WO1999009238A1 - Fibre de polyester et textile prepare au moyen de cette fibre - Google Patents

Fibre de polyester et textile prepare au moyen de cette fibre Download PDF

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Publication number
WO1999009238A1
WO1999009238A1 PCT/JP1998/003660 JP9803660W WO9909238A1 WO 1999009238 A1 WO1999009238 A1 WO 1999009238A1 JP 9803660 W JP9803660 W JP 9803660W WO 9909238 A1 WO9909238 A1 WO 9909238A1
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Prior art keywords
fiber
dye
fabric
weight
polyester fiber
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PCT/JP1998/003660
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English (en)
Japanese (ja)
Inventor
Jinichiro Kato
Katsuhiro Fujimoto
Original Assignee
Asahi Kasei Kogyo Kabushiki Kaisha
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Application filed by Asahi Kasei Kogyo Kabushiki Kaisha filed Critical Asahi Kasei Kogyo Kabushiki Kaisha
Priority to US09/485,938 priority Critical patent/US6652964B1/en
Priority to KR1020007001596A priority patent/KR100359347B1/ko
Priority to JP51302799A priority patent/JP3226931B2/ja
Priority to EP98937854A priority patent/EP1006220A4/fr
Publication of WO1999009238A1 publication Critical patent/WO1999009238A1/fr

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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
    • D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
    • D01F6/84—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyesters

Definitions

  • the present invention relates to a polymethylene terephthalate fiber, particularly a polymethylene terephthalate fiber which can be dyed in a deep color under normal pressure with one or both of a cationic dye and a disperse dye.
  • the present invention relates to a fabric using this fiber.
  • Polymethylene terephthalate fiber has soft texture derived from low modulus, excellent elastic recovery and similar properties to nylon fiber, and low wearability and dimensions. This is an epoch-making fiber that has properties similar to polyethylene terephthalate fiber, such as stability and yellowing resistance, and is being applied to clothing, power plants, etc. It is getting.
  • polymethylene terephthalate fiber has a problem with dyeability. That is, in the known polymethylene terephthalate fiber, the dye to be used is limited to a disperse dye, and it can be dyed in a deep color only under a high pressure of 110 to 120 ° C. There was a major problem with staining.
  • the fact that the dyes used to dye the fibers are limited to disperse dyes means that the resulting dyed products have low clarity, and dry cleaning fastness, wet rub fastness, and sublimation fastness are slightly inferior. means.
  • the dyeing temperature for the dyeing in the dark is 1 1 0 ⁇ 1 2 0 D C, for example, other fibers pyrolysis occurs at these high temperatures
  • the mixed fabric cannot be dyed.
  • mixing polymethyl terephthalate fibers with other fibers, such as polyurethane elastic yarn, cotton, silk, and acetate fibers results in a softer texture than ever before.
  • Mixed textiles can be expected, but if these other fibers exceed 11 oC at the dyeing stage, their strength will be greatly reduced or they will be devitrified white, greatly impairing their merchantability. There was a problem.
  • polytrimethylene terephthalate fibers can be dyed at normal pressure with either a cation dye or a disperse dye, or with both dyes. It was not known.
  • a copolymer is prepared by adding isophthalic acid having a sulfonate metal base / sulfonate quaternary phosphonium base to the polyester before the completion of the polycondensation reaction (Japanese Patent Publication No. Japanese Patent Application Laid-Open No. 2004-977, Japanese Patent Publication No. Sho 47-22334, and Japanese Patent Laid-Open No. Hei 5-23013) are known.
  • the fibers thus obtained do not have the dyeing properties of a normal pressure thione dye and have a high modulus of elasticity, so that they give only a firm and stiff cloth.
  • adipic acid and isophthalic acid are used in addition to isophthalic acid having a sulfonate metal base in polyethylene phthalate.
  • dicarboxylic acids such as acids or their alkyl esters as copolymer components are known (for example, Japanese Patent Application Laid-Open No. 57-661119).
  • the fibers obtained in this way still have a high modulus of elasticity and give only rugged fabrics.
  • Fibers having good dyeability to disperse dyes, low elastic modulus, and excellent elastic recovery properties include, for example, a polymer disclosed in JP-A-52-530. Remethylene terephthalate fiber is an example.
  • Japanese Patent Publication No. Hei 9-5092225 discloses a method of dyeing polymethylene terephthalate fibers with a disperse dye under normal pressure. However, these fibers cannot be dyed at all under normal pressure with cationic dyes. Further, as has been clarified by detailed studies by the present inventors, with regard to disperse dyes, the techniques disclosed in these known documents only dye at extremely low dye concentration at normal pressure. I realized that I could't. For example, the dye concentration used in the example of Japanese Patent Publication No.
  • Hei 9-5099225 is at most 0.5% 0 wf (where the unit of% 0w ⁇ is the dye concentration in the dye solution). This is shown in terms of% by weight of the fiber that stains the same.)
