EP4092185A1 - Fibre de cellulose régénérée fibrillée et tissu utilisant ladite fibre - Google Patents

Fibre de cellulose régénérée fibrillée et tissu utilisant ladite fibre Download PDF

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Publication number
EP4092185A1
EP4092185A1 EP20913922.9A EP20913922A EP4092185A1 EP 4092185 A1 EP4092185 A1 EP 4092185A1 EP 20913922 A EP20913922 A EP 20913922A EP 4092185 A1 EP4092185 A1 EP 4092185A1
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EP
European Patent Office
Prior art keywords
treatment
fabric
dtex
regenerated cellulose
cellulose fibers
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EP20913922.9A
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German (de)
English (en)
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EP4092185A4 (fr
Inventor
Motoya MATSUBARA
Shogo JITSUMATSU
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Asahi Kasei Corp
Asahi Chemical Industry Co Ltd
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Asahi Kasei Corp
Asahi Chemical Industry Co Ltd
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Publication of EP4092185A1 publication Critical patent/EP4092185A1/fr
Publication of EP4092185A4 publication Critical patent/EP4092185A4/fr
Pending legal-status Critical Current

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    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D13/00—Woven fabrics characterised by the special disposition of the warp or weft threads, e.g. with curved weft threads, with discontinuous warp threads, with diagonal warp or weft
    • D03D13/008—Woven fabrics characterised by the special disposition of the warp or weft threads, e.g. with curved weft threads, with discontinuous warp threads, with diagonal warp or weft characterised by weave density or surface weight
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/02—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from solutions of cellulose in acids, bases or salts
    • D01F2/04—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from solutions of cellulose in acids, bases or salts from cuprammonium solutions
    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/20—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
    • D03D15/208—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads cellulose-based
    • D03D15/225—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads cellulose-based artificial, e.g. viscose
    • D—TEXTILES; PAPER
    • D03—WEAVING
    • D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/50—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the properties of the yarns or threads
    • D03D15/573—Tensile strength
    • 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
    • D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/188—Monocarboxylic acids; Anhydrides, halides or salts thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/20—Cellulose-derived artificial fibres
    • D10B2201/22—Cellulose-derived artificial fibres made from cellulose solutions

Definitions

  • the present invention relates to a fibrillated regenerated cellulose fiber having a characteristic surface texture, softness and a resilient feel, being fibrillated by rubbing and tanning treatment in a wetted state, and having an excellent surface texture after water washing and a long-lasting feel, thereby exhibiting high quality, as well as to a fabric including the fiber as constituent yarn.
  • Regenerated cellulose fibers include cuprammonium rayon and organic solvent-obtained cellulose fibers wherein the cellulose fibers all comprise aggregated fibrils composed mainly of cellulose microfibrils, and the fibers having a feature of splitting and becoming fibrillated in the fiber axis direction when subjected to rubbing or cloth kneading treatment in a wetted state.
  • a processing method involving fibrillation is disclosed in PTL 1, as a method using impact during raising treatment and dyeing with a jet dyeing machine.
  • the expression level of the fibrils is not constant, being dependent on the dyeing conditions including the dyeing time, the liquor to goods ratio, the fabric speed and the concentration of the alkali used, there is a disadvantage in that products of consistent quality cannot be provided in a repeatable manner, and furthermore the polymerization degree of the regenerated cellulose fibers is specified to be 400 or greater and shedding of fibrils by water washing is not mentioned.
  • PTL 2 discloses fibrillation using an aqueous alkali solution.
  • the polymerization degree of the regenerated cellulose fibers is specified to be 300 or greater, and since the treatment method is carried out in an aqueous alkali solution, the regenerated cellulose fibers are structurally modified to be easily fibrillated only in an aqueous alkali solution, while fibrillation is difficult by water washing with a weak degree of weak alkalinity, and furthermore, nothing is mentioned regarding shedding of the fibrils by water washing.
  • PTL 3 discloses a method using an aqueous acid solution or an aqueous oxidizing agent solution, but nothing is mentioned regarding the polymerization degree of the regenerated cellulose fibers.
  • the conditions for the treatment described in PTL 3 are compared to the conditions disclosed herein, while extended treatment is carried out at high temperature under ordinary pressure in a high-concentration acid solution with the aim of inhibiting reduction in strength, nothing is mentioned regarding the rate of strength reduction by the treatment method, and although it is stated that the strength is reduced by treatment under high pressure, the processing conditions are completely different from those disclosed in the present specification.
