Classifications

• • 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
  • D01F1/00—General methods for the manufacture of artificial filaments or the like
  • D01F1/02—Addition of substances to the spinning solution or to the melt
  • D01F1/06—Dyes
• • 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
  • D01F1/00—General methods for the manufacture of artificial filaments or the like
  • D01F1/02—Addition of substances to the spinning solution or to the melt
  • D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
• • 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
  • D01F1/00—General methods for the manufacture of artificial filaments or the like
  • D01F1/02—Addition of substances to the spinning solution or to the melt
  • D01F1/10—Other agents for modifying properties
  • D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
• • 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
  • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
  • D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
  • D01F6/605—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides from aromatic polyamides
• • 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
  • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
  • D01F6/74—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polycondensates of cyclic compounds, e.g. polyimides, polybenzimidazoles
• • 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
  • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
  • D01F6/76—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from other polycondensation products
• • 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
  • D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
  • D01F6/80—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyamides
  • D01F6/805—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyamides from aromatic copolyamides
• • 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
  • D06P1/44—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 using insoluble pigments or auxiliary substances, e.g. binders
  • D06P1/60—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 using insoluble pigments or auxiliary substances, e.g. binders using compositions containing polyethers
  • D06P1/613—Polyethers without nitrogen

Definitions

• the present invention relates to a colored organic fiber that is dark and excellent in flame retardancy, and a fabric, a garment, and a method for manufacturing the fabric using the organic fiber.
• Patent Documents 1 to 3 propose the use of a core-sheath structured yarn.
• the core-sheath structure yarn is used, there is a problem that it takes a lot of time and cost, and a problem that the flame retardant property is not sufficient because it is necessary to use a normal synthetic fiber inferior in flame retardancy for the sheath yarn.
• Patent Document 4 proposes that a fabric is dyed with a carrier agent and then washed, but it has not been sufficient in terms of flame retardancy.
• the present invention has been made in view of the above-described background, and an object thereof is a colored organic fiber that is dark and excellent in flame retardancy, a fabric and a garment using the organic fiber, and a fabric. It is in providing the manufacturing method of.
• the inventor of the present invention has a dark color and flame retardancy by reducing the amount of the carrier agent remaining in the organic fiber in the organic fiber dyed with the carrier agent.
• the inventors have found that an excellent organic fiber can be obtained, and have further studied earnestly to complete the present invention.
• colored organic fiber characterized in that the content of the carrier agent is 1.8% by mass or less with respect to the mass of the fiber”.
• the content of the carrier agent is preferably in the range of 0.1 to 1.8% by mass relative to the fiber mass.
• the carrier agent may be DL- ⁇ -ethylphenethyl alcohol, 2-ethoxybenzyl alcohol, 3-chlorobenzyl alcohol, 2,5-dimethylbenzyl alcohol, 2-nitrobenzyl alcohol, p-isopropylbenzyl alcohol, 2-methyl.
• the organic fiber may be a meta-type wholly aromatic polyamide fiber, para-type wholly aromatic polyamide fiber, polybenzoxazole (PBO) fiber, polybenzimidazole (PBI) fiber, polybenzthiazole (PBTZ) fiber, polyimide (PI).
• Fiber polysulfonamide (PSA), polyether ether ketone (PEEK) fiber, polyetherimide (PEI) fiber, polyarylate (PAr) fiber, melamine fiber, phenol fiber, fluorine-based fiber, polyphenylene sulfide (PPS) fiber It is preferably any one selected from the group consisting of
• the organic fiber is preferably a meta-type wholly aromatic polyamide fiber having a crystallinity of 15 to 25%. Moreover, it is preferable that the said organic fiber is a meta-type wholly aromatic polyamide fiber whose residual solvent amount is 1.0 mass% or less. Moreover, it is preferable that the said organic fiber is a meta type wholly aromatic polyamide fiber whose residual solvent amount is 0.1 mass% or less.
• the residual solvent is preferably any one selected from the group consisting of N, N-dimethylformamide, N, N-dimethylacetamide, N-methyl-2-pyrrolidone, and dimethyl sulfoxide.
• the organic fiber is a meta-type wholly aromatic polyamide fiber
• the meta-type wholly aromatic polyamide forming the meta-type wholly aromatic polyamide fiber includes a repeating structural unit represented by the following formula (1).