  • fabrics that are dyed dark as well as light and medium colors are required.
  • Such a deep dyeing requires a dye concentration of 4% owf or more, and sometimes 10% owf or more.
  • a dye concentration of 4% owf or more cannot be dyed deeply at normal pressure because the dye cannot be exhausted sufficiently at normal pressure. Disclosure of the invention
  • An object of the present invention is to provide a polymethylethylene terephthalate fiber which can be dyed in a deep color under normal pressure by using either a cationic dye or a disperse dye or both dyes. is there.
  • Another object of the present invention is to provide a polyurethane elastic fiber, wool, silk.
  • the objective is to provide polytrimethylene terephthalate-based fibers that can dye composite fiber products mixed with tea, etc., without impairing the physical properties of these relatively low heat-resistant fibers. is there.
  • Still another object of the present invention is to provide a cross-woven, blended, or cross-knitted fabric of a polymethylentelephthalate fiber capable of being fast dyed under normal pressure and another fiber material. That is.
  • One specific object of the present invention is to provide a polyurethan elastic fiber and a polymethylene terephthalate-based fiber which can be fast dyed in a simple manner using ordinary atmospheric dyeing equipment. And providing a mixed fabric.
  • the present inventors have used polymethylene terephthalate obtained by copolymerizing a specific third component at a specific copolymerization ratio as a polymer, and have a very limited range of loss tangent peaks.
  • the present inventors have found that a polyester fiber prepared to have a temperature, an elastic modulus, and an elastic recovery can solve the above-mentioned problems, and have reached the present invention.
  • the first aspect of the present invention is that, in a fiber composed of polyester obtained by copolymerizing polymethylene terephthalate with a third component, the third component has an ester formation ratio of 0.5 to 5 mol% in a copolymerization ratio of 0.5 to 5 mol%.
  • the fiber has a loss tangent peak temperature of 85 to 115 ° C, an elastic modulus Q (g / d) and an elastic recovery rate R (%) of the fiber.
  • a second aspect of the present invention is a fiber comprising a polyester obtained by copolymerizing a poly (methylene terephthalate) with a third component, wherein the third component is (1) a copolymerization ratio of 1.5 to 12% by weight of carbon.
  • Aliphatic or alicyclic glycol having a number of 4 to 12; (2) a carbon number of 2 to 9 having a copolymerization ratio of 3 to 9% by weight; At least one selected from aliphatic or alicyclic dicarboxylic acids up to 14 or isophthalic acid; and (3) a polyalkylene glycol having a copolymerization ratio of 3 to 10% by weight.
  • the loss tangent peak temperature of the fiber is 85 to 102 ° C, and the relationship between the elastic modulus Q (g / d) and the elastic recovery rate R (%) of the fiber is expressed by the following equation (1).
  • a polyester fiber characterized by satisfying and a fabric using the same.
  • the polymer constituting the polyester fiber of the present invention has a specific amount of the third polymer in the polymethylene terephthalate. It is a polyester obtained by copolymerizing the components.
  • polymethylethylene terephthalate is a polyester containing terephthalic acid as an acid component and trimethylene glycol (also referred to as 1,3-propanediol) as a diol component. It is.
  • a normal pressure thione dye-dyable fiber When a specific amount of an ester-forming sulfonate compound is used as the third component to be copolymerized, a normal pressure thione dye-dyable fiber can be obtained. Also, (1) aliphatic or alicyclic glycol having 4 to 12 carbon atoms, (2) aliphatic or alicyclic dicarboxylic acid having 2 to 14 carbon atoms, or isophthalic acid When a specific amount of at least one selected from an acid and (3) polyalkylene glycol is copolymerized, a normal pressure disperse dye-dyable fiber can be obtained.
  • ester-forming sulfonate compound used in the present invention examples include a sulfonate group-containing compound represented by the following general formula.
  • R,, R may be the same group or different groups.
  • M is a metal, NH 4 , or a phosphonium group represented by the formula PR 3 RRR (wherein R 3 , R 4 , R 5 , and R 6 are a hydrogen atom, an alkyl group, an aryl group, and an arsenic group) And represents the same or different group selected from the droxyalkyl groups, and is preferably an alkyl group having 1 to 10 carbon atoms.
  • M is a metal, it is preferably an alkali metal or an alkaline earth metal.
  • Z is a trivalent organic group, preferably a trivalent aromatic group.
  • a fiber that can be dyed to a deep color with a cationic dye under normal pressure is obtained. Also, compared to polytrimethylene terephthalate homopolymer fiber, it becomes easier to dye the disperse dye.
  • the fact that dyeing can be performed at normal pressure means that the exhaustion rate to fibers at 95 ° C. is approximately 70% or more.
  • the cationic dyeable yarn exhibits an appropriate amount of weight loss characteristics, it is possible to obtain a softer texture by reducing the amount of alkali after weaving.
  • the alkali weight reduction means that the fabric is heated in an aqueous alkali solution to dissolve a part of the polymer on the fiber surface.