  • PTL 4 discloses a method using an aqueous acid solution, but nothing is mentioned regarding the polymerization degree of the regenerated cellulose fibers.
  • PTL 4 describes tumbling treatment with an acid water-soluble solution for 30 to 80 minutes aimed at strength reduction, in order to remove long fibrils, and high-speed tumbling treatment in a dry state.
  • the lyocell-containing fabric disclosed in PTL 4 has the long fibrils removed, which are responsible for producing a "hairy effect" on fabric surfaces as the characteristic surface texture that is disclosed in the present specification, while PTL 4 states that the short fibrils on the fabric surface have a characteristically "clean" surface finish, unlike a "hairy effect", and they are therefore different from the fibrillated regenerated cellulose fiber disclosed herein.
  • PTL 4 completely fails to indicate the rate of strength reduction of the fabric by the treatment method used to remove the long fibrils, and also mentions nothing regarding shedding of the fibrils by water washing.
  • the problem to be solved by the invention is to provide a fibrillated regenerated cellulose fiber having a characteristic surface texture, softness and resilient feel, being fibrillated by rubbing and tanning treatment in a wetted state, and having an excellent surface texture after water washing and a long-lasting feel, thereby exhibiting high quality, as well as a fabric using the fiber.
  • the present inventors Upon avid research with the goal of solving this problem, the present inventors have discovered that rather than modifying the expressed fibrils so that they are not shed it is more effective to modify them so that even if the fibrils are shed they are re-expressed during washing, and as a result of much further experimentation based on this discovery, studying methods of modification whereby even if the fibrils are shed they are re-expressed during washing, the present inventors have completed this invention upon finding, unexpectedly, that if the polymerization degree of regenerated cellulose fibers is controlled to 100 to 250, the fibrils can be easily expressed with only the weak rubbing effect of washing, and a lightweight feel, softness and a resilient feel are exhibited.
  • the present invention is as follows.
  • the fibrillated regenerated cellulose fibers of the invention are fibers that have a characteristic surface texture, softness and resilient feel, and that are also fibrillated by rubbing and tanning treatment in a wetted state and exhibit an excellent surface texture after water washing and a long-lasting feel, thereby exhibiting high quality.
  • One embodiment of the invention is regenerated cellulose fibers that are fibrillated on their surfaces, having a polymerization degree of 100 to 250, and a dry tensile strength of greater than 1.0 cN/dtex and 3.0 cN/dtex or lower.
  • Regenerated cellulose fibers are regenerated cellulose fibers spun from a molten cellulose starting material such as cuprammonium rayon or organic solvent-obtained cellulose fibers, and they are preferably cuprammonium rayon or organic solvent-obtained cellulose fibers, and more preferably organic solvent-obtained cellulose fibers.
  • the yarn form of the regenerated cellulose fibers may be staple fibers or long fibers, but long-fiber multifilament yarn is preferred.
  • the single fiber size is not particularly restricted but is preferably 0.5 to 5.0 dtex.
  • the total fineness is not particularly restricted but is preferably 22 to 330 dtex, and the yarn count is not particularly restricted but is preferably 5 to 100.
  • the monofilament cross-section shape is also not particularly restricted. There are likewise no particular restrictions on the state of twisting, which may be without twists, false-twisting or with twisting, or on the number of twists, which is preferably no more than 2000 added twists. Lack of twisting is preferred from the viewpoint of the tactile feel.
  • Combination with other materials is likewise not particularly restricted since this embodiment is not affected by other materials, but acryl, diacetate or wool is not preferred for such other combined materials since the processing method involves treatment under high pressure which can lead to strength reduction, hardened feel and loss of transparency.
  • the proportion of regenerated cellulose fibers used in a fabric that includes a woven or knitted fabric or nonwoven fabric is not particularly restricted, but in order to satisfactorily exhibit the desired effect it is preferably 10 wt% or greater, more preferably 20 wt% or greater and even more preferably 30 wt% or greater of the total weight of the fabric. If the amount used is 10 wt% or lower, fibrillation will be observed but it will be more difficult to obtain softness and a resilient feel.
  • the yarn combination method may be combined twisting, interlaced filament combination, Taslan filament combination, covering, cotton blending, worsted or woollen spinning or fine spun yarn doubling.
