US20180119311A1 - Acrylic fiber and method for manufacturing same - Google Patents

Acrylic fiber and method for manufacturing same Download PDF

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Publication number
US20180119311A1
US20180119311A1 US15/851,119 US201715851119A US2018119311A1 US 20180119311 A1 US20180119311 A1 US 20180119311A1 US 201715851119 A US201715851119 A US 201715851119A US 2018119311 A1 US2018119311 A1 US 2018119311A1
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Prior art keywords
acrylic fiber
acrylic
mass
fibers
water
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US15/851,119
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English (en)
Inventor
Ryohei Noishiki
Masanobu Tamura
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Kaneka Corp
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Kaneka Corp
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    • 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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/18—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of unsaturated nitriles, e.g. polyacrylonitrile, polyvinylidene cyanide
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/06—Washing or drying
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/06—Wet spinning methods
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/12—Stretch-spinning methods
    • D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
    • 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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/40—Modacrylic fibres, i.e. containing 35 to 85% acrylonitrile

Definitions

  • One or more embodiments of the present invention relate to acrylic fibers composed of acrylic polymers, and a method for producing the same.
  • Acrylic fibers are generally produced by wet spinning or dry-wet spinning in which a spinning solution that is obtained by dissolving an acrylic polymer in an organic solvent is discharged from a spinning nozzle into a coagulation bath to form fibers.
  • a spinning solution that is obtained by dissolving an acrylic polymer in an organic solvent
  • the spinning solution after the spinning solution has been discharged from the spinning nozzle and coagulated in the coagulation bath, if coagulated yarns (fibers) in a wet state due to the organic solvent, etc., in the spinning solution are directly and immediately dried, the fibers adhere to one another.
  • a washing step is generally performed in a water bath before drying to remove the organic solvent in the fibers.
  • Patent Document 1 discloses that wet spun acrylic fibers are washed in a water bath at high temperature before drying to remove the organic solvent.
  • pressing of fibers with nip rolls is commonly performed before sending the fibers from a bath liquid of a coagulation bath, water bath, or the like, to the next step, so as to reduce an amount of the bath liquid to be sent to the next step.
  • Patent Document 1 JP 2004-346447A
  • the present invention provides acrylic fibers with less cross-sectional collapse and high surface smoothness, and a production method of acrylic fibers that can improve the surface smoothness of acrylic fibers while reducing the cross-sectional collapse of acrylic fibers in the production of acrylic fibers by wet spinning or dry-wet spinning.
  • One or more embodiments of the present invention relate to an acrylic fiber composed of an acrylic polymer containing acrylonitrile.
  • the acrylic fiber has a deformation degree of 0.13 or less and a surface roughness of 6000 ⁇ m 2 or less.
  • One or more embodiments of the present invention also relate to a method for producing an acrylic fiber by wet spinning or dry-wet spinning using a spinning solution in which an acrylic polymer containing acrylonitrile is dissolved in an organic solvent.
  • the method includes at least a coagulation step, a water washing step, and a drying step.
  • the acrylic fiber that has been pressed with a nip roll is subjected to predrying before the drying step, using a dryer into which steam is fed.
  • the method for producing an acrylic fiber further includes a bath drawing step of drawing the acrylic fiber in a drawing bath before or after the water washing step.
  • the water washing step is performed by spraying water on the acrylic fiber and pressing with the nip roll the acrylic fiber on which water has been sprayed.
  • the predrying is performed at a dry-bulb temperature of 100 to 160° C. and a wet-bulb temperature of 60 to 100° C.
  • the organic solvent in the spinning solution is at least one selected from the group consisting of dimethyl sulfoxide, dimethylacetamide, and N,N-dimethylformamide.
  • the coagulation step is performed using a coagulation bath including at least one organic solvent selected from the group consisting of dimethyl sulfoxide, dimethylacetamide, and N,N-dimethylformamide.
  • the acrylic polymer includes acrylonitrile in an amount of 20 to 85 mass %, halogen-containing vinyl and/or halogen-containing vinylidene in an amount of 15 to 80 mass %, and a sulfonic acid group-containing monomer in an amount of 0 to 10 mass % with respect to the total mass of the acrylic polymer. In one or more embodiments, the acrylic polymer has a specific viscosity of 0.1 to 0.3.
  • acrylic fiber has a single fiber fineness of 10 to 100 dtex.
  • One or more embodiments of the present invention provide acrylic fibers that are composed of acrylic polymers containing acrylonitrile, and that have less cross-sectional collapse and high surface smoothness.
