GB2483886A - Treating wool with animal fibre derived polypeptide extract, to impart shrink resistance - Google Patents

Treating wool with animal fibre derived polypeptide extract, to impart shrink resistance Download PDF

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GB2483886A
GB2483886A GB1015962.2A GB201015962A GB2483886A GB 2483886 A GB2483886 A GB 2483886A GB 201015962 A GB201015962 A GB 201015962A GB 2483886 A GB2483886 A GB 2483886A
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wool
treated
treatment
polypeptide extract
protease
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Shen Jinsong
Edward J Smith
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De Montfort University
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De Montfort University
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/51Treating 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 sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/54Treating 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 sulfur, selenium, tellurium, polonium or compounds thereof with sulfur dioxide; with sulfurous acid or its salts
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/73Treating 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 carbon or compounds thereof
    • D06M11/76Treating 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 carbon or compounds thereof with carbon oxides or carbonates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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
    • D06M13/11Compounds containing epoxy groups or precursors thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/192Polycarboxylic acids; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/207Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating 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
    • D06M13/325Amines
    • D06M13/328Amines the amino group being bound to an acyclic or cycloaliphatic carbon atom
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating 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
    • D06M13/402Amides imides, sulfamic acids
    • D06M13/432Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/15Proteins or derivatives thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/263Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/55Epoxy resins
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • D06M16/003Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic with enzymes or microorganisms
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/10Animal fibres
    • D06M2101/12Keratin fibres or silk
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/45Shrinking resistance, anti-felting properties

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Microbiology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

A polypeptide extract is obtained by treating animal fibre with a protease and a reducing agent. The polypeptide extract is applied to wool, which has preferably been scoured with an alkali carbonate. Preferably the animal fibre is wool, the reducing agent is sodium sulphite or sodium hydrosulphite, the enzyme is serine-type protease. The polypeptide is preferably denatured. Preferably the treated wool is cross-linked with glycerol diglycidyl ether, 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride or 1,4-butandiol diglycidyl ether. The treated wool can be used in machine washable, woven or knitted garments.

Description

TITLE
Wool Treatment
DESCRIPTION
The invention relates to the treatment of wool to impart shrink resistance thereto.
Wool fabric, whether knitted or woven, will naturally shrink and felt when washed.
Consumers, however, demand that woollen garments should be machine washable and have a soft handle. To be commercially useful, the wool must be treated so that it becomes shrink resistant. The commonly used treatment is the Chlorine-Hercosett process in which chlorination of the wool is followed by polymer deposition upon it, but this has major drawbacks. The contamination of waste water with absorbable organic chlorides is damaging to the environment and the deposition of polymer on the wool fibre may give it a harsh handle. Recent European Union legislation has imposed restrictions on absorbable organic chlorides in effluent. If the chlorination is omitted to avoid the effluent problem, increased polymer deposition then becomes necessary and the resulting product feels more like a synthetic fabric and less like wool. A more environmentally friendly process is required.
The invention provides a method for the treatment of wool to impart shrink resistance thereto, the method comprising (a) obtaining a polypeptide extract by treating animal fibre with a protease and a reducing agent, and (b) applying the polypeptide extract to the wool to be treated.
The animal fibre used in step (a) is preferably wool fibre. For reasons of economy, the fibre used in step (a), whether wool or of non-sheep origin, is preferably a low grade or waste fibre, waste wool or other waste protein fibres. Loose stock or top is suitable.
Suitable proteases for use in the invention are those classified as a serine endopeptidases with the corresponding Enzyme Commission number EC 3.4.21.X (such as trypsin and subtilisin); cystaine endopeptidases EC 3.4.22.X (such as papain); Aspartic endopeptidases EC 3.4.23.X (such as pepsin) and Metalloendopeptidases EC 3.4.24.X (such as thermolysin).
Those most preferred are commercial proteases (serine-type proteases) with the corresponding Enzyme Commission number EC 3.4.21.62, such as Esperase 8.OL (Novozymes), Savinase 1 6L Type EX (Novozymes), Protex Multiplus L (Genencor), Protex Gentle L (Genencor) and modified protease (proteases enlarged in size by covalent bonding to polymers), see Smith E et al, Enzyme and Microbial Technology, 47, 105-111(2010), Covalent bonding of protease to different sized enteric polymers and their potential use in Suitable reducing agents include sulphur-based reducing agents such as alkali metal and ammonium sulphites; alkali metal bisulphites, metabisulphites, thiosuiphites, sulphates, hydrosulphites or sulphides, and sodium or zinc formaldehyde suiphoxylate. The preferred reducing agents are those customarily used in textile treatment, such as sodium sulphite (Na2SO3) and sodium hydrosulphite (sodium dithionite Na2S2O4).