  • Moderate alkaline weight loss means that the amount and rate of alkaline weight loss can be controlled industrially. This is a surprisingly great feature. For example, in the case of cationic dyeable poly (ethylene terephthalate) fiber, the weight loss rate is too fast to control industrially, and in the polyester fiber of the present invention, the control is practically impossible.
  • the weight loss rate is the same as that of ordinary polyethylene terephthalate fiber that is not dyeable by Kachion, and it is possible to perform the weight loss using a known method.
  • the polyester fiber of the present invention whose weight has been reduced, becomes more soft and has micropores of several // m on the surface of the fiber, so that it has a dry feeling. It is possible to provide a feature that dyeing can be performed more clearly.
  • ester-forming sulfonate compounds include 5_ sodium sulfeusophthalic acid, 5_ calcium sulfoisophtalic acid, 41 sodium sulfo-1,2, 6_ naphtha range Carboxylic acid, 2-sodium sulfo 4-hydroxybenzoic acid, 3,5-dicarboxylate benzenesulfonate tetramethyl phosphonium salt, 3,5-dicarboxylic acid benzene sulfonate tetrabutyl phosphonium salt, 3, 5 Tricarboxylic acid benzenesulfonic acid tributylmethylphosphonium salt, 2,6-dicarboxylic acid naphthalene 1-4,2-sulfonic acid tetrabutylphosphonium salt, 2,6-dicarboxylic acid naphthalene-1 4—snolefone Tetramethylphosphonium acid salt, 3,5—dicarboxylic acid benzenesulfonic acid
  • the copolymerization ratio of the ester-forming sulfonate compound to the poly (methylene terephthalate) is 0.5 to 5 mol based on the total number of mols of all the acid components constituting the polyester. It needs to be%.
  • the copolymerization ratio of the ester-forming sulfonate compound is less than 0.5 mol%, it becomes impossible to dye with a cationic dye at normal pressure.
  • the proportion of the ester-forming sulfonate compound exceeds 5 mol%, the heat resistance of the polymer deteriorates, the polymerizability and the spinnability deteriorate, and the fiber is liable to yellow. From the viewpoint of having both polymerizability and spinnability while maintaining sufficient dyeability for cationic dyes, it is preferably 1 to 3 mol%, particularly preferably 1.2 to 2.5 mol%.
  • aliphatic and alicyclic glycols having 4 to 12 carbon atoms used in the present invention include, for example, 1,2-butanediol, 1,3-butanediol, and 1,4-butanediol.
  • the copolymerization ratio should be 1.5 to 12% by weight based on the weight of the polymer. If the copolymerization ratio is less than 1.5% by weight, it becomes impossible to dye a disperse dye to a deep color at normal pressure.
  • the copolymerization ratio of glycol has a strong correlation with the elastic modulus, elastic recovery, melting point, glass transition point, and dyeability. If the copolymerization ratio exceeds 12% by weight, the melting point and the glass transition point are greatly reduced, and the post-processing represented by heat setting and the usual use represented by ironing are performed. There are drawbacks in that the texture changes hardly in stages, and the dry cleaning fastness of the dyed fabric is reduced. Preferably it is 2 to 10% by weight, more preferably 3 to 7% by weight.
  • the aliphatic or alicyclic dica having 2 to 14 carbon atoms used in the present invention include oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, heptane diacid, octane diacid, sebacic acid, dodecane diacid, and 2 — Methylglutaric acid, 2-Methyladipic acid, fumaric acid, maleic acid, itaconic acid, 1,4-cyclohexanedicarboxylic acid, 1,3—cyclohexanedicarboxylic acid, 1,2— Hexanedicarboxylic acid and the like.
  • By copolymerizing these dicarboxylic acids with polytrimethylene terephthalate it becomes possible to dye to a deep color using a disperse dye at normal pressure.
  • dicarboxylic acids or isophthalic acids sebacic acid, dodecane diacid, and 1,4-cyclohexane in terms of polymerization rate and light resistance during copolymerization are excellent.
  • Dicarboxylic acid and isophthalic acid are preferred.
  • isophthalic acid is particularly preferred in view of the excellent whiteness of the polymer.
  • the copolymerization ratio of the aliphatic or alicyclic dicarboxylic acid or isophthalic acid to polymethylene terephthalate needs to be 3 to 9% by weight based on one weight of the polymer. If the copolymerization ratio is less than 3% by weight, it becomes impossible to dye a deep color at normal pressure. When the copolymerization ratio is more than 9% by weight, the melting point and the glass transition point are too low, so that the post-processing typified by heat setting property and the normal use stage represented by ironing are required. However, there are drawbacks in that the texture is hardly changed and the dry cleaning fastness of the dyed fabric is reduced. It is preferably from 3 to 8% by weight, more preferably from 3 to 7% by weight.
  • polyalkylene glycol may be used as the copolymerization component.