  • the fibrillated regenerated cellulose fibers according to this embodiment have a polymerization degree of 100 to 250, preferably 150 to 250 and more preferably 200 to 250. If the polymerization degree is less than 100 the dry tensile breaking strength will fall below 1.0 cN/dtex, and the physical properties necessary for post-treatment and for use as a clothing article will not be exhibited. However, a polymerization degree of higher than 250 is not preferred since re-expression of the fibrils by water washing will not be possible.
  • the polymerization degree is the value measured by the viscosity method using a copper-ammonia solution.
  • the fabric may be a woven fabric, warp knit fabric, circular knit fabric, horizontal knit fabric or nonwoven fabric, and is preferably a woven fabric, warp knit fabric, circular knit fabric or horizontal knit fabric, and more preferably a woven fabric or circular knit fabric.
  • the texture and density of the fabric are also not particularly restricted.
  • the method of combination with other materials may be mixed weaving, mixed knitting, composite yarn or insertion of weft yarn into warp yarn.
  • modifying treatment to adjust the polymerization degree of the fibrillated regenerated cellulose fiber of this embodiment to 100 to 250.
  • modifying treatment to adjust the polymerization degree to 100 to 250 and the dry tensile strength to greater than 1.0 cN/dtex and 3.0 cN/dtex or lower by treatment in an acid solution, since adjustment of the physical properties of the yarn and the polymerization degree will thus be facilitated.
  • the type of acid used is not particularly restricted and may be citric acid, malic acid, acetic acid, formic acid, sulfuric acid, nitric acid, hydrochloric acid or oxalic acid, preferred among which are acids with low corrosivity for metals, with formic acid, citric acid and malic acid being more preferred.
  • the treatment temperature is preferably 110°C to 150°C, more preferably 120°C to 150°C and even more preferably 130°C to 140°C, for modification to the desired polymerization degree and tensile strength.
  • a temperature range of lower than 110°C is not preferred because a longer treatment time will be necessary for modification and the tensile strength will be significantly reduced even with successful modification to the desired polymerization degree.
  • a short period treatment time at lower than 110°C is also not preferred because it requires a lower pH, and treatment for a short period at a low pH results in local reduction in polymerization degree and strength reduction making it difficult to achieve homogeneous modification, while variation in quality between different modifying treatments also occurs.
  • a temperature above 150°C or higher is also not preferred because temperature management becomes more difficult and homogeneous modification is more difficult to achieve.
  • the treatment pH and treatment time must be adjusted depending on the regenerated cellulose fibers used, but the treatment pH is preferably 2.6 to 3.4 and more preferably 2.8 to 3.2, while the treatment time is preferably 10 to 30 minutes, more preferably 12 to 28 minutes and even more preferably 15 to 25 minutes.
  • regenerated cellulose fibers having a polymerization degree of about 450 to 600 and a dry tensile strength of 2.0 cN/dtex or greater are treated using formic acid
  • 20 minutes of treatment at 130°C in an acid bath at pH 2.8 having a 76% formic acid concentration of 1.0 g/L can modify the polymerization degree to 100 to 250 and can maintain a dry tensile strength of greater than 1.0 cN/dtex and 3.0 cN/dtex or lower.
  • the form used in the modifying treatment is not particularly restricted, but it is preferably a yarn or fabric form, and more preferably a fabric form.
  • the equipment used for processing is not particularly restricted for either yarn or fabrics, but for yarn forms it is preferred to use a cheese dyeing machine or skein dyeing machine and for fabric forms it is preferred to use a jet dyeing machine, airflow dyeing machine, beam dyeing machine, jigger dyeing machine, paddle dyeing machine, drum dyeing machine, washer dyeing machine or winch dyeing machine, with a jet dyeing machine or airflow dyeing machine being preferred.
  • fibrillation treatment in water is necessary to express fibrils after modifying treatment, either the fibrillation treatment must be carried out simultaneously with the modifying treatment, or the fibrillation treatment must be carried out after modifying treatment.
  • the form used in the fibrillation treatment is not particularly restricted but is preferably a fabric form.
  • the equipment used for processing is not particularly restricted, but it is preferred to use a jet dyeing machine, airflow dyeing machine, paddle dyeing machine, drum dyeing machine, washer dyeing machine or winch dyeing machine, with a jet dyeing machine or airflow dyeing machine being preferred.