  • One or more embodiments of the production method of acrylic fibers of the present invention can improve the surface smoothness of acrylic fibers while reducing the cross-sectional collapse of acrylic fibers in the production of acrylic fibers by wet spinning or dry-wet spinning.
  • FIG. 1 is a schematic cross-sectional view of a washing device used in examples of the present invention.
  • FIG. 2A is a schematic cross-sectional view for explaining a nip pressure applied by nip rolls
  • FIG. 2B is a schematic surface view for explaining the same.
  • FIGS. 3A to 3D are schematic views for explaining a method for measuring the deformation degree of fibers.
  • FIG. 4 is a photograph showing the cross sections of acrylic fibers of Example 1 (400 ⁇ magnification).
  • FIG. 5 is a photograph showing the cross sections of acrylic fibers of Comparative Example 1 (400 ⁇ magnification).
  • the present inventors repeatedly examined ways to reduce the cross-sectional collapse of acrylic fibers occurring when acrylic fibers in a wet state before drying are pressed with nip rolls in wet spinning or dry-wet spinning.
  • the cross-sectional collapse can be reduced by subjecting acrylic fibers that have been pressed with nip rolls in any of the stages before a drying step to predrying in a dryer into which steam is fed and thereafter drying the predried fibers.
  • the reason for this is considered as follows. By subjecting acrylic fibers in a wet state whose cross sections collapse due to pressing with nip rolls to predrying in a dryer into which steam is fed, the cross-sectional collapse recovers. It was also found that there is a tendency for the fiber surfaces to smoothen by subjecting the acrylic fibers to predrying using a dryer into which steam is fed and then proceeding to a drying step.
  • the acrylic fibers of one or more embodiments of the present invention have a deformation degree of 0.13 or less and a surface roughness of 6000 ⁇ m 2 or less. Within these ranges, the cross-sectional collapse is reduced and the surface smoothness is improved.
  • the deformation degree of the fibers can be measured and calculated in the manner described below.
  • the deformation degree is an index indicating the degree of the cross-sectional collapse.
  • the deformation degree increases, the number of fibers with different cross-sectional shapes increases, and the fiber bundle includes more fibers with cross-sectional collapse.
  • the fiber bundle includes fewer fibers with cross-sectional collapse.
  • the present inventors found that, in the case of using the acrylic fibers as artificial hair, a hackling loss rate decreases in keeping with the deformation degree. Specifically, the hackling loss rate can be reduced to 5% or less by controlling the deformation degree to be 0.13 or less.
  • the deformation degree of the acrylic fibers is 0.13 or less, or 0.12 or less, or 0.115 or less, from the viewpoint of improving hackling properties. Moreover, if the cross-sectional shapes of the fibers are excessively uniform, the acrylic fibers are unnatural as artificial hair. From this viewpoint, it may be preferred that the deformation degree be in a range from 0.05 to 0.13 in products that are important to have good appearance.
  • the surface roughness of the fibers can be measured and calculated in the manner described below.
  • the surface roughness is an index indicating the degree of the smoothness of the fiber surfaces.
  • the fiber surface is smoother as the surface roughness is lower.
  • the present inventors found that, in the case of using the acrylic fibers as artificial hair, the hackling loss rate decreases in keeping with the surface roughness. Specifically, the hackling loss rate can be reduced to 5% or less by controlling the surface roughness to be 6000 ⁇ m 2 or less.
  • the surface roughness of the acrylic fibers is 6000 ⁇ m 2 or less, or 5800 ⁇ m 2 or less, or 5500 ⁇ m 2 or less, from the viewpoint of improving hackling properties.
  • the surface roughness is less than 3500 ⁇ m 2 , the fiber surfaces are too smooth, and the grip feeling of the acrylic fibers as artificial hair products in the case of using the fibers as artificial hair products becomes too high. From this viewpoint, it may be preferred that the surface roughness be in a range from 3500 to 6000 ⁇ m 2 in products that are important to have natural touch.
  • the acrylic polymer may be a homopolymer of acrylonitrile, or may be a copolymer of acrylonitrile and another copolymerizable monomer. Any monomer that is copolymerizable with acrylonitrile can be used as the other copolymerizable monomer.
  • vinyl compounds such as vinyl halides exemplified by vinyl chloride, vinyl bromide, and the like; vinylidene halides exemplified by vinylidene chloride, vinylidene bromide, and the like; unsaturated carboxylic acids exemplified by acrylic acid and methacrylic acid as well as their salts; methacrylic acid esters exemplified by methyl methacrylate; unsaturated carboxylic acid esters exemplified by glycidyl methacrylate and the like; and vinyl esters exemplified by vinyl acetate and vinyl butyrate.
