Classifications

• • 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
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
  • D06B15/00—Removing liquids, gases or vapours from textile materials in association with treatment of the materials by liquids, gases or vapours
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
  • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
  • D06P1/0004—General aspects of dyeing
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
  • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
  • D06P1/0036—Dyeing and sizing in one process
• • 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
  • D06M2101/10—Animal fibres

Definitions

• the present invention relates to the method according to the preamble of claims 1 and 2 to a method for finishing woollen textiles, and to a woollen textile according to the preamble of claim 18.
• chlorine based compounds have been used, including gaseous chlorine, sodium hypochlorite, dichloroisocyanuric acid or potassium permanganate in conjunction with hypochlorite at a high pH, or sodium sulphate or permonosulphuric acid at a low pH.
• gaseous chlorine sodium hypochlorite, dichloroisocyanuric acid or potassium permanganate in conjunction with hypochlorite at a high pH, or sodium sulphate or permonosulphuric acid at a low pH.
• hexame- thylenediamine has been used in a first stage, and sebacoyl chloride in a second stage.
• a processing method of wool most commonly used is the IWS/CSIRO Chlorine Hercosett method, wherein an acid chlorination is followed by a treatment with the polymer.
• Treating keratin-containing material with an alkaU-containing alcohol solution and a protease- containing aqueous solution has also been suggested (WO 00/50686).
• the published patent application WO 99/42649 treats wool in water with subtilisin protease in a large amount of water at various temperatures.
• the wool is treated by means of wet waxing.
• about 50% of the strength of the wool fibre is lost. If the tips of the scales are filled chemically with various resins, for example, the effect will cease as soon as after the first water washing cycle, whereby the product turns rough and fuzzy.
• wool articles finished with the techniques presently used shrink about 10 - 15% when washed with water, whereas the goal is below 3%.
• woollen articles do not withstand washing with water, the manufacturers of the articles must recommend dry cleaning for the articles, which, in turn, renders the use of woollen articles more expensive and more difficult to the consumer. For all the above reasons, woollen articles are not widely used, although the good proper- ties of woollen articles are commonly known.
• the purpose of the present invention is to provide solutions, which can be used to improve the finish of woollen textiles so as to maintain the good properties of the same.
• the purpose in particular, is to provide solutions, which can be used to make woollen textiles resistant to abrasion and water wash without shrinking, felting or pilling, and to maintain the good properties, such as warmth and excellent appearance, as well as the strength properties.
• a further purpose is to provide solutions, which can be used to make the woollen textiles feel softer.
• woollen textiles are treated using a method, wherein the woollen textile in an aqueous solution is brought into contact with protease in a large amount of water so that the woollen textile is moved as little as possible or not at all.
• the temperature should be about 60°C or less.
• the treatment time can be about 10 to 90 min. After this, the enzyme is inactivated. After the protease treatment, the woollen textile is taken to dry in mechanical drying method so as to reach residual moisture content of about 10 to 45%. The final drying of the woollen textile is preferably carried out without any mechanics, e.g., flat or in a hanging form.
• the method according to the invention is mainly characterized by what is stated in the characterizing part of claim 1.
• the woollen textile according to the invention is mainly characterized by what is stated in the characterizing part of claim 18.
• the enzyme is inactivated by using a method, wherein the temperature is not raised to above 60°C. Decreasing the pH sufficiently low or, for example, by adding copper ions may inactivate the en- zyme. On the other hand, wool endures even higher temperatures, when the pH is made sufficiently low. Therefore, according to another preferred embodiment of the invention, the enzyme is inactivated by means of a method, wherein the pH is lowered to a range of about pH 4 to 5 or less.
• Dyeing can also be combined with the treating method of woollen textiles. Dyeing is preferably carried out in connection with the wet process. If dyeing is carried out after the enzyme treatment, the enzyme does not need a separate inactivation but the enzyme can be allowed to inactivate under the dyeing conditions.
• the method according to the invention which dyeing is incorporated into, is characterized by what is stated in the characterizing part of claim 2.
• a substantial part of the edges of the tips of the wool fibre scales can be removed enzymatically. This causes some decrease in weight during treatment but, as a whole, the treatment causes no essential weakening of the strength properties of woollen textiles, which is the case in previously known enzymatic finishing methods, as in them, both de- sired and undesired parts come off the fibres uncontrollably because of the heavy enzymatic and mechanical treatments.
• the mechanical drying phase such as the tumble-drying stage, normally causes a decrease in strength, but in this method, the mechanical drying stage is kept so short that no essential decrease in strength takes place.
• Mechanical drying is continued to certain residual moisture content only, after which the final drying is preferably carried out without mechanics, for example, flat or in a hanging form.
• the finish according to the present invention can be carried out on dyed or undyed woollen textiles.