  • glycol or acid is copolymerized as the third component
  • the melting point is inevitably lowered, and the spinnability is deteriorated. Welding ⁇ noticeable shrinkage, etc. This may cause poor handling.
  • polyalkylene glycol is used as the third component, the melting point hardly decreases and such a problem does not occur. This is thought to be because the polyalkylene glycol component is localized in the polymer due to its high molecular weight.
  • the polyalkylene glycol used may be polyethylene glycol, polymethylene glycol, polytetramethylene glycol or a copolymer thereof, but polyethylene is preferred in view of thermal stability. Glycol is most preferred.
  • the average molecular weight of polyalkylene glycol is preferably from 300 to 20000.
  • the average molecular weight is less than 300, since a very low molecular weight polyalkylene glycol is contained, it is distilled off under reduced pressure during polymerization under high vacuum, and the resulting polymer is obtained.
  • the amount of polyalkylene glycol contained is not constant. Therefore, the properties of the raw yarn such as high elongation properties, dyeing properties and thermal properties are not uniform, and the properties of the product vary.
  • the average molecular weight of polyalkylene glycol is preferably from 400 to 100,000, more preferably from 500 to 500,000.
  • the copolymerization ratio of the polyalkylene glycol to the polymethylene terephthalate must be 3 to 10% by weight based on the weight of the polymer.
  • the proportion of the polyalkylene glycol is less than 3% by weight, it becomes impossible to dye the disperse dye to a deep color at normal pressure.
  • the proportion of polyalkylene glycol exceeds 10% by weight, the heat resistance of the polymer decreases, and the polymerizability and spinnability deteriorate significantly.
  • the glass transition point is too low, and the texture changes to hard during normal use, such as post-processing, such as heat setting, and the drying of the fabric after dyeing.
  • a disadvantage arises in that cleaning fastness and light fastness are greatly reduced. It is preferably 4 to 8% by weight.
  • the polymer constituting the polyester fiber of the present invention can be copolymerized and blended with the fourth component within a range not to impair the purpose of the present invention. Even when such a fourth component is used, it is necessary to keep the copolymerization ratio in the range described above so as not to hinder the object of the present invention.
  • ester-forming sulfonate compounds and (1) aliphatic or cycloaliphatic glycols having 4 to 12 carbon atoms, and (2) aliphatics having 2 to 14 carbon atoms.
  • copolymerization of at least one selected from alicyclic dicarboxylic acid, isophthalic acid, and (3) polyalkylene glycol makes it possible to dye both cationic dyes and disperse dyes at normal pressure.
  • Polyester fibers can be obtained.
  • the copolymerization ratio is preferably from 2 to 2.5 mol% of the ester-forming sulfonate compound, and at least one selected from the above (1) to (3). It is preferred that one species be 3 to 7% by weight.
  • additives may be added to the polyester fiber of the present invention, for example, an anti-glazing agent, a heat stabilizer, an anti-foaming agent, a coloring agent, a flame retardant, an antioxidant, an ultraviolet absorber, and an infrared absorber.
  • an anti-glazing agent for example, an anti-glazing agent, a heat stabilizer, an anti-foaming agent, a coloring agent, a flame retardant, an antioxidant, an ultraviolet absorber, and an infrared absorber.
  • Agents, crystal nucleating agents, fluorescent whitening agents and the like may be copolymerized or mixed.
  • the molecular weight of the polyester used in the present invention can be defined by the intrinsic viscosity.
  • the intrinsic viscosity [? 7] is preferably 0.3 to 2.0, more preferably 0.35 to 2.0. With a value of 1.5, particularly preferably of 0.4 to 2, a polyester fiber having excellent strength and spinnability can be obtained. If the intrinsic viscosity is less than 0.3, the polymerization degree of the polymer is too low. The spinnability becomes unstable. Also, the strength of the obtained fiber is low and not satisfactory. On the other hand, when the intrinsic viscosity exceeds 2.0, the melt viscosity is too high, so that the metering by the gear pump cannot be performed smoothly, and the spinnability is reduced due to poor discharge.
  • polymerization can be basically carried out by using a known method. That is, in the ordinary production process of polymethylene terephthalate, a transesterification reaction followed by a polycondensation reaction of terephthalic acid or a lower ester of terephthalic acid such as dimethyl terephthalate with trimethylene glycol is carried out.
  • the third component can be added at any stage during the process. In this case, the ester-forming sulfonate compound and the aliphatic or alicyclic dicarboxylic acid or isophthalic acid need to be added before the transesterification reaction because the reaction with trimethylene glycol must be promoted.
  • polyalkylene glycol it is preferable to add polyalkylene glycol at the end of the transesterification reaction in order to prevent yellowing of the polymer and bumping at reduced pressure.
  • the transesterification catalyst it is preferable to use metal acetate, titanium alkoxide, etc. in an amount of 0.01 to 0.1% by weight, because it has the reaction speed, the whiteness of the polymer, and the thermal stability. .