  • vinyl halides exemplified by vinyl chloride, vinyl bromide, and the like
  • vinylidene halides exemplified by vinylidene chloride, vinylidene bromide, and the like
  • unsaturated carboxylic acids exemplified by acrylic acid and methacrylic acid as well as their salts
  • methacrylic acid esters exemp
  • a sulfonic acid group-containing monomer may also be used as the other copolymerizable monomer.
  • the sulfonic acid group-containing monomer allyl sulfonic add, methallyl sulfonic add, styrene sulfonic acid, isoprene sulfonic acid, 2-acrylamide-2-methylpropane sulfonic acid, as well as metallic salts, such as sodium salts, and amine salts thereof can be used.
  • These other copolymerizable monomers can be used alone or in combination of two or more.
  • the acrylic polymer contains acrylonitrile in an amount of 20 to 85 mass %, halogen-containing vinyl and/or halogen-containing vinylidene in an amount of 15 to 80 mass %, and a sulfonic acid group-containing monomer in an amount of 0 to 10 mass % with respect to the total mass of the acrylic polymer.
  • the content of the acrylonitrile in the acrylic polymer is 20 to 85 mass %, heat resistance improves, and the processing temperature for curling of the acrylic fibers can be set appropriately in the case of using the fibers as artificial hair.
  • the content of the halogen-containing vinyl and/or halogen-containing vinylidene in the acrylic polymer is 15 to 80 mass %, flame resistance improves.
  • the acrylic polymer contains acrylonitrile in an amount of 30 to 70 mass %, halogen-containing vinyl and/or halogen-containing vinylidene in an amount of 30 to 70 mass %, and a sulfonic acid group-containing monomer in an amount of 0 to 10 mass %.
  • the acrylic polymer in terms of hydrophilicity, contains acrylonitrile in an amount of 20 to 85 mass %, halogen-containing vinyl and/or halogen-containing vinylidene in an amount of 14.5 to 79.5 mass %, and a sulfonic acid group-containing monomer in an amount of 0.5 to 10 mass %, or contains acrylonitrile in an amount of 20 to 80 mass %, halogen-containing vinyl and/or halogen-containing vinylidene in an amount of 19.5 to 79.5 mass %, and a sulfonic acid group-containing monomer in an amount of 0.5 to 5 mass %, or contains acrylonitrile in an amount of 20 to 75 mass %, halogen-containing vinyl and/or halogen-containing vinylidene in an amount of 24.5 to 79.5 mass %, and a sulfonic acid group-containing monomer in an amount of 0.5 to 5 mass %, with respect to the total mass of the acrylic polymer.
  • the acrylic polymer has a specific viscosity of 0.1 to 0.3, or 0.15 to 0.25, from the viewpoint of easy dissolution in organic solvents.
  • 2 g of an acrylic polymer is dissolved in 1 L of dimethylformamide, and the specific viscosity of the obtained polymer solution is measured at 30° C. with an Ostwald viscometer to determine the specific viscosity of the acrylic polymer.
  • the acrylic fibers have a single fiber fineness of 10 to 100 dtex, or 20 to 90 dtex, or 30 to 85 dtex, or 40 to 80 dtex, or 45 to 70 dtex, from the viewpoint of suitable use as artificial hair.
  • the acrylic fibers can be produced by wet spinning or dry-wet spinning using the above-described spinning solution in which an acrylic polymer is dissolved in an organic solvent.
  • the spinning solution contains the acrylic polymer in an amount of 15 to 40 mass %, the organic solvent in an amount of 60 to 85 mass %, and water in an amount of 0 to 10 mass %, or contains the acrylic polymer in an amount of 20 to 35 mass %, the organic solvent in an amount of 65 to 80 mass %, and water in an amount of 0 to 10 mass % with respect to the total mass of the spinning solution, from the viewpoint of spinning stability.
  • the spinning solution contains the acrylic polymer in an amount of 20 to 30 mass %, the organic solvent (e.g., dimethyl sulfoxide) in an amount of 65.2 to 78.5 mass %, and water in an amount of 1.5 to 4.8 mass %, or contains the acrylic polymer in an amount of 22 to 30 mass %, the organic solvent in an amount of 66 to 76 mass %, and water in an amount of 2 to 4 mass %, or contains the acrylic polymer in an amount of 25 to 30 mass %, the organic solvent in an amount of 66.5 to 72.5 mass %, and water in an amount of 2.5 to 3.5 mass % with respect to the total mass of the spinning solution, from the viewpoint of improving hackling properties in the case of using the acrylic fibers as artificial hair.