In a preferred procedure, the clean wool fibre is agitated in a buffer with from 3 to 24 g/L of the reducing agent for up to 2'/2 hours, preferably 15 to 60 minutes, at up to 65°C. The protease is then added, suitably in an amount of from 9 to 36 activity units per gram of wool fibre, and stirring is continued at the same temperature for from I to 24 hours, but preferably about 2 hours. The mixture may be centrifuged and the supernatant liquid layer is taken for the next step.
Before centrifuging, it is possible to denature the protease by raising the temperature, for example to 80 to 85°C. Alternatively, this step may be omitted and the polypeptide extract containing active enzyme is then used in step (b).
The wool which is to be treated with the polypeptide extract in step (b) may be a knitted wool fabric or a woven wool fabric. Alternatively wool yarn may be treated for subsequent knitting or weaving, or wool fibre may be treated for subsequent spinning and knitting or weaving.
Whatever the form of the wool used, it may be pre-treated with an alkali scour solution, suitably at pH range of 9 -11. This preferably comprises an alkali metal carbonate, such as sodium carbonate which can be used in combination with surfactants, preferably a non-ionic surfactant (ethoxylated fatty alcohol). The pre-treatment may be with dilute solutions of alkali metal carbonate and surfactant, e.g. less than 1% w/v, for up to an hour at up to 60°C.
A liquor to goods ratio of 50:1 may be suitable.
The polypeptide extract is then applied to the wool which is to be treated. The polypeptide extract can be used neat or can be diluted up to 50%. The treatment, under light agitation at up to 60°C, may be for 15 minutes up to 4 hours. Shorter treatment times, e.g. 30 minutes, are suitable when the enzyme remains activated or when fresh protease is added to the polypeptide extract before application to the wool to be treated. When the protease has been denatured, and fresh protease is not added, times of 2 hours or more are preferred. A liquor to goods ratio of from 12:1 to 24:1 is suitable.
The treated wool is desirably further treated, for up to 1 hour at up to 60°C, with a crosslinking agent, such as glycerol diglycidyl ether, 1-(3-dimethylamino-propyl)3-ethyl.-carbodiimide hydrochloride or 1, 4-butandioldiglycidyl ether. A preferred concentration of crosslinking agent is from 5 to 20 WL and a liquor to goods ratio of from 12:1 to 24:1 is
suitable.
Cross-linking agents can be diepoxide and other polyepoxides including glycerol diglycidyl ether or 1,4-butandioldiglycidyl ether; carbodiimides such as 1-(3-dimethylamino-propyl) 3-ethyl-carbodiimide hydrochloride; polycarboxylic acids such as citric acid, polyacrylic acid or 1,2,3,4-butanetetracarboxylic acid; or protein crosslinking enzymes such as transglutaminase.
The treated wool may then be dried, and the crosslinking agent may be cured in an oven.
Curing could also be done alternatively be effected using a hot air baking unit (stenter), a high temperature steamer or infTra-red radiation.
In addition to imparting shrink resistance to wool, the method of the invention may also impart improved whiteness and soft handle to the wool.
The following examples illustrate the invention.
Example 1
Shrink-resist treatment with polypeptides extracted from wool Preparation of wool polypeptide extract Clean wool fibre either loose stock or top was cut into snippets and placed in a 0.02M phosphate buffer (made from 0.02M Na2FIPO4 and adjusted to p1-I 8 with 0.02M NaH2PO4) containing 12g1'L of the reducing agent sodium sulphite and treated at 60°C for 30 minutes with an agitation of 40rpm. The liquor to goods ratio was 20:1. 0.15% v/v (18 activity units of enzyme per gram of wool fibre) of the alkaline protease Esperase 8.OL (Novozyme) was added to the mixture and mixed for a further 2 hours at 65°C with an agitation of 40rpm. The temperature was then raised to 80-85°C for 10 minutes to denature the enzyme; agitation was maintained at 40 rpm. The resulting suspension was separated by centrifugation (swing-out rotor) at 4500 rpm for 5 minutes. The supernatant liquid layer was collected for use in the treatment of wool.