  • the reaction temperature is about 200 to 240 ° C.
  • antimony oxide, titan alkoxide, or the like can be used. In particular, when titan alkoxide is used, it may be used also as a transesterification catalyst.
  • the amount of the catalyst is 0.01 to 0.1% by weight based on the total amount of rubonic acid used from the viewpoint of the reaction rate and the whiteness of the polymer.
  • the reaction temperature is 240 to 280. C, and the degree of vacuum is 0.001 to 1 t0 rr.
  • various additives may be added at any stage of the polymerization process.However, in order to minimize the inhibition of the reaction, they are added at any stage after the transesterification reaction. I prefer to do that.
  • the polymer constituting the polyester fiber of the present invention may be obtained by increasing the molecular weight by subjecting the polymer obtained by the above method to solid phase polymerization in an inert gas such as nitrogen or argon or under reduced pressure.
  • an inert gas such as nitrogen or argon or under reduced pressure.
  • solid phase polymerization for example, a known method used for polyethylene terephthalate can be applied as it is, but the intrinsic viscosity of the prepolymer before solid-phase polymerization is 0.4 to 0.8 as whiteness.
  • the solid-state polymerization temperature is preferably 170 to 230 ° C, and the time varies depending on the desired viscosity, but is usually about 3 to 36 hours. It is.
  • the polymer constituting the polyester fiber of the present invention may be produced by blending two kinds of polymers so as to obtain a desired copolymer composition.
  • polymethylene terephthalate prepared by copolymerizing 1,4-butanediol at 5% by weight has 95% by weight of polymethylene terephthalate and 95% by weight of polybutylene terephthalate. It may be manufactured by mixing 5% by weight of tallate.
  • Mixing here means that the mixture may be mixed in a polymerization kettle and sufficiently transesterified before being discharged, or more simply, the reaction may be performed in an extruder with the tip blended. Even with such a method, the transesterification rate is sufficiently high, so that a homogeneous polymer can be obtained.
  • What is important in the method for producing the polymer constituting the polyester fiber of the present invention is to maintain the whiteness of the polymer.
  • the third component is copolymerized with polymethylene terephthalate, it generally becomes easier to color during the polymerization process and the spinning process. Therefore, as a method for increasing the whiteness, it is preferable to use the above-mentioned preferable amount of catalyst and reaction temperature, and at the same time, use a heat stabilizer and a coloring inhibitor.
  • Trivalent or trivalent phosphorus compounds are preferred, e.g., trimethyl phosphate, triethyl phosphate, triphenyl phosphate, trimethyl phosphate, triethyl phosphate And triphenylphosphite, phosphoric acid, phosphorous acid and the like, and it is preferable to add 0.01 to 0.07% by weight to the polymer.
  • the coloring inhibitor include cobalt acetate and cobalt formate, and it is preferable to add 0.01 to 0.07% by weight to the polymer.
  • additives include lithium acetate, lithium carbonate, lithium formate, sodium acetate, sodium carbonate, sodium formate, sodium hydroxide, and sodium hydroxide.
  • Basic metal salts such as calcium and potassium hydroxide may be mentioned, and the amount thereof is 20 to 400 mol%, preferably 70 to 100 mol%, based on the ester-forming sulfonate compound. ⁇ 200 mol%.
  • the form of the polyester fiber of the present invention may be any of a long fiber and a short fiber, and in the case of a long fiber, any of a multifilament and a monofilament may be used. .
  • the total denier there is no particular limitation on the total denier, and it is preferably 5 to 1000 d, and especially 5 to 200 d when used for clothing.
  • the single yarn denier is not particularly limited, but is preferably 0.001 to 10 d.
  • the cross-sectional shape is not particularly limited, such as a round shape, a triangular shape, a flat shape, a star shape, and a w shape, and may be solid or hollow.
  • the peak temperature of the loss tangent (hereinafter abbreviated as “T max”) obtained from the dynamic viscoelasticity measurement is 85 to 85 when the third component is an ester-forming sulfonate compound.
  • the third component is (1) a copolymerization ratio of 1.5 to ⁇ 2% by weight of an aliphatic or alicyclic glycol having 4 to 12 carbon atoms, and (2) a copolymerization ratio of 3 From 9 to 9% by weight of an aliphatic or alicyclic dicarboxylic acid having 2 to 14 carbon atoms or isophthalic acid; (3) from a copolymerization ratio of 3 to 10% by weight of a polyalkylene glycol; It must be 85 to 102 for at least one of the selected species.
  • Tmax corresponds to the molecular density of the amorphous part
  • the exhaustion rate increases.
  • Tmax is less than 85 ° C
  • molecules can easily move at low temperatures when any of the third components is used.Therefore, typical post-processing such as heat setting and ironing are typical examples. During normal use, the shrinkage becomes too great and the texture becomes worse, or the dry cleaning fastness of the fabric after dyeing is reduced.
  • the third component is an ester-forming sulfonate.