  • the organic solvent e.g., dimethyl sulfoxide
  • the spinning solution may contain other additives for improving fiber properties as needed.
  • the additives include gloss adjusting agents such as titanium dioxide, silicon dioxide, esters and ethers of cellulose derivatives including cellulose acetate, coloring agents such as organic pigments, inorganic pigments, and dyes, and stabilizers for improving light resistance and heat resistance.
  • the acrylic fibers can be produced in the same procedure as that of general wet spinning or dry-wet spinning, except that acrylic fibers that have been pressed with nip rolls are subjected to predrying before the drying step, using a dryer into which steam is fed.
  • the production method of the acrylic fibers includes at least a coagulation step, a water washing step, and a drying step.
  • the method includes a bath drawing step before or after the water washing step.
  • the method may include a finishing oil application step before the drying step, and a drawing step and a thermal relaxation treatment step after the drying step.
  • the spinning solution is discharged into a coagulation bath containing an aqueous solution of an organic solvent directly or via a spinning nozzle to coagulate the spinning solution, and thus fibers are formed.
  • the coagulation bath is preferably a mixed solution of water and an organic solvent, from the viewpoint of easy control of the coagulation state.
  • the coagulation bath is an aqueous solution of an organic solvent that contains an organic solvent in an amount of 20 to 75 mass % and water in an amount of 25 to 80 mass %, or an aqueous solution of an organic solvent that contains an organic solvent in an amount of 30 to 70 mass % and water in an amount of 30 to 70 mass %, or an aqueous solution of an organic solvent that contains an organic solvent in an amount of 40 to 70 mass % and water in an amount of 30 to 60 mass %, with respect to the total mass of the coagulation bath.
  • the temperature of the coagulation bath may be, e.g., 5 to 40° C. If the concentration of the solvent in the coagulation bath is excessively low, coagulation proceeds fast, which tends to create a rough coagulation structure and form voids inside fibers.
  • any good solvents for the acrylic polymer can be used as the organic solvent in the spinning solution and the organic solvent in the coagulation bath.
  • the organic solvents are at least one selected from the group consisting of dimethyl sulfoxide (DMSO), dimethylacetamide (DMAc), and N,N-dimethylformamide (DMF) for the viewpoint of productivity, and may be dimethyl sulfoxide from the viewpoint of safety.
  • the organic solvent in the spinning solution and the organic solvent in the coagulation bath are the same, from the viewpoints of the quality of the acrylic fibers and the ease of process control.
  • the acrylic fibers are drawn in a drawing bath.
  • the drawing bath may be a water bath or an aqueous solution of an organic solvent having a lower organic solvent concentration than the coagulation bath.
  • the temperature of the drawing bath is 30° C. or more, or 40° C. or more, or 50° C. or more.
  • the organic solvent in the drawing bath is the same as the organic solvent in the coagulation bath.
  • the drawing ratio is not particularly limited, but the drawing ratio may be 2 to 8 times, or 2 to 7 times, or 2 to 6 times, from the viewpoint of enhancing the fiber strength and productivity.
  • the acrylic fibers (coagulated yarns or drawn yarns) are washed with water to remove the organic solvent.
  • the water washing step can be performed by soaking the acrylic fibers in a water bath and then pressing the fibers with nip rolls, or spraying water on the acrylic fibers and pressing with nip rolls the acrylic fibers on which water has been sprayed.
  • the water washing step is performed by spraying water on the acrylic fibers and pressing with nip rolls the acrylic fibers on which water has been sprayed, from the viewpoint of removing the organic solvent in the acrylic fibers in a short time without using a water bath.
  • nip rolls can be any rolls that are commonly used in the production of fibers through wet spinning.
  • the “pressing with nip rolls” refers to application of a pressure to acrylic fibers by passing the fibers between a pair of upper and lower nip rolls, or a pressure applied to the acrylic fibers at the time of winding the fibers on nip rolls.
  • the method for applying a pressure is not particularly limited as long as a pressure can be applied to the acrylic fibers with nip rolls.
  • Examples of the method include a method in which a pressure is applied to the upper nip roll by a cylinder, a method in which a weight is placed on the upper nip roll, and a method in which the upper nip roll is pulled down.
  • the nip rolls may be, e.g., rubber nip rolls and metallic nip rolls.