  • the fibrillation treatment in water is not particularly restricted, and examples of performed fibrillation treatment are with a jet dyeing machine, airflow dyeing machine or winch dyeing machine as the equipment, at a temperature of 10 to 130°C, a fabric speed of 100 m/min or greater and a treatment time of 20 minutes or longer, or paddle dyeing machine, drum dyeing machine or washer dyeing machine as the equipment, at a temperature of 10 to 130°C and a treatment time of 20 minutes or longer.
  • the regenerated cellulose fibers of this embodiment have a dry tensile strength of greater than 1.0 cN/dtex and 3.0 cN/dtex or lower, preferably 1.3 cN/dtex to 2.5 cN/dtex and more preferably 1.5 cN/dtex to 2.0 cN/dtex. If the dry tensile strength is 1.0 cN/dtex or lower, the fibers will suffer damage during the steps up until production of the fabric, making it difficult to obtain a practical fabric and impairing the resilient feel, while if it is greater than 3.0 cN/dtex the softness will be impaired.
  • fibrillated refers to a state in which aggregated fibrils composed mainly of cellulose microfibrils on the surfaces of the regenerated cellulose fibers are split in the fiber axis direction.
  • Fig. 1 is a photograph of the surface of a woven fabric, showing the fibrillated state of the regenerated cellulose fibers as the constituent yarn, with arrow 1 indicating a state where aggregated fibrils composed mainly of cellulose microfibrils are split in the fiber axis direction (a fibrillated state).
  • Fig. 2 is a magnified photograph of the fibrillated state of regenerated cellulose fibers, with arrow 2 indicating cellulose microfibrils.
  • Cellulose fiber samples with different polymerization degrees were each dissolved in a copper-ammonia solution as a molecular dispersion and the polymerization degree was measured based on the formula shown above in a Nakano viscosity tube, after which the viscosity of the fiber substance sample dissolved in a copper-ammonia solution at a fixed concentration in a Tappy viscosity tube was measured, the relationship between viscosity and polymerization degree was determined, the actual viscosity dissolved in a copper-ammonia solution at the same fixed concentration in a Tappy viscosity tube was measured, and the polymerization degree was calculated from a prepared relationship table for viscosity and polymerization degree.
  • the method of measuring the viscosity with a Tappy viscosity tube is as follows.
  • the sample is allowed to stand for 24 hours or longer in a constant temperature and humidity room at 20°C, 65% humidity for equilibration of the moisture content.
  • a 0.1 g portion of the sample is weighed out.
  • the viscosity tube is set in a rotating device and rotated for 30 minutes at a speed of 3 rpm to dissolve the sample.
  • the viscosity tube is removed from the rotating device and immersed for 5 minutes in a thermobath at 20°C.
  • the lower plug of the viscosity tube is removed and set in a thermobath, inserting the whole into a jacket.
  • the plug cock at the top of the viscosity tube is opened and the time for flow of the solution between gauge marks A and B of the viscometer is measured.
  • the value calculated for the absolute viscosity is then compared with the aforementioned relationship table for viscosity and polymerization degree, to determine the polymerization degree.
  • the sample was allowed to stand for 24 hours or longer in a constant temperature and humidity room at 20°C, 65% humidity for equilibration of the moisture content.
  • a TENSILON RTC Series universal material tester product of A&D Co., Ltd.
  • the sample was stretched to a sample length (yarn length) of 200 mm at a pull speed of 200 mm/min, and the breaking strength was recorded.
  • the sample is set in a VHX-6000 microscope (product of Keyence Corp.), and with the magnification of a VH-Z20 lens (product of Keyence Corp.) set to 200x and the luminance and sensitivity adjusted, the sample is both irradiated and photographed with light that produces white dots on the fibril portions.
  • the proportion of white dot area with respect to photographed area was calculated and the degree of fibrillation was evaluated based on the following 3-level evaluation scale.
  • the sample both before washing and after washing, is set in a VHX-6000 microscope (product of Keyence Corp.), and with the magnification of a VH-Z20 lens (product of Keyence Corp.) set to 200x and the luminance and sensitivity adjusted, the sample is both irradiated and photographed with light that produces white dots on the fibril portions.
  • the sample before washing was examined for feel by a tactile sensory test with repeated gripping and evaluated based on the following 3-level evaluation scale, also evaluating the sample after washing when the evaluation of the sample before washing was G or F.
  • An 84 dtex/45 cuprammonium rayon filament was prepared with a polymerization degree of 580 and a dry tensile strength of 2.3 cN/dtex.