  • the dyeability which is the object of the present invention, is reduced, and the space for the dye is too small, so that the cation dye under normal pressure is used.
  • the dye cannot be dyed to a dark color.
  • the third component (1) a copolymerization ratio of 1.5 to 12% by weight, an aliphatic or alicyclic glycol having 4 to 12 carbon atoms, and (2) a copolymerization ratio of 3 to 9% by weight.
  • Tmax is a structural factor of a fiber, spinning temperature, spinning speed, draw ratio, heat treatment temperature, scouring conditions, and alkali reduction even for polymers having the same copolymer composition. It shows different values depending on spinning conditions such as conditions and dyeing conditions, and post-processing conditions. In particular, since this value greatly changes with the heat set temperature, it is important to change the heat set temperature to keep T max in the above range.
  • the concept of setting the heat set temperature is roughly described. In the case of the polyester fiber specified in the present invention, T is set when the heat set temperature is in the range from room temperature to about 150 ° C.
  • ma X is a gradually increasing force, and after about 160 ° C, it drops significantly thereafter.
  • T max varies slightly depending on the type of the third component, but when an ester-forming sulfonate compound is used as the third component, the range of 97 to 112 ° C.
  • at least one selected from aliphatic or alicyclic dicarboxylic acids up to 14 and (3) alkylene glycol having a copolymerization ratio of 3 to 10% by weight 85 to 102 is used.
  • ° C particularly preferably 90-98 ° C.
  • the elastic modulus Q (g / d) of the polyester fiber of the present invention and the elastic recovery rate R (%) after standing for 20 minutes after elongation of 20% may satisfy the following expression (1). is necessary. This is because, when the formula (1) is satisfied, the fabric obtained from the polyester fiber of the present invention has a soft texture equal to or higher than that of nylon, unlike the fabric obtained from the conventional polyester fiber. It is because it can have.
  • the ester-forming sulfonate compound having a copolymerization ratio of 1.2 to 2.5 mol% and a copolymer having a copolymerization ratio of 3 to 7% by weight (1) a fatty acid having a carbon number of 4 to 12 or Alicyclic glycol, (2) having 4 to 12 carbon atoms Aliphatic or cycloaliphatic dicarboxylic acids, or isophthalic acid, up to (
  • the Tmax of the fiber is 85 to 115 ° C and
  • the reason that the relationship between the elastic modulus Q (g / d) and the elastic recovery rate R (%) of the fiber satisfies the equation (1) is the same as the detailed T max and the basis of the equation (1) described above. Required from.
  • the polyester fiber of the present invention can be obtained by the following method.
  • the polyester fiber of the present invention is obtained by melting a polymer dried to a water content of at least 100 ppm, and preferably 50 ppm or less using an extruder or the like, and then melting the polymer. It can be obtained by winding after extruding from a spinneret and then stretching. Stretching after winding here means that the yarn is wound on a bobbin or the like after spinning, and this yarn is stretched using another device, a so-called ordinary method, or a polymer extruded from a spinneret.
  • the spinning temperature for melt spinning the polymer is 240 to 320 ° C, preferably 240 to 300 ° C, and more preferably 240 to 28 ° C. A range of 0 ° C is appropriate. If the spinning temperature is lower than 240 ° C., the temperature is too low to be in a stable molten state, the resulting fibers have large spots, and no satisfactory strength and elongation are exhibited. On the other hand, when the spinning temperature exceeds 320 ° C., thermal decomposition becomes severe, and the obtained yarn is colored and does not show satisfactory strength and elongation.
  • the winding speed of the yarn is not particularly limited, but is usually 350 m / min or less, preferably 250 m / min or less, and more preferably 200 m / min or less. Take up. If the winding speed exceeds 350 m / min, the crystallization proceeds too much before winding, and the stretching ratio cannot be increased in the stretching process. Insufficient thread strength and elastic recovery rate cannot be obtained, or winding and tightening occur, and the bobbin and the like cannot be pulled out of the winder.
  • the stretching ratio at the time of stretching is 2 to 4 times, preferably 2.2 to 3.7 times, and more preferably 2.5 to 3.5 times.
  • the draw ratio is not more than 2 times, the polymer cannot be oriented sufficiently by drawing, and the elastic recovery of the obtained yarn will be low, which satisfies the expression (1). I can't do that. If it is 4 times or more, thread breakage is severe and it is not possible to perform stable elongation.
  • 3 0 ⁇ 8 0 Q C temperature is a stretching zone during stretching, favored properly the 3 5 ⁇ 7 0 ° C, rather further favored good 4 0 ⁇ 6 5 ° C. If the temperature of the drawing zone is lower than 30 ° C., yarn breakage frequently occurs during drawing, and continuous fibers cannot be obtained. If the temperature exceeds 80 ° C, slippage of the fiber against a heating zone such as a drawing roll deteriorates, so that single yarn breakage occurs frequently and the yarn becomes full of fluff. In addition, the polymers will slip through each other, resulting in insufficient orientation and lowering the elastic recovery rate.