  • the upper nip roll is a rubber nip roll (also referred to as a rubber roll)
  • the lower nip roll is a metallic nip roll (also referred to as a metal roll).
  • the material for the rubber nip rolls include natural rubber, styrene-butadiene rubber, nitrile rubber, chloroprene rubber, butyl rubber, ethylene-propylene rubber, chlorosulfonated polyethylene rubber, silicone rubber, fluororubber, and urethane rubber.
  • the rubber nip rolls may be obtained by wrapping a metallic roll with rubber.
  • the thickness of the rubber is 3 mm or more, or 5 mm or more, or 8 mm or more, from the viewpoint of maintaining the cross-sectional shape of the fibers.
  • An exemplary material for the metallic nip rolls is stainless.
  • the hardness of the nip rolls is 40 to 100, or 50 to 85, or 55 to 80, as measured by a type A durometer in accordance with JIS K 6253.
  • spraying of water and pressing with the nip rolls may be alternately performed several times, or spraying of water may be performed at least twice and thereafter pressing with the nip rolls may be performed at least once.
  • the spraying of water and pressing with the nip rolls are alternately performed six times or more, or eight times or more, or ten times or more.
  • the water washing step can be performed by nip rolls and a means for spraying water that are alternately arranged.
  • a washing device including two or more sets of nip rolls and means for spraying water that are alternately arranged can be used.
  • the plurality of nip rolls and means for spraying water may be alternately arranged in series, or may be alternately arranged in two or more rows. For example, as shown in FIG.
  • a washing device 10 constituted by thirteen pairs of nip rolls 2 , each pair including an upper nip roll 21 and a lower nip roll 22 , and twelve water spraying means 3 (shower nozzles), the nip rolls 2 and the water spraying means 3 (shower nozzles) are arranged in three rows, i.e., a group “a”, a group “b”, and a group “c”.
  • Water receiving members 4 are disposed for the respective groups, and washing water that has been sprayed once is collected and drained by corresponding one of the water receiving members 4 .
  • the acrylic fibers move through the washing device 10 in the order of the group “a”, the group “b”, and the group “c”.
  • the group “a” is constituted by five pairs of nip rolls 2 and four water spraying means 3 (shower nozzles) that are alternately arranged
  • the group “b” is constituted by four pairs of nip rolls 2 and four water spraying means 3 (shower nozzles) that are alternately arranged
  • the group “c” is constituted by four pairs of nip rolls 2 and four water spraying means 3 (shower nozzles) that are alternately arranged.
  • the means for spraying water is not limited particularly, but a nozzle may be preferred from the viewpoint of the ease of spraying. Any nozzle that can spray water can be used as the nozzle, and the shape and the like of the nozzle are not limited particulars. For example, a slit-like nozzle or a hole-shaped nozzle can be used.
  • the direction in which water is sprayed is not limited particularly, and water may be sprayed from the side or from below. In one or more embodiments, from the viewpoint of uniformly spraying water, it may be preferable to use a shower nozzle having a plurality of holes.
  • the temperature of water used for spraying of water is not limited particularly, but, for example, water within a temperature range of 20 to 95° C. can be used. In one or more embodiments, from the viewpoint of improving the desolvation effect of removing the organic solvent, the temperature of water is 40° C. or more, or 50° C. or more, or 60° C. or more.
  • the amount of water (amount of water sprayed) coming out from each nozzle used for the spraying of water per unit time is, from the viewpoint of improving the desolvation effect, two times or more, or three times or more, or four times or more the dry mass of a resin constituting the acrylic fibers passing through the nip rolls per unit time.
  • the above-described amount of water is eight times or less, or seven times or less, or six times or less the dry mass of the resin constituting the acrylic fibers.
  • the amounts of water sprayed from respective nozzles may be uniform or may be different from nozzle to nozzle.
  • the ratio of the amount of water coming out from each nozzle per unit time to the dry mass of the resin constituting the acrylic fibers passing through the nip rolls per unit time is also referred to as the washing ratio.
  • the solid concentration (mass %) in the spinning solution refers to the concentration of the acrylic polymer in the spinning solution.
  • the amount of water coming out from each nozzle per unit time is calculated as follows.