• an aromatic diamine component or an aromatic dicarboxylic acid halide component different from the main structural unit of the repeating structure is 1 to 10 mol% based on the total amount of the repeating structural unit of the aromatic polyamide as the third component.
• An aromatic polyamide copolymerized as described above is preferable.
• Ar1 is a divalent aromatic group having a bonding group other than in the meta-coordinate or parallel axis direction.
• the aromatic diamine as the third component is the formula (2), (3), or the aromatic dicarboxylic acid halide is the formula (4), (5).
• Ar2 is a divalent aromatic group different from Ar1
• Ar3 is a divalent aromatic group different from Ar1
• Y is at least one atom selected from the group consisting of an oxygen atom, a sulfur atom, and an alkylene group Or it is a functional group and X represents a halogen atom.
• the fabric containing the said colored organic fiber is provided.
• the fabric is polyester fiber, cellulose fiber, polyamide fiber, polyolefin fiber, acrylic fiber, rayon fiber, cotton fiber, animal hair fiber, polyurethane fiber, polyvinyl chloride fiber, polyvinylidene chloride fiber, acetate fiber, and polycarbonate fiber. It is preferable to include any one or more selected from the group consisting of: Moreover, it is preferable that any fiber which comprises a fabric contains a flame retardant. Moreover, it is preferable that any fiber which comprises a fabric contains a ultraviolet absorber or a ultraviolet reflector. Moreover, it is preferable that the fabric weight is 300 g / m 2 or less.
• LOI is 26 or more.
• the afterflame time is preferably 1 second or less in the vertical combustion test (JIS L1091A-4 method 3s flame contact).
• the lightness index L value is 80 or less.
• a method for producing a fabric containing the above-described colored organic fiber wherein the fabric containing the organic fiber is dyed with a carrier agent, and then the fabric is heated at a temperature of 90 to 140 ° C.
• a method for producing a fabric in which the content of the carrier agent contained in the organic fiber is 1.8% by mass or less with respect to the mass of the fiber is provided.
• a colored organic fiber that is dark and excellent in flame retardancy, a fabric and clothing using the organic fiber, and a method for producing the fabric are obtained.
• the present invention is directed to colored organic fibers.
• the content of the carrier agent is 1.8% by mass or less with respect to the mass of the fiber.
• the carrier agent is a dyeing assistant and is also called a swelling agent.
• the kind of carrier agent is not particularly limited. Specifically, L- ⁇ -ethylphenethyl alcohol, 2-ethoxybenzyl alcohol, 3-chlorobenzyl alcohol, 2,5-dimethylbenzyl alcohol, 2-nitrobenzyl alcohol, p-isopropylbenzyl alcohol, 2-methylphenethyl alcohol , 3-methylphenethyl alcohol, 4-methylphenethyl alcohol, 2-methoxybenzyl alcohol, 3-iodobenzyl alcohol, cinnamon alcohol, p-anisyl alcohol, benzhydrol, benzyl alcohol, propylene glycol phenyl ether, ethylene glycol phenyl Examples include ether and N-methylformanilide.
• the type of the organic fiber is not particularly limited.
• meta-type wholly aromatic polyamide fibers are preferable.
• the meta-type wholly aromatic polyamide fiber is a fiber made of a polymer in which 85 mol% or more of the repeating units is m-phenylene isophthalamide.
• Such a meta-type wholly aromatic polyamide may be a copolymer containing a third component within a range of less than 15 mol%.
• Such a meta-type wholly aromatic polyamide can be produced by a conventionally known interfacial polymerization method.
• the degree of polymerization of the polymer is such that the intrinsic viscosity (IV) measured with an N-methyl-2-pyrrolidone solution having a concentration of 0.5 g / 100 ml is in the range of 1.3 to 1.9 dl / g. Preferably used.
• the meta-type wholly aromatic polyamide may contain an alkylbenzene sulfonic acid onium salt.
• alkylbenzene sulfonic acid onium salt examples include tetrabutyl phosphonium salt of hexyl benzene sulfonate, tributyl benzyl phosphonium salt of hexyl benzene sulfonate, tetraphenyl phosphonium salt of dodecyl benzene sulfonate, tributyl tetradecyl phosphonate of dodecyl benzene sulfonate.
• Preferred examples include compounds such as a nium salt, tetrabutylphosphonium salt of dodecylbenzenesulfonate, and tributylbenzylammonium salt of dodecylbenzenesulfonate.