• the woollen textile is first subjected to enzyme treatment and then to dyeing. It has been ob- served that extremely good dyeing results are obtained in this way. The colours have been found to be brighter and deeper, when dyeing is carried out after the enzyme treatment.
• Woollen textiles are mainly made by using the worsted or the carded wool yarns methods.
• the worsted method long-stapled wool is used, from which lightweight or medium-heavy woven and knitted fabrics are made.
• Examples of worsted articles include suiting, trousering and light knitted fabrics. Woollen textiles can be dyed as tops, yarn, fabric or ready-made articles.
• carded wool yarns short-staple wool is used, from which heavy weight woven and knitted fabrics are made.
• Examples of products made by using the carded wool yarns include upholstery fabrics, thick knitted fabrics, felts, flannels and tweeds. These woollen textiles are dyed as fibre, yarn, fabric or finished articles.
• the finish of woollen textiles refers to any procedure that can be used to remove the rough feeling of the woollen textile and to make the surface of the wool look smooth, not pilling.
• the woollen textiles can be finished by means of either wet or dry finishing. In yarn dyed fabrics, mere steaming may be enough; generally, however, the woollen textiles are washed and stentered (wet fixing) after weaving.
• the finish of woollen textiles refers to wet finishing, which can also include dyeing treatment.
• the term "woollen textile” in connection with this invention refers to wool fibre or wool fibre-containing tops, yarn, knitted or woven fabric containing at least 30%, preferably at least 50%, most preferably at least 70% of wool fibre.
• the wool fibre refers to fibre containing 100% wool.
• the wool tops or bay-yarn can be pure wool, or the wool fibre may have been woven into or mixed with a synthetic fibre, such as polyacryl or polyester.
• the wool fibre may also have been woven into or mixed with some other protein-containing fibre, such as silk, or with some other natural fibre, such as cotton or its derivatives, such as viscose.
• the tops refer to a bundle of fibres, from which the yarn is spun. The yarn is used to make knitted or woven fabrics and the finished textile products are then sown from them.
• the reason for adding synthetic fibres to wool fibres in knitted and woven fabrics is that the synthetic fibres are normally less expensive, whereby the price of the knitted or woven woollen fabric becomes more advantageous. Another reason is that the synthetic fibre makes wool-containing products dry quicker, which is of importance when making sports wear in particular. Synthetic fibres are added to knitted and woven woollen fabrics also because they enhance the strength of the knitted or woven fabric.
• the properties of the wool fibre are influenced in particular. If the portion of wool fibre is less than 30%, the properties of the other fibres become dominant. For example, polyacryl and polyester pill fairly easily, and this property cannot be influenced by the present wool treatment method.
• the present method is the most advantageous when treating woollen textiles containing more than 70%, preferably more than 80%, and most preferably 100% of wool.
• Enzyme treatment causes a decrease in weight of woollen textiles, and if the treatment is too strong, also in the strength of the textile. On the other hand, the decrease in weight of the textile indicates that the enzyme has worked.
• Water wash of wool in connection with the invention refers to washing by means of a normal wool- washing program (the standard EN 60456) at a temperature of 40°C, the program taking 45 to 70 min.
• the detergent used is a wool-washing agent; softeners can also be used.
• the strength loss of the woollen material that was treated with dosages of 0.1 ml/g or greater was over 50% compared with a corresponding untreated woollen material.
• the instructions of the manufacturer of protease for the dosage were 0.125 ml/g at a minimum.
• the strength loss even at the most advantageous residual moisture levels was 53%.
• the strength loss at the most advantageous residual moisture levels was from 56 to 60%.
• the strength loss was 20%.
• the strength loss was 14%.
• the abrasion resistance was defined by the Martindale method in accordance with the standard SFS 4328 (BS 5690:1979).
• the abrasion resistance measures the wear and tear properties of the woollen textile.
• the abrasion resistance result indicates the number of rotations needed for the textile to wear out upon rubbing the woollen textile under examination against a friction surface.
• the abrasion resistance is assessed as the number of rotations needed for the wearing surface of the textile to break.
• “Lint forming or pilling” refers to the small fibre bundles or lint, which are formed on the surface of the woollen textile.
• the tendency to pill was defined by rubbing the samples by means of the Martindale method for 125, 500 and 2000 rotations, after which the rubbed samples were evaluated by means of a scale of reference in accordance with the standard SFS 3378 on the basis of the appearance of the samples.
• the value 5 on a scale of 0 to 5 signifies the smallest amount of pilling.
• the term “no substantial lint” means that the majority of the textile surface is free of lint, i.e., the pilling value is in a range of 3 to 5.
• the tendency to form lint decreases directly in proportion to increasing the dosage.