  • This heat treatment is carried out at 90 to 200 ° C, preferably at 100 to 190 ° C, and more preferably at 110 to 180 ° C. If the heat treatment temperature is lower than 90 ° C, the crystallization of the fiber does not sufficiently occur, and the elastic recovery is deteriorated. At a temperature higher than 200 ° C., the fiber is cut by the heat treatment zone and cannot be drawn.
  • the polymer is extruded in the same manner as in the conventional method, and the molten multi-filament coming out of the spinneret is not immediately quenched, but is placed immediately below the spinneret at 30 to 200 ° C. After passing through a heat retaining area of 2 to 80 cm in length maintained at the same ambient temperature to suppress rapid cooling, this molten multifilament is rapidly cooled and converted into a solid multifilament, followed by stretching. It is extremely preferred to submit to the process. By allowing the polymer to pass through this heat insulation region, it is possible to suppress the generation of fine crystals and extremely oriented amorphous parts due to rapid cooling of the polymer, and to create an amorphous structure that is easily stretched in the stretching step.
  • Polyethylene terephthalate has a much faster crystallization rate than, for example, polyester such as polyethylene terephthalate. Performing such slow cooling is an extremely effective method for suppressing the formation of fine crystals and extremely oriented amorphous parts. If the temperature is lower than 30 ° C, the film is rapidly cooled, making it difficult to increase the draw ratio. Above 200 ° C., thread breakage tends to occur.
  • the temperature of such a heat retaining region is preferably from 40 to 200 ° C, more preferably from 50 to 150 ° C. Also, this The length of the heat insulation area is preferably 5 to 30 cm.
  • the winding speed of the first roll is 300 to 300 m / min.
  • the spinning speed is less than 300 m / min, spinning stability is excellent, but productivity is greatly reduced. If it exceeds 300 m / min, the orientation of the amorphous part or partial crystallization proceeds before winding, and the stretching ratio cannot be increased in the stretching process. And it is difficult to develop sufficient yarn strength.
  • it is 150 to 270 m / min.
  • the relax ratio (winding speed Z second roll speed) is about 0.95 to 0.99, preferably 0.95 to 0.98.
  • the speed of the second roll is determined by the stretching ratio, but is usually from 600 to 600 m / min.
  • the stretching ratio between the first roll and the second roll is 1.3 to 3 times, preferably 2 to 2.7 times. If the draw ratio is 1.3 or less, the polymer cannot be sufficiently oriented by stretching, and the strength and elastic recovery of the obtained fiber will be low. On the other hand, if it is three times or more, the fluff is so severe that stretching cannot be performed stably.
  • the temperature of the first roll is 40 to 70. C, and it is possible to create a situation where stretching is easy in this range. It is preferably between 50 and 60.
  • the heat is set at the second port, but the temperature is 120 to 160 ° C.
  • the temperature is lower than 120 ° C, thermal stability is poor, thermal deformation, and aging change. At a temperature of 160 ° C. or higher, fluff and yarn breakage occur, and stable spinning cannot be performed. Preferably, it is between 120 and 150 ° C. It is important to apply the favorable conditions indicated by the ordinary method and the straight-rolling method described above in order to ensure the homogeneity and quality of the obtained fiber.
  • u% can be used as a parameter for evaluating the quality of a fiber obtained by applying preferable spinning conditions.
  • u% is a parameter that indicates the homogeneity of the fiber cross-section. Under favorable conditions, U% is less than 2.5%, and in some cases less than 1.5%.
  • the polyester fiber obtained as described above can be used alone or as a part of a fabric to provide a fabric having excellent softness, stretchability, and coloring.
  • There are no particular restrictions on other fibers used in part of the fabric but in particular stretch fibers, cellulose fibers, wool, silk, acetate, etc. represented by polyurethane elastic fibers.
  • stretch fibers cellulose fibers, wool, silk, acetate, etc. represented by polyurethane elastic fibers.
  • the fabric can be dyed at normal pressure by using, for example, a cationic dye and / or a disperse dye, and has a unique texture that has a softness and a stretch property that have not existed conventionally.
  • the polyester fiber of the present invention can be used as a field in which either the cation dye or the disperse dye, or both dyes, can be dyed in a deep color. It can be dyed quickly and can have a different softness and sunset from the mixed fabric of nylon fiber and stretch fiber typified by polyurethane elastic fiber.
  • a mixed fabric of the poly (methylene terephthalate) fiber and a stretch fiber represented by a polyurea elastic fiber is exemplified as a particularly preferred fabric. You.
  • the form and knitting and weaving method of the cloth of the present invention including the above-mentioned mixed cloth are not particularly limited, and known methods can be used.
  • An example Examples thereof include plain woven fabrics using the polyester fiber of the present invention as warp or weft yarns, woven fabrics such as reversible woven fabrics, and knitted fabrics such as tricots and raschels. You may.