• dodecylbenzenesulfonic acid tetrabutylphosphonium salt or dodecylbenzenesulfonic acid tributylbenzylammonium salt is particularly easy to obtain and has good thermal stability and high solubility in N-methyl-2-pyrrolidone.
• tributylbenzylammonium salt is particularly easy to obtain and has good thermal stability and high solubility in N-methyl-2-pyrrolidone.
• the content ratio of the alkylbenzenesulfonic acid onium salt is 2.5 mol% or more, preferably 3.0 to 7.0 mol, relative to poly-m-phenyleneisophthalamide in order to obtain a sufficient dyeing effect. Those in the range of% are preferred.
• poly-m-phenylene isophthalamide As a method of mixing poly-m-phenylene isophthalamide and alkylbenzene sulfonic acid onium salt, poly-m-phenylene isophthalamide is mixed and dissolved in a solvent, and alkylbenzene sulfonic acid onium salt is dissolved in the solvent. Any of these may be used.
• the dope thus obtained is formed into fibers by a conventionally known method.
• the polymer used for the meta-type wholly aromatic polyamide fiber has a repeating structure in an aromatic polyamide skeleton containing a repeating structural unit represented by the following formula (2) for the purpose of improving dyeability and resistance to discoloration. It is also possible to copolymerize an aromatic diamine component or aromatic dicarboxylic acid halide component different from the main structural unit of 1 to 10 mol% with respect to the total amount of the repeating structural units of the aromatic polyamide as the third component. It is.
• Ar1 is a divalent aromatic group having a bonding group other than in the meta-coordinate or parallel axis direction.
• aromatic diamine represented by the formulas (2) and (3) include, for example, p-phenylenediamine, chlorophenylenediamine, methylphenylenediamine, Examples include acetylphenylenediamine, aminoanisidine, benzidine, bis (aminophenyl) ether, bis (aminophenyl) sulfone, diaminobenzanilide, diaminoazobenzene, and the like.
• aromatic dicarboxylic acid dichloride represented by the formulas (4) and (5) include, for example, terephthalic acid chloride, 1,4-naphthalenedicarboxylic acid chloride, 2,6-naphthalenedicarboxylic acid chloride, 4,4 Examples include '-biphenyldicarboxylic acid chloride, 5-chloroisophthalic acid chloride, 5-methoxyisophthalic acid chloride, bis (chlorocarbonylphenyl) ether, and the like.
• Ar2 is a divalent aromatic group different from Ar1
• Ar3 is a divalent aromatic group different from Ar1
• Y is at least one atom selected from the group consisting of an oxygen atom, a sulfur atom, and an alkylene group Or it is a functional group and X represents a halogen atom.
• the crystallinity of the meta-type wholly aromatic polyamide fiber is 5 to 35% in terms of good exhaustibility of the dye and easy adjustment to the target color even with less dye or weak dyeing conditions. Preferably there is. Further, it is more preferably 15 to 25% from the viewpoint that the surface uneven distribution of the dye hardly occurs, the discoloration resistance is high, and the dimensional stability necessary for practical use can be secured.
• the residual solvent amount of the meta-type wholly aromatic polyamide fiber is 1.
• It is preferably 0% by mass or less (more preferably 0.1% by mass or less, and still more preferably 0.01 to 0.09% by mass).
• the meta-type wholly aromatic polyamide fiber can be produced by the following method, and in particular, the crystallinity and the residual solvent amount can be within the above ranges by the method described later.
• the polymerization method of the meta-type wholly aromatic polyamide polymer is not particularly limited.
• the solution polymerization method and the interfacial polymerization method described in Japanese Patent Publication No. 35-14399, US Pat. No. 3,360,595, Japanese Patent Publication No. 47-10863 may be used.
• the spinning solution is not particularly limited.
• An amide solvent solution containing an aromatic copolyamide polymer obtained by the solution polymerization or interfacial polymerization may be used, or the polymer is isolated from the polymerization solution and dissolved in an amide solvent. It may be used.
• examples of the amide solvent include N, N-dimethylformamide, N, N-dimethylacetamide, N-methyl-2-pyrrolidone, dimethyl sulfoxide, and the like, and in particular, N, N-dimethylacetamide. Is preferred.
• the obtained copolymer aromatic polyamide polymer solution is further stabilized by containing an alkali metal salt or an alkaline earth metal salt, and can be used at a higher concentration and lower temperature, which is preferable.