• the pilling values at the most advantageous residual moisture contents for all revolutions of rubbing were in a range of 4.0 to 4.7.
• the pilling values on dosages of 0.025 ml/g were in a range of 3.5 to 4.2 and on dosages of 0.05 ml/g in a range of 3.5 to 4.5.
• the pilling values of the most advantageous finishing conditions correspond to the common quality requirements of those who buy products made of woollen materials, which is at the level of 3 to 4.
• the woollen textiles that were treated under the conditions of protease treatment which were the most advantageous to the woollen textiles (the protease dosage was 0.0125 ml/g and the residual moisture content in the mechanical drying stage was from 10 to 30%), lost a maximum of 14% of their strength in the treatments, and shrank in the washings by 0.7% at a maximum in the direction of the warp, and by 0.8% at the maximum in the direction of the weft.
• the pilling values of these sam- pies were in a range of 3.5 to 4.2%, the touch had softened in the treatments the most and, in addition, the softened touch kept well in the washings.
• the term "felting" or "interlacing” refers to the effect on the appearance of woollen textiles caused by shrinkage.
• shrinkage means that the size of the woollen textile has decreased, i.e., a dimensional change has taken place. This is indicated as percent of the size of the untreated material It is given separately in the direction of the weft and the warp for both woven and knitted fabrics. Some shrinkage takes place during the finishing of the woollen textile; however, this is of no importance to the consumer. The shrinkage that takes place after finishing is essential. If the shrinkage after finishing is less than 3%, it is acceptable. Shrinkage greater than this affects the appearance of the textile, making the textile look felted. This invention is concerned with monitoring the shrinkage, which takes place during finishing and which generally varied from about 3% to 5%. The shrinkage that took place after finishing was measured after 5 times of washing.
• the amount of shrinkage was less than 3% after finishing and, generally, varied within 0% and 2%.
• the term "no substantial felt- ing" means that the textile has not shown essential shrinkage, i.e., the shrinkage is less than 3%.
• the dimensional changes were defined in accordance with the standard SFS 5157 (ISO 5077-1984). For the definition of the dimensional changes, areas of 50 cm x 50 cm were marked on the pieces of material, enabling measurements in the direc- tion of the weft and the warp, which had taken place in finishing and in the subsequent water washes.
• the dimensional change that took place during the finishing was measured and given in % of the original untreated material.
• the dimensional change that took place in 5 water washes (the 2 nd dimensional change) was defined and given in % of unwashed and finished material.
• the shrinkage of the woollen material that took place during the finishing (the 1 st dimensional change) in the direction of the warp was in a range of 1.8 to 4.5% and in the direction of the weft in a range of 0 to 5%. Under the most preferable conditions, it was 2.8 to 4% in the direction of the warp, and 0.5 to 2.5% in the direction of the weft.
• the dimensional change of the finished materials in the test series varied in the direction of the warp in a range of 0 to 1.9% and in the direction of the weft from 0 to 4.9%.
• the dimensional change of the samples that were finished under the most advantageous conditions after the water washes was 0 to 1% in the direction of the warp, and 0.2 to 0.8% in the direction of the weft.
• the dimen- sional change of the original material after five water washes was 4.5% in the direction of the weft and 5.0% in the direction of the warp.
• the appearance and the touch were evaluated by panel determinations. The panel consisted of five judges, and the results given by them were used to calculate a mean value, which was then given as the result.
• the appearance and the touch of the materials were graded on a scale of 5, 4, 3, 2 or 1 minuses, 0 or 1, 2, 3, 4 or 5 plusses.
• the touch was evaluated for the softness of the materials.
• the appearance was visually evaluated for a trim and smooth surface of the material, for the opening of the stitches and the overturning and bias of the stitches and the wales.
• an original unfinished woollen woven or knitted fabric was used as a reference. According to the touch and appearance grading, all samples that were treated felt softer than the original untreated samples.
• the references were the ones that showed the least degree of softening among the treated samples.
• the method according to the present invention can be used to treat wool fibre, tops, yarn, knitted fabric, woven fabric or finished articles made of the knitted or the woven fabric.
• the process can just as well be implemented for metre material and ready made products.
• the materials containing the above-mentioned wool fibre are herein called woollen textiles.
• a woollen textile in an aqueous solution is brought into contact with a protease enzyme in a large amount of water so that the woollen textile is moved as little as possible or not at all at a temperature of 60°C or less.
• the temperature of about 60°C herein also refers to tem- peratures that are 1 to 3° higher or lower.
• the treatment time can be from 10 to 90 min.
• the treatment time is preferably 15 to 60 min, more preferably 15 to 30 min.
• the treatment time is preferably 15 to 60 min, more preferably 15 to 45 min.
• the protease enzyme is preferably an alkaline protease, most preferably serine pro- tease.