Pre-treatment of wool fabric (alkali scour) Fine rib 1:1 knitted wool fabric with a fibre diameter of 21.3gm was pre-treated in an alkali scour solution containing 2g/L non-ionic surfactant (Ultravon PL (Ciba)) and 1.6 g/L sodium carbonate at a liquor to goods ratio of 50:1 for 30 minutes at 60°C with up to 5 rpm agitation.
The fabric was then rinsed in deionised water with a liquor to goods ratio of 50:1 for 10 minutes at 60°C with up to 5rpm agitation. After treatment, the wool sample was washed thoroughly with water, hydro-extracted at 2800rpm and then left to air-dry.
Shrink-resist treatment of wool fabric The alkali scoured fabric was then treated in the neat supernatant wool extract at a liquor to goods ratio of 12:1 for 2 hours at 60°C with up to 5 rpm agitation. The fabric was then transferred into a new bath of 0.02M phosphate buffer (made from 0.02M Na2HPO4 and adjusted to pH 7.2 to 7,3 with 0.02M NaH2PO4) containing lOg/L of the cross-linking agent glycerol diglycidyl ether (ODE) with a liquor to goods ratio of 12:1 for 30 minutes at 60°C with up to 5 rpm agitation. The fabric was then hydro-extracted at 2800rpm to remove excess wetness then cured at 140°C for 10 minutes in a fan assisted oven.
Testing of treated wool samples Wool samples treated as described above were conditioned for 24 hours at 20°C +/-2°C and 65% +/-2% relative humidity and then tested using the following methods.
Weight loss. The weight loss of the wool fabric after enzyme treatment was expressed as a percentage WL and was calculated using the following equation: %WL 100(Wi-W2)/W1 where WI is the weight of conditioned wool fabric prior to enzymatic treatment and W2 is the weight of conditioned wool fabric after enzymatic treatment.
Bursting strength. The strength of the knitted wool fabric after enzyme treatment was measured using bursting strength. A Heals TruBurst 610 Bursting Strength Tester was used according to ISO 13938-2:1999. A test area of 10 cm2 (35.7 mm diameter) was used and the pressure rate was set at 21 kPa The mean bursting pressure and mean height (distension) at burst were recorded.
Whiteness. A Datacolor SF600 Plus CT reflectance spectrophotometer was used to determine the whiteness of the treated woollen fabric in terms of the CIE whiteness index. Each sample was folded into four and measured four times. All values were measured and calculated using ColorTools QC software with illuminantlobscrver conditions of D65 10°. The higher the CIE whiteness index value, the greater the whiteness of the fabric sample.
Shrinkage. The measurement of shrinkage due to washing of the enzyme treated knitted woollen fabric was tested according to Woolmark Test Method TM3 1: Washing of Wool Textile Products. The samples were subjected to a 7A wash cycle (a gentle wash cycle performed at 40°C) for relaxation shrinkage and 5A wash cycles (performed at 40°C -a single 5A wash cycle is equivalent to 10 domestic wash cycles) up to 3 times for felting shrinkage using a programmable test washing machine (Electrolux Wascator FOM 71 or Miele Novotronic W980 computer controlled washing machine). Between each washing cycle the samples were flat -dried in a 50°C oven for 4 hours then conditioned at 20°C and 65% relative humidity then weighed so weight loss due to washing could be determined. The weight loss of the wool fabric after enzyme treatment was expressed as a percentage, WLW and was calculated using the following equation: %WLW 100 (W3-W4)/ W3 where W3 is the weight of conditioned treated wool fabric before being subjected to the series of washing cycles and W4 is the weight of conditioned treated wool fabric after machine washing.
The mean length, width and area shrinkage and weight loss due to washing was calculated.