  • the raw yarn was subjected to modifying treatment with a cheese dyeing machine at 130°C for 20 minutes using 76% formic acid at 1.0 g/L, to convert the polymerization degree to 200 and obtain modified cuprammonium rayon.
  • the obtained modified cuprammonium rayon raw yarn was used as warp yarn and weft yarn for weaving of a 2/1 twill weave fabric, having a warp density of 144/2.54 cm and a weft density of 100/2.54 cm.
  • the obtained greige was subjected to scouring relaxation and fibrillation treatment at 80°C for 20 minutes with a jet dyeing machine using 1 g/L of nonionic surfactant, after which dyeing of the cuprammonium rayon was again carried out for 60 minutes with a jet dyeing machine at a dyeing temperature of 60°C, followed by soaping for 10 minutes at 80°C.
  • the fabric was impregnated with a 1 wt% aqueous silicon-based softener solution, padded with a pickup of 80%, dried for 1 minute at 150°C, subjected to texture treatment with an air tumbler for 30 minutes at 80°C at a speed of 700 m/min, and provided for final setting at 130°C for 1 minute to obtain a dyed fabric with a warp density of 153/2.54 cm and a weft density of 104/2.54 cm.
  • the polymerization degree of the 84 dtex/45 filament cuprammonium rayon of warp yarn removed from the woven fabric was 200.
  • An 84 dtex/45 cuprammonium rayon filament with a polymerization degree of 580 and a dry tensile strength of 2.3 cN/dtex was used as warp yarn and weft yarn for weaving of a 2/1 twill weave fabric, having a warp density of 144/2.54 cm and a weft density of 100/2.54 cm.
  • the obtained greige was subjected to modifying and fibrillation treatment for 20 minutes with a jet dyeing machine at 130°C using 1.0 g/L of 76% formic acid, to adjust the polymerization degree to 200, after which dyeing of the cuprammonium rayon was again carried out for 60 minutes with a jet dyeing machine at a dyeing temperature of 60°C, followed by soaping for 10 minutes at 80°C.
  • the fabric was impregnated with a 1 wt% aqueous silicon-based softener solution, padded with a pickup of 80%, dried for 1 minute at 150°C, subjected to texture treatment with an air tumbler for 30 minutes at 80°C at a speed of 700 m/min, and provided for final setting at 130°C for 1 minute to obtain a dyed fabric with a warp density of 153/2.54 cm and a weft density of 104/2.54 cm.
  • the polymerization degree of an 84 dtex/45 cuprammonium rayon filament of warp yarn removed from the woven fabric was 200.
  • An 89 dtex/30 organic solvent-obtained cellulose fiber filament was prepared with a polymerization degree of 490 and a dry tensile strength of 3.5 cN/dtex.
  • the raw yarn was subjected to modifying treatment with a cheese dyeing machine at 130°C for 20 minutes using 76% formic acid at 1.0 g/L, to convert the polymerization degree to 220 and obtain modified organic solvent-obtained cellulose fibers.
  • the obtained modified organic solvent-obtained cellulose fibers were used as warp yarn and weft yarn for weaving of a plain woven fabric having a warp density of 105/2.54 cm and a weft density of 89/2.54 cm.
  • the obtained greige was subjected to scouring relaxation and fibrillation treatment for 20 minutes with a jet dyeing machine using 1 g/L of nonionic surfactant at 80°C, after which dyeing of the organic solvent-obtained cellulose fibers was again carried out for 60 minutes with a jet dyeing machine at a dyeing temperature of 60°C, followed by soaping for 10 minutes at 80°C.
  • the fabric was impregnated with a 1 wt% aqueous silicon-based softener solution, padded with a pickup of 80%, dried for 1 minute at 150°C, subjected to texture treatment with an air tumbler for 30 minutes at 80°C at a speed of 700 m/min, and provided for final setting at 130°C for 1 minute to obtain a dyed fabric with a warp density of 109/2.54 cm and a weft density of 92/2.54 cm.
  • the polymerization degree of the 89 dtex/30 filament organic solvent-obtained cellulose fibers of warp yarn removed from the woven fabric was 220.
  • the 89 dtex/30 filament organic solvent-obtained cellulose fibers with a polymerization degree of 490 and a dry tensile strength of 3.5 cN/dtex were used as warp yarn and weft yarn for weaving of a plain woven fabric having a warp density of 105/2.54 cm and a weft density of 89/2.54 cm.