• proteases of various manufacturers are suitable for the purpose, however, preferably proteases that the manufacturers recommend for the treatment of wool.
• proteases include, e.g., Genencor's Multiplus L or Gentle L, Novo's Novolan L or Novon Savinase.
• the pH is preferably adjusted to a range of 6 to 11, more preferably to a range of 7 to 11, particularly to a range of 7 to 9 or even 9 to 11.
• the pH the manufacturer recommends for the proteases used should be taken into account.
• the manufacturer recommends that Genencor's Protex Multiplus L enzyme preparation should be used at pH of 7 to 9.5, Protex Gentle L at pH of 6.5 to 10, Novo's Novolan L at pH of about 8.5, Novo's Savinase at pH of 8 to 8.5.
• the appearance and the touch of woollen textiles even improved some, when the pH was raised to 11, while the temperature was 50°C.
• the dosage for knitted fabrics is preferably less than 8 mg/g of dry textile, more preferably less than 4.4 mg/g; most preferably less than 3.5 mg/g of dry textile.
• a preferred dosage for woven fabrics is less than 35 mg/g of dry textile, more preferably less than 17.5 mg/g, most preferably less than 8 mg/g of dry textile.
• increasing the amount of mechanics and lengthening the enzyme treatment time also had a weakening effect on the strength of the woollen textiles.
• wool fibre in an aqueous solution is brought into contact with a protease enzyme in a large amount of water.
• the large amount of water in this connection refers to the fact that the ratio of the weight of the knitted or woven fabric under treatment to the weight of the water is at least 1/10; the liquor ratio is preferably in a range of 1/20 to 1/40, the liquor ratio is most preferably about 1/30.
• the temperature of about 60°C herein also refers to any temperatures that are 1 to 3°C higher or lower). This is the case in particularly, when the conditions in the treatment solution are neutral or alkaline. In that case, it is not preferable to inactivate the enzyme by means of temperature (i.e., increasing the temperature).
• Recommendable inactivation methods of enzyme include, e.g., chemical inactiva- tion, such as lowering the pH sufficiently low, to acidity of pH 4 to 5, or by adding copper ions, for example.
• the drum or tunnel drying times are short, less than 10 min, preferably 5 to 10 min, most preferably about 6 min (+/- 1 min).
• the residual moisture content is 35 to 40% at a maximum, 5 to 10% at a minimum, and preferably 10 to 20%.
• room temperature refers to a temperature of about 18 to 30°C, most commonly about 20 to 25°C.
• the dyed woollen textiles can be treated with enzyme or the dyeing treatment can be carried out after the enzyme treatment.
• the latter in particular, brings about extremely good dyeing results.
• Dyeing can be carried out by means of the methods well known by those skilled in the art.
• the temperature increases to over 90°C; typically, the temperature is 90 to 98°C, preferably 90 to 95°C, but when the pH is below 5, typically in a range of pH 4 to 5, the wool withstands the dyeing well.
• the effect of the enzyme is terminated or it stops before the dyeing stage.
• the equipment used in this invention it was preferable to adjust the mechanics to 6 - 10 rpm during dyeing.
• dyeing wool any commonly used and commercially available wool dyestuffs can be used.
• Dyeing can be carried out at temperatures of about 90 to 98°C, preferably at temperatures of 90 to 95°C, with a pH of 4 to 5. Under these conditions, the wool withstands treatments of as much as about 1 hour in duration.
• so called reactive dyestuffs can also be used, whereby temperatures as high as the above and a low pH are used, but part of the treatment is carried out at lower temperatures of about 40 to 60°C.
• protease treatment are the same for the same material independent of whether the material is yarn dyed or if the material is dyed in the same wet process with the protease treatment.
• the wool fibre is not subjected to a temperature of over about 60°C in any other stage except during dyeing. If the temperature is raised to over 60°C, when inactivating the enzyme, for example, the pH should be low, i.e., in a range of 4 to 5 or less. Another essential fact is that, under no circumstances should the wool fibre be subjected to excessive mechanical stress, especially not during the wet process. It is also of importance to leave a suitable residual moisture content to the woollen textile after the mechanical treatment and before final drying, which is preferably carried out without mechanics. Neither the amounts of enzyme should be so great so as to essentially weaken the woollen textile.
• the method according to the present invention is a combination of the stages of a method, where in every step, a wrong type of stress on the wool fibre is avoided.
• woollen textiles can be manufactured, which last at least 5 times washing with water according to the wool instructions. Indeed, it has been observed that the woollen textiles that were treated with the method according to the most advantageous embodiments of the invention withstood well as many as 10 or 20 washings without shrinking more than 3%, and without essentially felting or pilling or becoming rougher in the water wash. It was also established, that one washing after the mechanical treatment further improved the touch and the appearance of the wool textile. This effect was most obvious in wool wash that is preferably carried out with cool water at about 30°C.