Results After 3x5A washes Fabric samples/treatment method Weight Burst CIE ___________________ Area Weight Loss strength whiteness Shrinkage Loss Pre-treatment Shrink-resist treatment (%) (kPa) mdex (%) (/o) Untreated Untreated ---397 --4.11 18.6 1.0 No further treatment ---389 -2.06 14.8 0.1 2hr treatment with extracted wool -0.2 374 12.81 5.6 0.9 Pre-treated polypeptide (deactivated) 2hr treatment with extracted with non-ionic wool polypeptide (deactivated) -0.4 350 8.49 3.8 0.1 surfactant followed by GDE 30mm +Na2CO3 2hr treatment with extracted wool for 30mm polypeptide (deactivated) followed 0.6 339 5.36 3.6 -0.2 by ODE 30mm and 140°C cure 10mm Scanning electron microscopy (SEM) To determine the extent of fibre damage and any changes to the external surface of the fibre, micrographs were taken using SEM of a wool sample treated according to this Example. A comparative micrograph of a wool sample that had only been alkali-scoured was also taken.
The samples were prepared by laying out the wool fibre across suitable aluminium stubs and held firmly in place with aluminium conducting tape across the wool fibre ends. For examination, the samples were sputter coated with gold! palladium under argon for 60 seconds using an Edwards ES 150 sputter coater. Samples were examined using a Leo 430 scanning electron microscope operating with a working distance of 25 mm, an accelerating voltage of 7 kV and a magnification of 500x. The micrographs are shown in Figure 1 and show that the fibres of the treated sample are intact and are not severely damaged by the shrink-resist treatment.
Example 2
Shrink-resist treatment with enzyme active extracted wool polypcptides Preparation of wool polypeptide extract The wool polypeptide extract was prepared as described in Example 1, except that the step of raising the temperature to 80-85°C for 10 minutes was omitted and as a result the enzyme was not denatured.
Pre-treatinent of wool fabric (alkali scour) The wool fabric was pre-treated as described in Example 1.
Shrink-resist treatment of wool fabric The alkali scoured fabric was treated as described in Example 1, except that the enzyme active wool polypeptide extract prepared in this Example was used in place of the enzyme denatured wool polypeptide extract prepared in Example 1 and that the treatment was canied out for 30 minutes rather than 2 hours.
Testing of treated wool samples Testing was carried out as described in Example 1.
Results After 3x5A After 5x5A Fabric samples/treatment method Weight Burst CLE washes washes Loss Strength whiteness -Area Weight Area -Weight (%) (kPa) index Shrinkage Loss Shrinkage Loss Pre-treatment Shrink-resist treatment (%) (%) (%) (%) untreated untreated ---397 -4.11 -18.6 -1.0 25.1 0.3 Nofurthertreatment ---389 -2.06 14.8 0.1 mm treatment with extracted wool polypeptide 4.3 316 11.26 4.0 8.3 (enzyme active) Pre-treated 30 mm treatment with --with nonionic extracted wool polypeptide 7.5 253 12.85 1.8 3.2 surfactarit + (enzyme active) followed by Na2CO3 ODE 30mm For30min 3omintreatmentwith -extracted wool polypeptide (enzyme active) followed by 5.7 305 14.85 1.1 1.1 1.0 1.6 ODE 30mm and 140°C cure 10mm Scanning electron microscopy (SEM) A micrograph of a wool sample treated according to this Example was taken, using the procedure described in Example 1, and is shown in Figure 1. It shows that the fibres of the treated sample of this Example are intact and are not severely damaged by the treatment.
Photographic Comparison Untreated knitted wool samples and knitted wool Samples treated according to this Example were photographed before washing, after washing for lx 7A and 3x SA wash cycles, and after washing for lx 7A and 5x 5A wash cycles. The photographs are shown in Figure 2. It is very clear that the washed samples that had been treated have withstood the rigours of washing to a much greater extent than the samples that had not been treated.
Example 3
Shrink-resist treatment with extracted wool polypetides in the presence of protease Preparation of wool polypeptide extract The wool polypeptide extract was prepared as described in Example 1.
Pre-treatment of wool fabric (alkali scour) The wool fabric was pre-treated as described in Example 1.
Shrink-resist treatment of wool fabric The alkali scoured fabric was treated as described in Example 1, except that protease (preferably native Esperase) was added to the neat supernatant wool extract immediately before wool fabric treatment. Different quantities of native Esperase were added (0.2lmL/L, 0.42mL/L, 0.63mlIL, 0.84mL/L or 1.68mLJL). Also, the treatment was carried out for 30 minutes rather than 2 hours.
Testing of treated wool samples Testing was carried out as described in Example 1.