• the alkali metal salt and alkaline earth metal salt are 1% by weight or less, more preferably 0.1% by weight or less, based on the total weight of the polymer solution.
• the spinning solution metal-type wholly aromatic polyamide polymer solution obtained above is spun into a coagulating solution and coagulated.
• the spinning apparatus is not particularly limited, and a conventionally known wet spinning apparatus can be used. Further, the number of spinning holes, the arrangement state, the hole shape and the like of the spinneret are not particularly limited. For example, a multi-hole spinneret for sufu having 1000 to 30000 holes and a spinning hole diameter of 0.05 to 0.2 mm may be used.
• the temperature of the spinning solution (meta-type wholly aromatic polyamide polymer solution) when spinning from the spinneret is preferably in the range of 20 to 90 ° C.
• an aqueous solution containing 45 to 60% by mass of an amide solvent (preferably NMP) substantially free of inorganic salt is used, and the temperature of the bath solution is in the range of 10 to 50 ° C. It is preferable to use in. If the concentration of the amide solvent (preferably NMP) is less than 45% by mass, the skin has a thick structure, and the cleaning efficiency in the cleaning process may be reduced, making it difficult to reduce the amount of residual solvent in the fiber. . On the other hand, when the concentration of the amide solvent (preferably NMP) exceeds 60% by mass, uniform coagulation cannot be performed up to the inside of the fiber, and therefore, the residual solvent amount of the fiber can be reduced. May become difficult.
• the fiber immersion time in the coagulation bath is preferably in the range of 0.1 to 30 seconds.
• an amide solvent preferably an aqueous solution having a concentration of NMP of 45 to 60% by mass, and a draw ratio of 3 to 4 times in a plastic drawing bath in which the temperature of the bath liquid is in the range of 10 to 50 ° C. It is preferable to perform stretching. After stretching, it is preferable to perform sufficient washing through an aqueous solution having an NMP concentration of 10 to 30 ° C. of 20 to 40% by mass, followed by a hot water bath of 50 to 70 ° C.
• the washed fiber is subjected to a dry heat treatment at a temperature of 270 to 290 ° C. to obtain a meta-type wholly aromatic aramid fiber satisfying the above-mentioned range of crystallinity and residual solvent amount.
• the fiber may be a long fiber (multifilament) or a short fiber.
• short fibers having a fiber length of 25 to 200 mm are preferable in blending with other fibers.
• the single fiber fineness of the organic fiber is preferably in the range of 1 to 5 dtex.
• a dyeing method using a carrier agent is preferable as a coloring method.
• a method of dyeing with a cationic dye is preferred for obtaining excellent darkness.
• the conditions for the dyeing process are not particularly limited.
• the content of the carrier agent is not more than 1.8% by mass relative to the mass of the fiber (preferably 0.1 to 1.8% by mass, more preferably 0.1 to 1.0% by mass, still more preferably Is 0.3 to 0.9% by mass). If the content is greater than 1.8% by mass, flame retardancy may be impaired. On the other hand, if the content is less than 0.1% by weight, excellent darkness may not be obtained, and the hot water washing process described later may be complicated.
• a dyed fabric is reduced and washed as necessary, and then heated with hot water at a temperature of 90 to 140 ° C. (more preferably 110 to 140 ° C.) for 10 to 30 A method of washing with hot water for a minute is exemplified.
• the fabric of the present invention is a fabric containing the above-mentioned colored organic fibers.
• a fabric may be composed of only the above-mentioned colored organic fibers, and further, polyester fiber, cellulose fiber, polyamide fiber, polyolefin fiber, acrylic fiber, rayon fiber, cotton fiber, animal hair fiber, polyurethane fiber, poly Other fibers such as vinyl chloride fiber, polyvinylidene chloride fiber, acetate fiber, and polycarbonate fiber may be included.
• the meta-type wholly aromatic polyamide fiber contained in the fabric is 50% by mass or more based on the mass of the fabric because excellent flame retardancy is obtained.
• the flame retardant fiber, synthetic fiber, regenerated fiber, and natural fiber can be arbitrarily mixed according to the application and use needs.
• the meta-type wholly aromatic polyamide fiber is 50 to 98% by mass
• the polyester fiber is 2 to 50% by mass
• the cellulosic mass fiber is 0 to 50%, which has both dyeability and comfort. It can also be done.