• the softness and pilling of the woollen textiles are controlled by means of a correct enzyme treatment, and the dimensional change of the textile is controlled by means of a correct process.
• the tests of the examples employed the following machines and equipment: The protease and dyeing treatments were carried out in the open drum machine Wasca- tor FOM 71 Special.
• the diameter of the inner drum was 515 mm, the depth 335 mm, and the volume 70 dm .
• the dram drying stage was carried out by means of the drying and punching machine LAKO KA 901, which includes an ITARA air- circulation system.
• the inner diameter of the drum was 1600 mm, the length 1350 mm, the volume 27001, and the rotational speed 30 rpm.
• the final drying stage was carried out in a hanging form in a steam tunnel VEIT (tailor made system) using hot-air chambers only, in other words, the steam in the steam chambers was not on.
• the tunnel contains 1 steam chamber and 3 air chambers. In these tests, only the air chambers were used, which comprise continuous heat regulation and had been adjusted to room temperature, 24°C.
• both woven and knitted woollen fabrics were treated, which had been made from 100% fine Merino wool yarn, which was spun by the worsted method and had a thickness of NM 2/28.
• the yarn was off-white and it had been treated to be ready for dyeing, i.e., washed and steamed after spinning.
• the woollen textiles had been cut into pieces of 60 cm x 60 cm for the tests.
• the dimensional changes were defined in accordance with the standard SFS 5157 (ISO 5077-1984).
• SFS 5157 ISO 5077-1984.
• areas of 50 cm x 50 cm had been marked on the pieces of material for measuring the dimensional changes in the direction of the weft and the warp, which had taken place in the finishes and the subsequent water washes.
• the strength measurements of the woven fabrics were defined by means of the tensile testing machine method in accordance with the standard SFS 3981 (SIS 251231).
• the abrasion resistance was defined by means of the Martindale method in accordance with the standard SFS 4328 (BS 5690:1979).
• the pilling tendency was defined by rubbing the samples by the Martindale method for 125, 500 and 2000 rubs, after which the abraded samples were assessed by means of a comparison scale according to the standard SFS 3378 on the basis of the appearance of the samples. On a scale of 0 to 5, the value 5 refers to the smallest amount of pilling.
• the woollen fabric used was woven from the yarn mentioned above; the weave was l x l plain weave, the basis weight 190 g/m . A series of 21 trial samples was conducted. The size of a trial sample was 1716 g.
• Genencor's protease enzyme (Genencor Protex Multiplus L) was used. Serine proteases of also other manufacturers had been used in preliminary tests, but no significant differences were observed between them.
• protease dosed was 0 or 0.025 or 0.05 or 0.1 or 0.2 ml/g of dry woollen textile.
• 0.1 ml of Genencor's Protex Multiplus L protease corresponds to 3.5 mg of protein.
• Other proteases could be dosed, correspondingly, calculated as protein grams per dry woollen textile.
• protease recommends an amount of 0.125 to 1 g/1.
• the dosages recommended by the protease manufacturers were tested, which dosages were found to be detrimental to the strength properties of the woollen textiles.
• the treatments were carried out in a liquor ratio of 1 :30, which in the preliminary tests was found to be large enough.
• the manufacturer of the enzyme had recommended a pH between 7 and 9.5, so the treatment in these tests was conducted at pH 9. When repeating the tests at pH 11, the touch and the appearance of the woollen textile were discovered to be as good as or better than at pH 9.
• the temperature in the protease treatment was 50°C.
• the treatment time was 30 min.
• the treatment was carried out in the above-mentioned open drum machine (machine 1).
• the mechanics of the machine were adjusted to the value 2.
• three different levels of mechanics were used.
• the mechanics 0 corresponded to a rotational speed of 4.0 rpm
• the mechanics 1 corresponded to 6.0 rpm
• the mechanics 2 corresponded to 10.0 rpm.
• the protease treatment was ended by the inactivation of the enzyme at a tempera- ture of 60°C.
• the pH was adjusted to a level of 4 for 15 minutes.
• rinsing at a temperature of 30 to 40°C was carried out for 10 minutes.
• the treated woollen materials were spin-dried so as to obtain a moisture content of 50 to 70%, which in this test corresponded to a spinning time of 2 minutes.
• the test material was brought to drying in tumble-drying (machine 2) at 50°C so as to obtain certain residual moisture content of 5 to 35%.
• machine 2 tumble-drying
• Table 1 shows the circumstantial variables for this test series (the protease dosage and the residual moisture content), the weight loss in the protease treatment and in the water washes following the same.
• the weight loss of the woollen textiles during the finish and in the water washess after the finish was measured and given in % of the original weight of the untreated woollen textile.