  • the obtained greige was subjected to modifying and fibrillation treatment for 20 minutes with a jet dyeing machine at 130°C using 1.0 g/L of 76% formic acid, to adjust the polymerization degree to 220, after which dyeing of the organic solvent-obtained cellulose fibers was again carried out for 60 minutes with a jet dyeing machine at a dyeing temperature of 60°C, followed by soaping for 10 minutes at 80°C.
  • the fabric was impregnated with a 1 wt% aqueous silicon-based softener solution, padded with a pickup of 80%, dried for 1 minute at 150°C, subjected to texture treatment with an air tumbler for 30 minutes at 80°C at a speed of 700 m/min, and provided for final setting at 130°C for 1 minute to obtain a dyed fabric with a warp density of 109/2.54 cm and a weft density of 92/2.54 cm.
  • the polymerization degree of the 89 dtex/30 filament organic solvent-obtained cellulose fibers of warp yarn removed from the woven fabric was 220.
  • An 84 dtex/45 cuprammonium rayon filament with a polymerization degree of 580 and a dry tensile strength of 2.3 cN/dtex was used as warp yarn and weft yarn for weaving of a 2/1 twill weave fabric, having a warp density of 144/2.54 cm and a weft density of 100/2.54 cm.
  • the obtained greige was dye finished in the same manner as Example 2, except that modifying treatment and fibrillation treatment were not carried out, to obtain a dyed fabric having a warp density of 153/2.54 cm and a weft density of 104/2.54 cm.
  • the polymerization degree of an 84 dtex/45 cuprammonium rayon filament of warp yarn removed from the woven fabric was 580.
  • the 89 dtex/30 filament organic solvent-obtained cellulose fibers with a polymerization degree of 490 and a dry tensile strength of 3.5 cN/dtex were used as warp yarn and weft yarn for weaving of a plain woven fabric having a warp density of 109/2.54 cm and a weft density of 92/2.54 cm.
  • the obtained greige was dye finished in the same manner as Example 4, except that modifying and fibrillation treatment were not carried out, to obtain a dyed fabric having a warp density of 109/2.54 cm and a weft density of 92/2.54 cm.
  • the polymerization degree of the 89 dtex/30 filament organic solvent-obtained cellulose fibers of warp yarn removed from the woven fabric was 490.
  • An 84 dtex/45 cuprammonium rayon filament with a polymerization degree of 580 and a dry tensile strength of 2.3 cN/dtex was used as warp yarn and weft yarn for weaving of a 2/1 twill weave fabric, having a warp density of 144/2.54 cm and a weft density of 100/2.54 cm.
  • the obtained greige was subjected to fibrillation treatment for 120 minutes with a jet dyeing machine using 40 g/L of sodium hydroxide at 80°C, after which dyeing of the cuprammonium rayon was again carried out for 60 minutes with a jet dyeing machine at a dyeing temperature of 60°C, followed by soaping for 10 minutes at 80°C.
  • the fabric was impregnated with a 1 wt% aqueous silicon-based softener solution, padded with a pickup of 80%, dried for 1 minute at 150°C, subjected to texture treatment with an air tumbler for 30 minutes at 80°C at a speed of 700 m/min, and provided for final setting at 130°C for 1 minute to obtain a dyed fabric with a warp density of 153/2.54 cm and a weft density of 104/2.54 cm.
  • the polymerization degree of an 84 dtex/45 cuprammonium rayon filament of warp yarn removed from the woven fabric was 440.
  • An 84 dtex/45 cuprammonium rayon filament with a polymerization degree of 580 and a dry tensile strength of 2.3 cN/dtex was used as warp yarn and weft yarn for weaving of a 2/1 twill weave fabric, having a warp density of 144/2.54 cm and a weft density of 100/2.54 cm.
  • the obtained greige was subjected to fibrillation treatment for 60 minutes with a jet dyeing machine using 50 g/L of 75% phosphoric acid at 100°C, after which dyeing of the cuprammonium rayon was again carried out for 60 minutes with a jet dyeing machine at a dyeing temperature of 60°C, followed by soaping for 10 minutes at 80°C.
  • the fabric was impregnated with a 1 wt% aqueous silicon-based softener solution, padded with a pickup of 80%, dried for 1 minute at 150°C, subjected to texture treatment with an air tumbler for 30 minutes at 80°C at a speed of 700 m/min, and provided for final setting at 130°C for 1 minute to obtain a dyed fabric with a warp density of 153/2.54 cm and a weft density of 104/2.54 cm.