• the ratio may be adjusted according to the performance to be emphasized.
• the solubility to water is 0.04 mg / L or less. If the solubility in water is greater than 0.04 mg / L, the ultraviolet absorber may be eluted when dyeing with a carrier agent, which may reduce the light resistance after dyeing.
• the method for producing the fabric is not particularly limited. For example, after obtaining a spun yarn using the organic fiber (or the organic fiber and other fibers), weaving or knitting with a single yarn or twin yarn, dyed with a carrier agent, It is good to wash with hot water by the method.
• the fabric structure is preferably a woven fabric such as plain weave, twill weave, satin or double weave, but may be knitted fabric or non-woven fabric.
• the method for producing the fabric is not particularly limited.
• known knitting and knitting machines such as rapier looms and gripper looms can be used.
• the obtained fabric is excellent in dark color and flame retardancy because it uses the organic fiber.
• the darkness is preferably 80 or less (more preferably 52.5 or less, and further preferably 10 to 52.3) in terms of lightness index L value.
• the LOI is preferably 26 or more (more preferably 26 to 40).
• the afterflame time is preferably 25 seconds or less (more preferably 1 second or less).
• the basis weight is preferably 300 g / m 2 or less (preferably 50 to 250 g / m 2 ). If the weight per unit area is larger than 300 g / m 2 , the lightness of the fabric may be impaired.
• the apparel of the present invention is apparel using the above-mentioned fabric.
• Such clothing includes protective clothing, fire fighting clothing, fire protection clothing, rescue clothing, activity clothing, office work clothing, motor sports racing suits, work clothing, gloves, hats, vests, and the like.
• the work clothes include work clothes worn when working in steelworks or steel factories, work clothes for welding work, work clothes in an explosion-proof area, and the like.
• the gloves include working gloves used in the aircraft industry, the information equipment industry, the precision equipment industry, etc. that handle precision parts.
• the fabric may be used for textile products such as curtains, car seats, bags and the like.
• each physical property in an Example is measured with the following method.
• the measurement conditions were a Cu-K ⁇ radiation source (50 kV, 300 mA), a scanning angle range of 10 to 35 °, a continuous measurement of 0.1 ° width measurement, and a scan of 1 ° / min. From the measured diffraction profile, air scattering and incoherent scattering were corrected by linear approximation to obtain a total scattering profile. Next, a crystal scattering profile was obtained by subtracting the amorphous scattering profile from the total scattering profile. The degree of crystallinity was determined by the following equation from the area intensity of the crystal scattering profile (crystal scattering intensity) and the area intensity of the total scattering profile (total scattering intensity).
• Crystallinity (%) [crystal scattering intensity / total scattering intensity] ⁇ 100 (4) Amount of residual carrier agent Measurement method: A GC / MS sample comprising a fiber sample was packed in a sample tube and measured by ATD. After confirming the carrier agent by qualitative analysis, quantitative analysis was performed under the following conditions.
• polymetaphenylene isophthalamide powder produced by an interfacial polymerization method according to the method described in Japanese Patent Publication No. 47-10863 and having an intrinsic viscosity (IV) of 1.9 is placed at ⁇ 10 ° C. It was suspended in 80.0 parts by mass of cooled N-methyl-2-pyrrolidone (NMP) to form a slurry. Subsequently, the suspension was heated to 60 ° C. and dissolved to obtain a transparent polymer solution.
• NMP N-methyl-2-pyrrolidone
• Spinning was performed by discharging into a coagulation bath at a yarn speed of 7 m / min.
• the washed fiber was subjected to a dry heat treatment with a heat roller having a surface temperature of 280 ° C. to obtain a meta-type wholly aromatic aramid fiber.
• the meta-type wholly aromatic aramid fiber was used for crimping and cutting to obtain a staple fiber (raw cotton) having a length of 51 mm.
• the physical properties of the obtained meta-type wholly aromatic aramid fiber were as follows: the single fiber fineness was 1.7 dtex, the residual solvent amount was 0.08% by mass, and the crystallinity was 19%.
• each staple fiber of meta type fully aromatic aramid fiber (MA) (length 51 mm), para type fully aromatic polyamide (PA) (length 50 mm), nylon conductive yarn (AS) (length 51 mm), MA / PA / AS 93/5/2 blended spun yarn 40 count / twist yarn, weaved at warp density of 65 / 25.4mm, weft 55 / 25.4mm, with a basis weight of 170g / m Two plain texture fabrics were obtained.