• the weight loss was stated to be directly proportional to the efficiency of the protease treatment. With the dosage increasing, the weight loss increased, correspondingly. According to the results, the weight loss in the protease treatments of the test series was in a range of 9 to 13%.
• the residual moisture content had no effect on the weight loss in the treatment or the subsequent washes.
• the most advantageous conditions were the dosages of 0.025 to 0.05 ml/g in combination with the residual moisture contents of 10 to 30% after tumble-drying. The weight loss occurring under these conditions was 9 to 9.5% both in the protease treatments and the washes subsequent to the treatment. On larger dosages of 0.1 to 0.2 ml/g, the weight loss in the treatments was at a level of 12 to 13%, and in the water washes subsequent to the treatment, a further weight loss of 10 to 20% took place.
• the dimensional changes are shown in Table 2.
• the dimensional change that took place during the finish (the 1 st dimensional change) was measured and given in % of the original untreated material.
• the dimensional change that took place in 5 washes (the 2 nd dimensional change) was defined and given in % of the unwashed, finished material.
• the shrinkage of the woollen material during the finish (the 1 st dimensional change) in the direction of the warp was in a range of 1.8 to 4.5%, and in the direction of the weft in a range of 0 to 5%. In the most advantageous conditions (samples 6, 7, 10 and 11), it was 2.8 to 4% in the direction of the warp and 0.5 to 2.5% in the direction of the weft.
• the dimensional change of the finished materials after five washes varied in the test series in the direction of the warp in a range of 0 to 1.9% and in the direction of the weft 0 to 4.9%.
• the dimensional change of the samples finished in the most advantageous conditions (samples 6, 7, 10 and 11) after the washes was 0 to 1% in the direction of the warp and 0.2 to 0.8% in the direction of the weft.
• the dimensional change of the original material after five washes was 4.5% in the direction of the weft and 5.0% in the direction of the warp.
• Table 3 shows the results of the strength and pilling measurements.
• the loss in strength of the woollen material treated with dosages of 0.1 ml/g or higher was over 50% compared with corresponding untreated woollen material.
• the instructions of the protease manufacturer for the dosage were 0.125 ml/g at a minimum.
• the loss in strength even at the most advantageous residual moisture content levels was 53%.
• dosages of 0.2 ml/g the loss in strength at the most advantageous levels of residual moisture contents was 56 to 60%.
• the loss in strength was 20% (samples 10).
• sample 6 was the softest in the test series, i.e., it showed the highest degree of softening in the treatments.
• the soft touch of sample 6 was the best in the series to maintain its softness in washing.
• Sample 7 had the second best touch in the series, i.e., it showed the second highest degree of softening in the treatments, the touch having also survived the washings.
• the woven woollen fabrics which were treated under the conditions of the protease treatment that are the most advantageous for the woollen fabric of the example (a protease dosage of 0.0125 ml/g and a residual moisture content of 10 to 30% after the mechanical drying stage), lost a maximum of 14% of their strength in the treatments, and shrank a maximum of 0.7% in the direction of the warp, and a maximum of 0.8% in the direction of the weft in the washings.
• the pilling values of these samples were between 3.5 and 4.2, the touch had softened the most in the treatments and, in addition, the softened touch had endured the washings well.
• the above-mentioned woollen yarn was dyed and 1/1-rib knit, i.e., plain fabric, was made of the dyed yarn for the protease treatment testing of dyed knitted fabrics.
• the basis weight of the knitted fabric was 375 g/m 2 .
• a series of 10 trial samples was conducted to find a level of dosing and mechanics of protease treatment that would be suitable for knitted materials.
• the size of the trial sample was 600 g.
• the enzyme of Example 1 was used.
• the numbers of the samples of the dyed materials of the test series (dyestuff 1) were 30 to 39.
• the protease treatment testing of dyed knitted fabric was continued using a test series of 20 tests, wherein the numbers of the samples of the dyed material (dyestuff 2) were 41 to 61.
• the circumstantial variables in the tests comprised the protease dosage, the protease treatment time, the pH of the treatment, and the level of mechanics.
• the amounts of the protease dosed were 0 or 0.0125 or 0.025 or 0.125 or 0.250 ml/g.
• the treatments were carried out in a liquor ratio of 1:30, which in the preliminary tests was found to be large enough also for knitted fabrics.
• the manufacturer of the enzyme had recommended a pH of between 7 and 9.5, so the treatment in these tests was carried out at the pH values of 7 and 9.5.
• the treatment times were 15 min and 30 min.
• the temperature in the enzyme treatment was 50°C.
• the treatment was carried out in an open drum machine (machine 1). The mechanics of the machine was 0 or 1 or 2.
• Inactivating the enzyme at a temperature of 60°C terminated the enzyme treatment.