  • the polymerization degree of an 84 dtex/45 cuprammonium rayon filament of warp yarn removed from the woven fabric was 400.
  • An 84 dtex/45 cuprammonium rayon filament with a polymerization degree of 580 and a dry tensile strength of 2.3 cN/dtex was used as warp yarn and weft yarn for weaving of a 2/1 twill weave fabric, having a warp density of 144/2.54 cm and a weft density of 100/2.54 cm.
  • the obtained greige was subjected to fibrillation treatment for 60 minutes with a jet dyeing machine using 30 g/L of aqueous 35% hydrogen peroxide at 100°C, after which dyeing of the cuprammonium rayon was again carried out for 60 minutes with a jet dyeing machine at a dyeing temperature of 60°C, followed by soaping for 10 minutes at 80°C.
  • the fabric was impregnated with a 1 wt% aqueous silicon-based softener solution, padded with a pickup of 80%, dried for 1 minute at 150°C, subjected to texture treatment with an air tumbler for 30 minutes at 80°C at a speed of 700 m/min, and provided for final setting at 130°C for 1 minute to obtain a dyed fabric with a warp density of 153/2.54 cm and a weft density of 104/2.54 cm.
  • the polymerization degree of an 84 dtex/45 cuprammonium rayon filament of warp yarn removed from the woven fabric was 180.
  • An 84 dtex/45 cuprammonium rayon filament with a polymerization degree of 580 and a dry tensile strength of 2.3 cN/dtex was used as warp yarn and weft yarn for weaving of a 2/1 twill weave fabric, having a warp density of 144/2.54 cm and a weft density of 100/2.54 cm.
  • the obtained greige was subjected to fibrillation treatment for 45 minutes with an airflow dyeing machine at 130°C using 6.4 g/L of acetic acid, after which dyeing of the cuprammonium rayon was again carried out for 360 minutes with an airflow dyeing machine at a dyeing temperature of 60°C, followed by soaping for 10 minutes at 80°C.
  • the fabric was impregnated with a 1 wt% aqueous silicon-based softener solution, padded with a pickup of 80%, dried for 1 minute at 150°C, subjected to texture treatment with an air tumbler for 30 minutes at 100°C at a speed of 900 m/min, and provided for final setting at 130°C for 1 minute to obtain a dyed fabric with a warp density of 153/2.54 cm and a weft density of 104/2.54 cm.
  • the polymerization degree of an 84 dtex/45 cuprammonium rayon filament of warp yarn removed from the woven fabric was 190.
  • Table 1 shows the sample yarn materials, modifying treatment and fibril treatment used in Examples 1 to 4 and Comparative Examples 1 to 6, and the evaluation results are shown in Table 2.
  • Sample yarn Modifying treatment Fibrillation treatment Treatment form Treatment solution Treatment pH Treatment time Treatment temperature Treatment solution Treatment time Treatment temperature Present invention
  • Example 1 Cuprammonium rayon Yarn 1.0 g/L 76% Formic acid 2.8 20 minutes 130°C In water 20 min 80°C
  • Example 2 Cuprammonium rayon Fabric 1.0 g/L 76% Formic acid 2.8 20 minutes 130°C No treatment No treatment No treatment
  • Example 3 Organic solvent-obtained cellulose fibers Yarn 1.0 g/L 76% Formic acid 2.8 20 minutes 130°C In water 20 min 80°C
  • Organic solvent-obtained cellulose fibers Fabric 1.0 g/L 76% Formic acid 2.8 20 minutes 130°C No treatment Prior art Comp.
  • Example 1 Cuprammonium rayon Fabric No treatment No treatment No treatment No treatment In water 20 min 80°C Comp.
  • Example 2 Organic solvent-obtained cellulose fibers Fabric No treatment No treatment No treatment No treatment In water 20 min 80°C Comp.
  • Example 3 Cuprammonium rayon Fabric No treatment No treatment No treatment No treatment 40 g/L Sodium hydroxide 120 min 80°C Comp.
  • Example 4 Cuprammonium rayon Fabric No treatment No treatment No treatment 50 g/L 75% phosphoric acid 60 min 100°C Comp.
  • Example 5 Cuprammonium rayon Fabric No treatment No treatment No treatment No treatment No treatment 30 g/L 35% Hydrogen peroxide solution 60 min 100°C Comp.