  • Amount of water coming out from each nozzle per unit time (g) dry mass of resin constituting acrylic fibers passing through nip rolls per unit time (g) ⁇ washing ratio (times)
  • the nip pressure applied by the nip rolls is 0.2 MPa or higher, or 0.4 MPa or higher, or 0.6 MPa or higher. Moreover, a plurality of nip rolls may apply the same nip pressure or may apply different nip pressures. In one or more embodiments, from the viewpoint of easily reducing the cross-sectional collapse of the fibers, in the case where the organic solvent content in the acrylic fibers is 50 mass % or more, the nip pressure applied by the nip rolls is 2 MPa or lower, or 1.5 MPa or lower, or 1 MPa or lower.
  • the nip pressure applied by a nip roll is expressed as the force applied to a contact portion between the nip roll and the fiber bundle/the area of the contact portion between the nip roll and the fiber bundle.
  • the nip pressure applied by a nip roll in the case where a pressure is applied to the nip roll by a cylinder will be described using the drawings.
  • FIG. 2A is a schematic cross-sectional view for explaining the nip pressure applied by nip rolls
  • FIG. 2B is a schematic surface view for explaining the same.
  • a cylinder 200 to which an air pressure is applied in the direction indicated by an arrow applies a pressure to an upper nip roll 101 , thereby pressing a fiber bundle 300 sandwiched by a pair of nip rolls 100 including the upper nip roll 101 and a lower nip roll 102 .
  • a portion indicated by reference numeral 400 is a contact portion between the nip rolls 100 and the fiber bundle 300 .
  • Nip pressure (air pressure applied to cylinder ⁇ area of inner cylinder of cylinder)/area of contact portion between nip roll and fiber bundle
  • the ratio of the total fineness to the width of the acrylic fiber bundle is 300,000 dtex/cm or less, or 200,000 dtex/cm or less, or 100,000 dtex/cm or less.
  • a finishing oil may be applied to the acrylic fibers before predrying. Any finishing oils that are commonly used for the purpose of preventing static electricity, adhesion between fibers, or improving texture in the spinning step may be used, and known finishing oils can be used.
  • the acrylic fibers are subjected to predrying using a dryer into which steam is fed.
  • a dry-bulb temperature inside the dryer is 100 to 160° C.
  • a wet-bulb temperature inside the dryer is 60 to 100° C., from the viewpoint of obtaining high effects of recovering the cross-sectional collapse.
  • the dry-bulb temperature is 110 to 150° C.
  • the wet-bulb temperature is 70 to 90° C.
  • the term “temperature” indicates “dry-bulb temperature” unless otherwise specified.
  • the predrying time is not particularly limited, but may be 1 to 10 minutes or 1 to 6 minutes.
  • any drier that can dry fibers may be used as the dryer.
  • the dryer may be, e.g., a hot-air dryer that can directly blow hot air onto fibers.
  • Specific examples of the dryer include a jet dryer, a hot-air convection dryer, and a suction drum drier.
  • the temperature of hot air is not particularly limited, but may be 80 to 170° C. or 100 to 160° C.
  • the temperature of the steam to be fed into the drier is not particularly limited, but may be 100° C. or more, or 100 to 150° C., or 110 to 140° C., from the viewpoint of maintaining high temperature inside the drier.
  • the feeding amount of the steam is not particularly limited, and can be determined appropriately based on a desired wet-bulb temperature.
  • the water content of the acrylic fibers after predrying is not particularly limited, but may be 10 to 80 mass % or 20 to 70 mass %, from the viewpoint of obtaining high effects of recovering the cross-sectional collapse.
  • the acrylic fibers after predrying are subjected to a drying step to remove water inside the fibers almost perfectly.
  • Any drying method that can remove water inside fibers can be used. Examples of the method include hot-air drying, and drying using a heat roll by bringing fibers into contact with the heat roll.
  • the drying temperature is not particularly limited, but may be 110 to 190° C. or 110 to 170° C.
  • the drawn fibers may then be drawn further as needed.
  • the drawing temperature is not particularly limited, but may be 110 to 190° C. or 110 to 160° C.
  • the drawing ratio is not particularly limited, but may be 1 to 4 times. In one or more embodiments, the total drawing ratio including the bath drawing before drying is 2 to 12 times.
  • the dried fibers or the fibers drawn further after drying are further subjected to a thermal relaxation treatment step for relaxation.
  • the relaxation rate is not particularly limited, but may be 5% or more or 10% or more.
  • the thermal relaxation treatment can be performed under a dry heat atmosphere or superheated steam atmosphere at a temperature of 130 to 200° C. or 140 to 190° C.
  • the thermal relaxation treatment can also be performed in a pressurized steam atmosphere or heated and pressurized steam atmosphere at 120 to 180° C. under 0.05 to 0.4 MPa or 0.1 to 0.4 MPa.