Results After 3x5A washes Kft Sx5A washes Fabric samples/treatment method Weight Burst CIE Area Weight Area Weight ________________________________________ Loss Strength ire-whiteness Shrinkage Loss Shrinkage Loss treatment Shrink-resist treatment (°"°) (a) index (%) (%) (%) (%) Untreated Untreated ---425 -4.11 16.8 0.4 22.9 -03 Noffirthertreatment ----408 --2.06 12.7 0.6 -- 30mm treatment with 0.02M phosphate buffer (pI-18) followed 0.9 392 0.38 14.1 -0.7 by 30mm ODE and 140°C cure 10mm 30mm treatment with extracted Pre-treated -0.1 379 6.43 7.8 -0.8 followed by 30mm ODE and with non- 140°C cure 10mm ionic 30mm treatment with extracted surfactant + Na2CO3 and 0.2lmL/L (1.5uJg)Esperase 3.7 345 8.98 3.6 -0.7 for 30mm 30mm followed by ODE 30mm and 140°C cure 10mm 30mm treatment with extracted ando.42mLIL (3uIg)Esperase 5.5 315 13.07 1.1 -0.2 0.4 -0.5 followed by 30mm ODE and 140°C cure 10mm Scanning electron microscopy (SEM) A micrograph of a wool sample treated according to this Example was taken, using the procedure described in Example 1, and is shown in Figure 1. It shows that the fibres of the treated sample of this Example are intact and are not severely damaged by the treatment. -11-*
Example 4
Dycability of Samples The dyeability of the treated knitted wool fabric was tested using the reactive dye Lanasol Red CE (Ciba) following standard dyeing protocols. The fabric was treated for 30 minutes at 50°C in a dye-bath containing 2% owf acetic acid, 5% owf sodium sulphate and 1% owf of the levelling agent Albegal B (Ciba). 4% owf Lanasol Red CE was then added to the dye-bath and the temperature was raised to 100°C at a rate of 1.5°C/mm and maintained at 100°C for 90 minutes. After dyeing the fabric was treated in a 1% owf ammonia solution @H 8.4) at 80°C for 15 minutes. Dyeing took place in a Datacolor Ahiba Nuance IR dye machine at an agitation of 5rpm and a liquor to goods ratio of 30:1.
To test dye fixation, a piece of the dyed fabric was placed in a soaping solution containing 5g/L Ultravon PL (Ciba) non-ionic surfactant and 5g/L sodium carbonate at a liquor to goods ratio of 30:1 and treated at 100°C for 20 minutes using a Datacolor Ahiba Nuance JR dye machine.
Dye exhaustion and total fixation efficiency were determined. Dye exhaustion, expressed as a percentage (%E), is a measure of the amount of dye absorbed on the fibre from the dye-bath solution using the exhaust method of dyeing. Total fixation efficiency, expressed as a percentage (%T), is the proportion of reactive dye originally applied in the dye-bath by an exhaust dyeing method which has been covalently bound to the fibre after dyeing and subsequent soaping. The dye-bath solutions sampled before and after the dyeing process and the solution after soaping were made up to the same fixed volume and absorbance measurements were taken at 5 lonm, the wavelength of maximum absorption specific to Lanasol Red CE) using a Unicam SP1 800 UV/visible spectrophotometer. The percentage of exhaustion (%E) was calculated using Equation (1) and the total fixation efficiency (%T) was calculated using Equation (2).
= 100 x (Abso -Abs1) / Abs0 Equation (1) = 100 x (Abso -Abs1 -Abs2) / Abs0 Equation (2) where Abs0 is the absorbance of the original dye-bath solution at Xm, Abs1 is the absorbance of the exhausted dye-bath solution at Xm and Abs2 is the absorbance of the solution after soaping at Washfastness of the dyed samples were assessed according to BS EN 20105:CO1 conditions at 40°C for 30 minutes.