• MA meta type fully aromatic aramid fiber
• PA para type fully aromatic polyamide
• AS nylon conductive yarn
• Example 2 The same operation as in Example 1 was performed except that 130 ° C. ⁇ 20 minutes once in the hot water cleaning prescription was changed to 130 ° C. ⁇ 20 minutes twice. The evaluation results are shown in Table 1.
• Example 3 The same operation as in Example 1 was performed except that 130 ° C. ⁇ 20 minutes once in the hot water washing prescription was changed to 120 ° C. ⁇ 20 minutes twice. The evaluation results are shown in Table 1.
• Example 4 The same operation as in Example 1 was performed except that Dawanol PPH 40 g / L in the above dyeing prescription was changed to benzyl alcohol 60 g / L. The evaluation results are shown in Table 1.
• Example 5 Same as Example 1 except that Dawanol PPH 40 g / L of the dyeing prescription is changed to benzyl alcohol 60 g / L, and 130 ° C. ⁇ 20 minutes of the hot water washing prescription is changed to 120 ° C. ⁇ 20 minutes twice. The operation was performed. The evaluation results are shown in Table 1.
• Example 6 Same as Example 1 except that Dawanol PPH 40 g / L of the dyeing prescription is changed to benzyl alcohol 60 g / L, and 130 ° C. ⁇ 20 minutes of the hot water washing prescription is changed to 120 ° C. ⁇ 20 minutes twice. The operation was performed. The evaluation results are shown in Table 1.
• Example 7 Same as Example 1 except that Dawanol PPH 40 g / L of the dyeing prescription is changed to benzyl alcohol 60 g / L, and 130 ° C. ⁇ 20 minutes of the hot water washing prescription is changed to 120 ° C. ⁇ 20 minutes twice. The operation was performed. The evaluation results are shown in Table 1.
• Example 1 The same operation as in Example 1 was performed except that 130 ° C. ⁇ 20 minutes of the hot water washing prescription was changed to 90 ° C. ⁇ 20 minutes once. The evaluation results are shown in Table 1.
• Example 8 The same operation as in Example 1 was performed except that 130 ° C. ⁇ 20 minutes of the hot water washing prescription was changed from 90 ° C. ⁇ 20 minutes to 5 times. The evaluation results are shown in Table 1.
• Example 9 The same operation as in Example 1 was performed except that 130 ° C. ⁇ 20 minutes of the hot water washing prescription was changed from 90 ° C. ⁇ 20 minutes to 10 times. The results are shown in Table 1.
• Example 10 The same operation as in Example 1 was performed except that Dawanol PPH of the dyeing prescription was changed to 30 g / L. The evaluation results are shown in Table 1.
• Example 11 The same operation as in Example 1 was performed except that Dawanol PPH of the dyeing prescription was changed to 20 g / L. The evaluation results are shown in Table 1.
• Example 12 The same operation as in Example 1 was performed except that Dawanol PPH of the dyeing prescription was changed to 10 g / L. The evaluation results are shown in Table 1.
• the organic fiber which was the colored organic fiber and was dark and excellent in the flame retardance, the fabric and clothing using this organic fiber, and the manufacturing method of a fabric are provided,
• the industrial value is the It is extremely large.

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• Engineering & Computer Science (AREA)
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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Manufacturing & Machinery (AREA)
• Coloring (AREA)
• Woven Fabrics (AREA)
• Artificial Filaments (AREA)
• Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
• Laminated Bodies (AREA)

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• 2015
  • 2015-04-06 WO PCT/JP2015/060712 patent/WO2015159749A1/ja active Application Filing
  • 2015-04-06 RU RU2016144442A patent/RU2658246C2/ru not_active IP Right Cessation
  • 2015-04-06 CN CN201580019932.3A patent/CN106232898B/zh active Active
  • 2015-04-06 AU AU2015247107A patent/AU2015247107B2/en not_active Ceased
  • 2015-04-06 CA CA2945737A patent/CA2945737A1/en not_active Abandoned
  • 2015-04-06 MX MX2016013384A patent/MX2016013384A/es unknown
  • 2015-04-06 US US15/303,824 patent/US20170037543A1/en not_active Abandoned
  • 2015-04-06 EP EP15779705.1A patent/EP3133204B1/en not_active Not-in-force
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