treatment solutions is given in Table 2.
  • the enzyme treatment was then carried out in a laboratory dyeing plant (Pretema Multicolor laboratory dyeing unit type MC 360, Caromatic, Switzerland).
  • a "total crude cellulose” Genencor, USA was used at a concentration of 3.5 IU / mg tissue (30 mg protein per mL).
  • the solution was buffered through a 50 mM acetate adjusted to pH 4.8.
  • the liquor ratio was 1 g tissue 25 ml treatment bath.
  • the hydrolysis was carried out at 55 ° C (+/- 1 ° C). After 1 hour of treatment, the weight loss was evaluated by measuring the concentration of glucose formed in the solution. Comparative measurements were performed with non-pretreated materials.
  • Table 2 shows the altered degradation measured as the concentration of glucose formed per L treatment bath after one hour.
  • Table 2 Glucose concentration in solution on enzymatic hydrolysis of viscose with and without alkaline activation glucose concentration fabric pattern [G / L] Untreated control 1.81 Activation with 1.04 mol / L NaOH, 60 sec 2.50 Activation with 2.20 mol / L NaOH, 60 sec 7.15 Activation with 3.48 mol / L NaOH, 60 sec 11.29
  • Fabrics made from other regenerated cellulose fibers can be treated in the same way.
  • Table 3 shows the increase in degradation rate measured after 1 hour of hydrolysis time.
  • Table 3. Degradation measured as g / L glucose and activation Concentration in g / L glucose Treatment in comparison sample 3.48 mol / L NaOH % Activation viscose 1.81 11.28 625 Modal 0.65 6.45 992 lyocell 0.47 3.95 848 Lyocell networked 0.33 5.26 1594
  • the degradation rate is increased by a factor of 6 - 15.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Microbiology (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Biochemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Coloring (AREA)
EP08009672A 2007-06-05 2008-05-28 Procédé de traitement de textile contenant de la cellulose Not-in-force EP2000583B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
AT0088407A AT505369A1 (de) 2007-06-05 2007-06-05 Verfahren zur behandlung von cellulosehältigem textil

Publications (2)

Publication Number Publication Date
EP2000583A1 true EP2000583A1 (fr) 2008-12-10
EP2000583B1 EP2000583B1 (fr) 2011-07-20

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EP08009672A Not-in-force EP2000583B1 (fr) 2007-06-05 2008-05-28 Procédé de traitement de textile contenant de la cellulose

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AT (2) AT505369A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2278063A1 (fr) 2009-07-24 2011-01-26 Universität Innsbruck Procédé de traitement enzymatique de textiles contenant de la cellulose

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5122159A (en) * 1988-09-15 1992-06-16 Ecolab Inc. Cellulase compositions and methods that introduce variations in color density into cellulosic fabrics, particularly indigo dyed denim
US5232851A (en) * 1990-10-16 1993-08-03 Springs Industries, Inc. Methods for treating non-dyed and non-finished cotton woven fabric with cellulase to improve appearance and feel characteristics
EP0636740A1 (fr) * 1993-02-18 1995-02-01 Meiji Seika Kabushiki Kaisha Preparation de cellulase et son utilisation pour le traitement des fibres de cellulose
US20020115193A1 (en) * 1996-03-06 2002-08-22 Hsieh You-Lo Enzyme treatment to enhance wettability and absorbancy of textiles
US20060225224A1 (en) * 2005-04-08 2006-10-12 Taylor Lawnie H Formation of patterns of fades on fabrics

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5122159A (en) * 1988-09-15 1992-06-16 Ecolab Inc. Cellulase compositions and methods that introduce variations in color density into cellulosic fabrics, particularly indigo dyed denim
US5232851A (en) * 1990-10-16 1993-08-03 Springs Industries, Inc. Methods for treating non-dyed and non-finished cotton woven fabric with cellulase to improve appearance and feel characteristics
EP0636740A1 (fr) * 1993-02-18 1995-02-01 Meiji Seika Kabushiki Kaisha Preparation de cellulase et son utilisation pour le traitement des fibres de cellulose
US20020115193A1 (en) * 1996-03-06 2002-08-22 Hsieh You-Lo Enzyme treatment to enhance wettability and absorbancy of textiles
US20060225224A1 (en) * 2005-04-08 2006-10-12 Taylor Lawnie H Formation of patterns of fades on fabrics

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2278063A1 (fr) 2009-07-24 2011-01-26 Universität Innsbruck Procédé de traitement enzymatique de textiles contenant de la cellulose
WO2011009803A2 (fr) 2009-07-24 2011-01-27 Universitaet Innsbruck Procédé de traitement enzymatique de textiles contenant de la cellulose
WO2011009803A3 (fr) * 2009-07-24 2011-04-21 Universitaet Innsbruck Procédé de traitement enzymatique de textiles contenant de la cellulose
US20120180229A1 (en) * 2009-07-24 2012-07-19 Universitaet Innsbruck Method for enzymatic treatment of cellulose-containing textiles by means of a solution that comprises at least one cellulase type

Also Published As

Publication number Publication date
ATE517208T1 (de) 2011-08-15
AT505369A1 (de) 2008-12-15
EP2000583B1 (fr) 2011-07-20

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