  • the cross-sectional collapse of the acrylic fibers is reduced by subjecting the acrylic fibers that have been pressed with nip rolls in any of the stages before drying to predrying in a dryer into which steam is fed, and thereafter drying the predried fibers.
  • An acrylic copolymer (specific viscosity: 0.174) constituted by 46.1 mass % acrylonitrile (hereinafter, also referred to as “AN”), 51.7 mass % vinyl chloride (hereinafter, also referred to as ‘VCM’), and 2.0 mass % sodium styrenesulfonate (hereinafter, also referred to as “3S”) was dissolved in dimethyl sulfoxide (hereinafter, also referred to as “DMSO”) to produce a spinning solution having a resin concentration of 28.0 mass % and a water concentration of 3.5 mass %.
  • DMSO dimethyl sulfoxide
  • drawn yarns 1 (fiber bundle) obtained were passed through a washing device 10 having thirteen pairs of nip rolls 2 (diameter: 100 mm, width: 85 mm), each pair including an upper nip roll 21 and a lower nip roll 22 , and twelve shower nozzles 3 each producing a fan-shaped spray to remove DMSO in the drawn yarns 1 .
  • the drawn yarns 1 were washed by being alternately subjected to pressing with nip rolls, which was performed by applying a pressure to the upper nip roll 21 by a cylinder while passing the drawing yarns 1 between the upper nip roll 21 and the lower nip roll 22 of the nip roll 2 , and spraying of water using the shower nozzle 3 .
  • the upper nip roll 21 was a rubber roll obtained by wrapping nitrile rubber (NBR) (hardness: 60, thickness: 6 mm) around a stainless roll
  • NBR nitrile rubber
  • the lower nip roll 22 was a metal roll made from SUS304.
  • the washing device 10 was equipped with water receiving members 4 , and washing water that was sprayed once was collected and drained by the water receiving members 4 .
  • Each pair of nip rolls applied a nip pressure of 0.96 MPa.
  • the amount of water (amount of water sprayed) coming out from each of the shower nozzles per unit time was set to be five times the thy mass of the resin constituting the acrylic fibers passing through the nip rolls per unit time.
  • the temperature of water sprayed by each shower nozzle was set at 70° C. After water washing, a finishing oil was applied to the washed yarns, and the washed yarns to which the finishing oil was applied were placed in a jet drier that directly blows hot air to fiber bundles.
  • the yarns in the jet drier were subjected to predrying for three minutes while controlling the dry-bulb temperature and the wet-bulb temperature inside the jet drier to be 140° C. and 80° C., respectively, by feeding steam at 120° C. into the dryer. Then, the fiber bundle after predrying was dried at 140° C. for three minutes inside a jet dryer into which steam was not fed. The wet-bulb temperature inside the jet drier into which steam was not fed was 55° C. Then, the fiber bundle was wound around a heat roll at 165° C. for 30 seconds, drawn to two times under a dry heat atmosphere at 140° C., and subjected to thermal relaxation treatment at a relaxation rate of 20% under a dry heat atmosphere at 160° C. to obtain acrylic fibers having a single fiber fineness of about 47 dtex.
  • Acrylic fibers of Example 2 having a single fiber fineness of about 47 dtex were obtained in the same manner as in Example 1 except that an acrylic polymer having the composition and specific viscosity shown in Table 1 below was used, and the relaxation rate in the thermal relaxation treatment was 15%.
  • Acrylic fibers of Example 3 having a single fiber fineness of about 47 dtex were obtained in the same manner as in Example 2 except that the concentration of DMSO in the coagulation bath (“Concentration of coagulation bath” in Table 2) was 57 mass %.
  • Acrylic fibers of Example 4 having a single fiber fineness of about 47 dtex were obtained in the same manner as in Example 3 except that an acrylic polymer having the composition and specific viscosity shown in Table 1 below was used, the spinning solution having the resin concentration and water concentration shown in Table 1 was used, the dry-bulb temperature in predrying, the drying temperature and the drawing temperature were 150° C., and the relaxation rate in the thermal relaxation treatment was 25%.
  • Acrylic fibers of Example 5 having a single fiber fineness of about 47 dtex were obtained in the same manner as in Example 4 except that the concentration of DMSO in the coagulation bath was 52 mass %.
  • Acrylic fibers of Comparative Example 1 having a single fiber fineness of about 47 dtex were obtained in the same manner as in Example 1 except that predrying was not performed, and the acrylic fibers were dried for six minutes in a jet drier at 140° C.