• the pH was adjusted to the level of 4 for 15 minutes.
• rinsing was carried out at 30 to 40 degrees for 5 minutes.
• the woollen textile was spin-dried so as to obtain a residual moisture content of 50 to 70%. This corresponded to a centrifu- gation of 2 minutes.
• the test material was taken to dry in tumble-drying (machine 2) at 50°C so as to reduce the residual moisture content to a level of 10 to 30%. On the basis of the preliminary tests, this residual moisture content had been found to be the most suitable.
• Tables 5, 6 and 7 show the circumstantial variables of the dyestuff 1 of the test series (the sample numbers of 30 to 39) and the results of the measurements.
• Tables 8, 9 and 10 show the circumstantial variables of the dye- stuff 2 of the test series (the sample numbers of 40 to 61) and the results of the measurements.
• Table 7 shows the assessments for the appearance and the touch of dyestuff 1. On the basis of the test series of the dyestuff 1, the level of mechanics 2 was too strong, causing, according to the touch and appearance assessment, felting or interlacing as early as in the finishing treatments (samples 35, 37 and 39). The felting of the materials in the treatments corresponded to a shrinkage of over 10% in the dimensional changes.
• sample 32 was the best after the treatment and, in addition, these properties had endured the washings best.
• Sample 38 was assessed to have an equal touch after the treatment, but its appearance was slightly better than that of sample 36. In samples 36 and 38, the stitch pattern had slightly opened in the treatments and the stitches showed a slight bias, making the surface of the knit more uneven compared with the untreated knitted fabric. According to the assessments of the appearance and the touch and regarding the circumstantial variables of the protease treatments, pH 9.5 was more advantageous than 7, and the mechanics 0 was more advantageous than the mechanics 1.
• the dimensional changes of the test series of dyestuff 1 were defined as in Example 1.
• the 1 st dimensional change and the 2 nd dimensional change are shown in Tables 5.
• the felting of the materials in the treatments is shown as shrinkages of over 10%.
• the 1 st dimensional changes in the direction of the warp were between 3.3 and 9.3%, and in the direction of the weft between -3.1 and 1.0%.
• the 2 nd dimensional changes in the direction of the warp were between -0.2 and 1.0%, and in the direction of the weft between -1.0 and 0.7%.
• the unfinished materials shrank by 5.1% in the direction of the warp, and stretched by 4.2% in the direction of the weft.
• the pilling and abrasion resistance results are shown in Table 6. These properties were not measured from the materials that felted in the treatments.
• the pilling val- ues of the samples that were graded high in the appearance and touch assessments (32, 36 and 38) were between 3.0 and 4.5, whereas the corresponding values for the unfinished samples were between 1.5 and 3.0.
• the abrasion resistance of the samples 32, 36 and 38 decreased 11.6 to 14.2% compared with the abrasion resistance value of the unfinished material.
• pilling values of the samples 33 and 34 which were not graded high in the appearance and touch assessments but had not felted in the treatments or washings either, were in a range of 2.0 to 4, and the loss in abrasion resistance in the treatments was from 16 to 24% compared with the corresponding value of the original unfinished sample.
• the mechanics levels 0 and 1 were se- lected for the testing of dyestuff 2.
• the other variables selected were treatment times of 15 and 30 min and pH levels of 7 and 9.5.
• the dosages were 0 or 0.0125 or 0.125 ml/g.
• Sample 58 was graded the highest in the touch and appearance assessments of this test series, its touch having become soft and pleasant, still retaining its woolly nature. The woolly touch also remained in washings.
• sample 50 (mechanics 0) after the treatment was better than that of sample 47 (mechanics 1), and the better appearance of sample 50 also kept well in the washings.
• Sample 59 (mechanics 1) was more uneven than sample 58 (mechanics 0) after the treatment.
• sample 60 (dosage 0.125 ml/g, the mechanics level 0) after the treatment was as good as sample 58, i.e., trim, but the touch had turned viscous. The viscous touch remained unchanged in the washings.
• sample 61 (dosage 0.125 ml/g, mechanics 1) was trim after the treatment, but the touch had turned viscous. The viscous touch had increased in washings. The samples, which had been graded high for the appearance and the touch, had in the protease treatment a pH of 7 and the mechanics level 0.
• Table 8 shows the dimensional changes of the test series, which were defined as in the previous tests.
• the dimensional changes of the samples (the 2 nd dimensional changes), whose appearance and touch were graded high, were in washing between -1.0 and 1.2% in the direction of the warp, and between -0.6 and 0.3% in the direction of the weft.
• Both the unfinished materials (samples 52) and the references (samples 44, 45, 46 and 51) had experienced dimensional changes of over 3% in the water washes.
• the abrasion resistance and the pilling results of dyestuff 2 are shown in Table 9.