Results
Example 1 samples
After 3x 5A washes Fabric samples/treatment method _____________________ Area Weight -%E %T Pre-treatment Shrink-resist treatment Shrinkage Loss (%) (°/o) No further treatment 99.5 88.8 13.3 0.5 Pre-treated ________________________________________________________________________ 2hr treatment with extracted wool with non-ionic 96.9 80.7 11.0 -1.7 polypeptide (deactivated) surfactant + ___________________________________________________________________ 2hr treatment with extracted Na2CO3 for polypeptide (deactivated) 99.1 89.6 5.5 1.8 30mm followed by ODE 30mm
Example 2 samples
Fabric samples/treatment method Dye Total Dye -Exhaustion Fixation Pre-treatment Shrink-resist treatment (%E) (%T) Pre-treated with No further treatment -99.5 88.8 -non-ionic 30 mm treatment with extracted wool surfactant + polypeptide (enzyme active) followed by 4 91 8 Na2CO3 for ODE 30mm and 140°C cure 10mm 30mm
Example 3 samples
After 3x 5A washes Fabric samples/treatment method ____________________ Area Weight ________________________________ %E %T Pre-treatment Shrink-resist treatment Shrinkage Loss (%) (%) No further treatment 99.5 88.8 13.3 0.5 Pre-treated __________________________________________________________________________ 30mm treatment with extracted with non-ionic surfactant + and O.42mL/L (3uJg)Esperase 99.3 86.1 1.5 -0.2 Na2CO3 for followed by 30mm ODE and 30mm 140°C cue 10mm No staining was observed for any of the dyed samples on the multifibre strip after washfastness test BS EN 20105:CO1 The results show that cross-linking with ODE is desirable to maintain the shrinkage benefits of the shrink-resist treatment after dyeing.

Claims (12)

  1. CLAIMS1. A method for the treatment of wool to impart shrink resistance thereto, the method comprising (a) obtaining a polypeptide extract by treating animal fibre with a protease and a reducing agent, and (b) applying the polypeptide extract to the wool to be treated.
  2. 2. A method according to claim 1 in which the animal fibre used in step (a) is wool fibre.
  3. 3. A method according to claim 1 or claim 2 in which the protease is a serine-type protease with the corresponding Enzyme Commission number BC 3.4.2 1.62.
  4. 4. A method according to any preceding claim in which the reducing agent is sodium suiphite or sodium hydrosulphite.
  5. 5. A method according to any preceding claim in which the protease in the polypeptide extract is denatured before step (b).
  6. 6. A method according to claim 5 in which fresh protease is added to the polypeptide extract before step (b).
  7. 7. A method according to any of claims I to 4 in which the protease remains active when the polypeptide extract is applied to the wool in step (b).
  8. 8. A method according to any preceding claim in which the wool which is to be treated with the polypeptide extract in step (b) is pre-treated with an alkali scour solution.
  9. 9. A method according to claim 8 in which the alkali scour solution comprises an alkali metal carbonate and a surfactant.
  10. 10. A method according to any preceding claim further comprising (c) treating the treated wool with a crosslinking agent.
  11. 11. A method according to claim 9 in which the crosslinking agent is glycerol diglycidyl ether, 1 -(3 -dimethylamino-propyl)3-ethyl-carbodiimide hydrochloride or 1, 4-butandioldiglycidyl ether.
  12. 12. A method according to claim 10 or claim 11 further comprising (d) curing the crosslinking agent.
GB1015962.2A 2010-09-23 2010-09-23 Treating wool with animal fibre derived polypeptide extract, to impart shrink resistance Withdrawn GB2483886A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB513919A (en) * 1938-04-21 1939-10-25 Wool Ind Res Association Treatment of wool to diminish shrinkage
JPS5119899A (en) * 1974-08-06 1976-02-17 Nakajima Spinning Co Yomono hisuikeikakohoho
WO2002004739A1 (en) * 2000-07-10 2002-01-17 The Nottingham Trent University A method for enzymatic treatment of textiles such as wool
CN101220355A (en) * 2008-01-18 2008-07-16 浙江雀屏纺织化工股份有限公司 Biological complex enzyme and use method of the enzyme on woollen sweater shrink-resistant finish

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB513919A (en) * 1938-04-21 1939-10-25 Wool Ind Res Association Treatment of wool to diminish shrinkage
JPS5119899A (en) * 1974-08-06 1976-02-17 Nakajima Spinning Co Yomono hisuikeikakohoho
WO2002004739A1 (en) * 2000-07-10 2002-01-17 The Nottingham Trent University A method for enzymatic treatment of textiles such as wool
CN101220355A (en) * 2008-01-18 2008-07-16 浙江雀屏纺织化工股份有限公司 Biological complex enzyme and use method of the enzyme on woollen sweater shrink-resistant finish

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