  • Acrylic fibers of Comparative Example 2 having a single fiber fineness of about 47 dtex were obtained in the same manner as in Example 2 except that predrying was not performed, and the acrylic fibers were dried for six minutes in a jet drier at 140° C.
  • Acrylic fibers of Comparative Example 3 having a single fiber fineness of about 47 dtex were obtained in the same manner as in Example 3 except that predrying was not performed, and the acrylic fibers were dried for six minutes in a jet drier at 140° C.
  • Acrylic fibers of Comparative Example 4 having a single fiber fineness of about 47 dtex were obtained in the same manner as in Example 4 except that predrying was not performed, and the acrylic fibers were dried for six minutes in a jet drier at 150° C.
  • Acrylic fibers of Comparative Example 5 having a single fiber fineness of about 47 dtex were obtained in the same manner as in Example 5 except that predrying was not performed, and the acrylic fibers were dried for six minutes in a jet drier at 150° C.
  • the side surfaces of the fibers were observed with an ultra-deep color 3S profile measurement microscope (model “VK-9500” manufactured by KEYENCE) at 300th magnification (object lens: 150 ⁇ magnification, internal lens: 20 ⁇ magnification) to obtain images of the side surfaces.
  • Sections each having a length of 40 ⁇ m and a width of 80 ⁇ m were selected arbitrary from the obtained images to measure the surface areas of the sections each having a length of 40 ⁇ m and a width of 80 ⁇ m using an image analysis software VK Analyzer (model “VK-H1XA” manufactured by KEYENCE). These surface areas measured were averaged (n) to determine the surface roughness.
  • the acrylic fibers were crimped with a crimping machine so that the crimp waveform length (length from the top to the bottom of the crimp waveform) would be about 3 mm.
  • the crimped fibers (total fineness: 1129000 dtex) were cut into a length of 2 m. The mass of the fibers before hackling was measured. Then, near the center of the cut fibers was grasped, and the fibers were tossed on a hackling table (table on which 1470 needles are arranged, width: 66 cm, length: 120 cm) and pulled out therefrom. This operation was repeated 10 times in total, 5 times for the front side and 5 times for the back aide.
  • the mass of the fibers after hackling was measured in the same manner as that before hackling.
  • a hackling loss rate was calculated from the formula (1) below.
  • the hackling properties were evaluated using the following criteria with three levels on the basis of the hackling loss rate.
  • the “before HL” in the formula (1) indicates the mass (g) before hackling, and the “after HL” indicates the mass (g) after hackling.
  • the evaluation of B or higher indicates that the fibers have good hackling properties.
  • FIGS. 4 and 5 are photographs (400 ⁇ magnification) showing the cross sections of the acrylic fibers of Example 1 and the cross sections of acrylic fibers of Comparative Example 1, respectively, observed with an ultra-deep color 3S profile measurement microscope (model “VK-9500” manufactured by KEYENCE).
  • the acrylic fibers of Examples 1-5 which were subjected to predrying before the drying step in the dryer into which steam was fed, had lower deformation degree and less cross-sectional collapse than the corresponding acrylic fibers of Comparative Examples 1-5, which were not subjected to predrying.
  • the acrylic fibers of the examples which were subjected to predrying in the dryer into which steam was fed, had lower surface roughness and smoother surfaces than the corresponding acrylic fibers of the comparative examples, which were not subjected to predrying.
  • the acrylic fibers of the examples had a hackling loss rate of 5% or less, and exhibited favorable hackling properties.

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US20170253998A1 (en) * 2014-11-21 2017-09-07 Kaneka Corporation Acrylic-fiber manufacturing method

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JP4521999B2 (ja) * 2000-01-28 2010-08-11 株式会社カネカ アクリル系繊維中の溶媒除去方法およびその装置
KR100982921B1 (ko) * 2002-07-31 2010-09-20 카네카 코포레이션 인공 모발용 섬유 및 그 제조방법
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CA2820976C (fr) * 2009-06-10 2014-02-25 Mitsubishi Rayon Co., Ltd. Fil en acrylonitrile expanse pour une fibre de carbone, faisceau de fibres de precurseur, faisceau de fibres resistant a la flamme, faisceau de fibres de carbone et procedes de production de ce fil

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US20170253998A1 (en) * 2014-11-21 2017-09-07 Kaneka Corporation Acrylic-fiber manufacturing method
US10676843B2 (en) * 2014-11-21 2020-06-09 Kaneka Corporation Acrylic-fiber manufacturing method

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