• the abrasion resistance had decreased in proportion to the dosages so that the greater the dosage, the more the abrasion resistance had decreased.
• the mechanics of the treatment was increased, the abrasion resistance correspondingly fur- ther decreased, the dosages of the protease treatment being the same.
• the samples with a protease treatment dosage of 0.125 ml/g showed a decrease of 14 to 21.3% in the abrasion resistance.
• the pilling results of the samples which in the appearance and touch assessments had gained at least 2 plusses, were between 3 and 5.
• the pilling values of the un- treated samples remained in a range of 1 to 3.
• the off-white knitted woollen fabric that was described at the beginning of the examples, comprising 1/1 ribbing and having a basis weight of 430 g/m2, was used, and subjected to the combined protease and dyeing treatments.
• a series of 16 tests was conducted.
• the size of the trial sample was 300 g.
• the circumstantial variables comprised the dyestuff, the dosage and pH of the protease treatment, the time and the mechanics.
• the amount of protease dosed was 0 or 0.0125 or 0.125 or 0.25 ml/g.
• the pH was 7 or 9.5.
• the mechanics was 0 or 1.
• the protease treatments were conducted either before or after the dyeing treatment.
• the protease treatments were carried out in a liquor ratio of 1:30.
• the pH was 7 or 9.5.
• the treatment time at pH 7 was 15 min and at pH 9.5 30 min.
• the temperature in the enzyme treatment was 50°C.
• the treatment was carried out in the above- mentioned open drum machine (machine 1).
• the mechanics of the machine was 0 or 1.
• the enzyme treatment was terminated by inactivating the enzyme at a temperature of 60°C by adjusting the pH to a level of 4 for 15 minutes. After this, rinsing was carried out for 5 minutes at 30 to 40°C.
• the liquor was changed, followed by the dyeing stage using a normal woollen textile dyeing method at a pH level of 4 to 5 and at a temperature of 90°C, the fixing time varying between 20 and 30 minutes, depending on the shade. After this, rinsing was carried out at 40°C for 5 minutes. Then, the procedure was continued by the centrifugation and drying methods according to the previous protease treatments. In this way, the so-called enzyme and dyeing tests were carried out, the samples 64, 66, 77, 78, 79, 80 and 81.
• the above-mentioned dyeing treatment was carried out, followed by the protease treatment so as to cool down the treatment liquor to 50°C after the dyeing and to exchange the liquor for a new one, wherein the protease treatment, which was described in connection with the previous tests, with its spinning and drying stages was carried out.
• so-called enzyme, drying and dyeing tests were carried out, the samples 67, 68, 69 and 70.
• the protease treatment was carried out, as described in the first tests of this series. After this, the spinning and the tumble-drying stage of the drying method were carried out so as to obtain a residual moisture content of 10 to 35% of the woollen textile. Thereafter, the dyeing treatment was carried out as described in the first tests of this series. After the dyeing, spinning and drying were carried out, as after the protease treatments of the previous tests.
• the dimensional changes were defined as in the previous tests and the results are shown in Table 10.
• the dimensional changes subsequent to the washings i.e., the 2 nd dimensional changes for the references (materials treated with a buffer and dyed) were in the direction of the warp between 3.7 and 4.5% and in the direction of the weft between -3.6 and 4.2%.
• the dimensional changes subsequent to the washings were minor for the samples dyed by the protease treatments, i.e., they were in the direction of the warp in a range of 0.6 to 1.8% and in the direction of the weft in a range of -2.0 to 0.5%.
• Adding a mechanical drying stage between the protease treatment and the dyeing treatment was not found to provide any improvements in the mechanical measurement results.
• the points received by these samples (67, 68, 69 and 70) in the touch and appearance assessments were also average.
• the samples that were graded highest in the touch and appearance assessments after the treatments were the samples 78 and 79, which had the most pleasant and softest touch and, at the same time, a trim and crease-resistant face, and these properties were the best in enduring the washings.
• the touch of sample 78 was graded the best of the whole series.
• the dosage was 0.0125 ml/g, which did not weaken the abrasion resistance by more than 10%.
• the dosage of the samples 79 was 0.125 ml/g, which caused a weakening of the abrasion resistance by 14 to 21% in the treatments. A weakening of the abrasion resistance of over 20% has been found to be harmful.
• the appearance of sample 80 was graded trim, but had lost its woolly touch.
• Example 3 it could be concluded that it is preferable to carry out the protease treatment in the same wet process with the dyeing treatment before the dyeing stage.
• the most advantageous conditions for the protease treatment are the same for the same material, independent of whether the material is yam dyed or if the material is dyed in the same wet process with the protease treatment.
• Test numbers 40 to 52, 58 to 61
• Test numbers 40 to 52, 58 to 61

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