  • Example 6 Cuprammonium rayon Fabric No treatment No treatment No treatment No treatment 6.4 g/L Acetic acid 45 min 130°C [Table 2] Polymerization degree Performance Fibrillation degree before washing Change in fibrillation degree before and after washing Feel Tensile strength Before washing After washing Present invention
  • Example 1 200 G G G 1.5 cN/dtex
  • Example 2 200 G G G 1.5 cN/dtex
  • Example 3 220 G G G G 1.8 cN/dtex
  • Example 4 220 G G G G G 1.8 cN/dtex Prior art Comp.
  • Example 2 490 P P P - 3.7 cN/dtex Comp.
  • Example 3 440 G P G F 1.4 cN/dtex Comp.
  • Example 4 400 G P G P 1.2 cN/dtex Comp.
  • Example 5 180 G G P - 0.2 cN/dtex Comp.
  • Example 6 190 P P P P - 1.0 c
  • the fabrics using the modified cellulose fibers of Examples 1 to 4 had satisfactory textures that were soft and resilient with no change in fibril feel by washing, and the tensile strengths were shown to be greater than 1.0 cN/dtex.
  • Examples 1 to 4 had characteristic surface texture, softness and resilient feel after washing, and excellent persistence of surface texture and feel even after washing.
  • the fabrics of Comparative Examples 1 to 6 had tensile strengths of 1.0 cN/dtex or lower, or had loss of fibrils at the stage before washing, or had a polymerization degree of greater than 250 and change in fibrillation degree due to shedding of fibrils after washing.
  • the change in surface texture or feel after washing was large, or strength as a fabric failed to be maintained, with holes being opened by friction during wear or washing, or the fibrils were removed at the stage before washing, making the fabric unsuitable as a fiber product with fibrils which must exhibit satisfactory texture.
  • the present invention can provide regenerated cellulose fibers having a characteristic surface texture, softness and resilient feel, being easily fibrillated by rubbing and tanning treatment in a wetted state, and having an excellent surface texture after water washing and a long-lasting feel, thereby exhibiting high quality, as well as a fabric using the fibers, and the invention therefore has industrial applicability.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
EP20913922.9A 2020-01-14 2020-01-14 Fibre de cellulose régénérée fibrillée et tissu utilisant ladite fibre Pending EP4092185A4 (fr)

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NL246561A (fr) * 1958-12-31
GB9103297D0 (en) * 1991-02-15 1991-04-03 Courtaulds Plc Fibre production method
JP3269143B2 (ja) 1992-11-27 2002-03-25 東洋紡績株式会社 風合いに優れた複合繊維織編物およびその製造方法
JP3267746B2 (ja) * 1993-06-07 2002-03-25 東洋紡績株式会社 複合繊維織編物の製造方法
GB9412500D0 (en) * 1994-06-22 1994-08-10 Courtaulds Fibres Holdings Ltd Fibre manufacture
GB9412501D0 (en) * 1994-06-22 1994-08-10 Courtaulds Fibres Holdings Ltd Manufacture of fibre
JPH08113846A (ja) 1994-08-22 1996-05-07 Toyobo Co Ltd 張り、腰及びソフト風合いに優れた布帛及びその製造法
JP3578227B2 (ja) * 1994-10-17 2004-10-20 東洋紡績株式会社 易フィブリル化ポリノジック繊維及びその製造方法
JP3611350B2 (ja) * 1994-11-09 2005-01-19 旭化成せんい株式会社 色見栄えに優れた丸編物
JPH08291481A (ja) * 1995-04-18 1996-11-05 Toyobo Co Ltd 再生セルロース系繊維を含む複合繊維織編物の染色加工方法
JPH11315474A (ja) * 1998-04-28 1999-11-16 Unitika Ltd 溶剤紡糸セルロース繊維含有布帛のフィブリル化加工方法
GB2399094A (en) 2003-03-04 2004-09-08 Tencel Ltd Treatment of lyocell containing fibres/fabrics with aqueous carboxylic acid at above atmospheric pressure & elevated temperature, prior to dyeing & tumbling
AT515693B1 (de) * 2014-10-29 2015-11-15 Chemiefaser Lenzing Ag Schnell fibrillierende Lyocellfasern und deren Verwendung
JP6505060B2 (ja) 2016-09-23 2019-04-24 山佐株式会社 遊技機
EP3536851A1 (fr) * 2018-03-06 2019-09-11 Lenzing Aktiengesellschaft Fibre lyocell présentant une tendance accrue à la fibrillation

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CN114929962A (zh) 2022-08-19

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