  • the stretch fiber used in the present invention is not particularly limited, but is a dry-spun or melt-spun polyurethane elastic fiber or a polybutylene terephthalate fiber.
  • polyester-based elastic fibers typified by polybutylene terephthalate fiber and polytetramethylene glycol copolymer.
  • the content of the polyester fiber of the present invention is not particularly limited, but is preferably 60 to 98%.
  • the fabric of the present invention can be dyed, for example, after knitting and weaving, through the steps of scouring, presetting, dyeing, and final set by a conventional method. If necessary, after scouring and before dyeing, it is possible to carry out a weight reduction treatment by an ordinary method.
  • Refining can be performed in a temperature range of 40 to 98 ° C.
  • scouring while relaxing is more preferable because it improves the elasticity.
  • the temperature of the heat set is from 120 to 190 ° C, preferably from 140 to 180 ° C, and the heat set time is 10 to 100 ° C. Seconds to 5 minutes, preferably 20 seconds to 3 minutes.
  • Staining is carried out at 70 to 150 ° C, preferably 90 to 120 ° C, and particularly preferably 90 to 100 ° C, without using a carrier. It can be carried out.
  • the cation When using dyes, metal or alkaline earth metals such as sodium sulfate, sodium nitrate, potassium sulfate, sulfate sulfate, etc. to improve the sharpness of the dyed material. It is particularly preferred to add a class of metal salts to the dye bath.
  • sorbing or reduction washing can be performed by a known method.
  • a mixed fabric consisting of a normal pressure dispersible dye-dyeable fiber and a polyurethan elastic fiber when mixed with stretch fiber
  • the reducing fiber is washed and the polyurethane is used. It is important to firmly remove the disperse dye that has contaminated the elastic fiber in order to improve the robustness of the fabric.
  • a reducing agent such as hydrosulfite sodium is dissolved in an aqueous solution of sodium carbonate such as sodium carbonate and sodium hydroxide.
  • the following is a special mention of the poly (methylene terephthalate) fiber of the present invention which can be dyed in a deep color with either a cationic dye or a disperse dye or both dyes at normal pressure.
  • the polymethylene terephthalate fiber of the present invention is a heat-resistant fiber such as stretch fiber, polyester, silk, and acetate represented by polyurethane elastic fiber.
  • a heat-resistant fiber such as stretch fiber, polyester, silk, and acetate represented by polyurethane elastic fiber.
  • polyurethane elastic fibers When mixed with fibers with low heat resistance, it can be dyed dark under normal pressure without impairing the performance of fibers with low heat resistance.
  • polymethylentelephthalate fibers are mixed with polyurethane elastic fibers, the softness and sunset are different from those of mixed fabrics using nylon fibers, Create a new sense of clothing that has easy-care characteristics
  • Polyurethane elastic fibers must be dyed at 110 ° C to 120 ° C for mixed fabrics of ordinary polymethylene terephthalate fibers and polyurethane elastic fibers. Thermal degradation. In addition, only with disperse dyes Does not stain. In the dyeing of the mixed fabric with the polyurethane elastic fiber by the disperse dye, the disperse dye is more exhausted by the polyurethane urethane fiber than by the polymethylene terephthalate fiber. Does not firmly adhere to the urethane elastic yarn fiber. For example, fiber disperse dyes are easily transferred by dry cleaning and washing, and stain the surrounding clothing.In some cases, the dyes are released and the color of the mixed fabric is faded, decreasing the color fastness. Let it. On the other hand, the above-mentioned problem has been solved by using the polytrimethylene terephthalate-based fiber of the present invention, which can dye either the cationic dye or the disperse dye or both dyes at normal pressure. it can.
  • the first method is to use the normal-pressure thione dye-dyeable polymethylene terephthalate fiber of the present invention.
  • Polyurethane elastic fibers are not dyed with cationic dyes. If polytrimethylene terephthalate fiber that can be dyed under normal pressure is used as the cationic dye, the above contamination will occur because only the polymethylene terephthalate fiber is selectively dyed. No problem.
  • the second method is the use of the normal pressure dispersible dyeable polymethylene terephthalate fiber of the present invention. If the polymethylene terephthalate fiber is modified to have normal pressure disperse dye dyeability, the transfer of the disperse dye to the polyurethan fiber can be considerably suppressed.
  • the fabric obtained using the polymethylene terephthalate fiber of the present invention is, for example, far more soft than a known mixed fabric of nylon fiber and polyurethane elastic fiber. There is no peculiar feeling unique to nylon fiber. In addition, it can be a new sensational garment with light stretch characteristics and excellent color development. Furthermore, polytrimethyl terephthalate-based fibers have a high heat setting property and are excellent in yellowing resistance. These properties indicate that there are no problems inherent to nylon fiber, and that it is easy to handle.
  • the polyester fiber of the present invention exhibits an excellent effect even when mixed with cellulose fiber.
  • a reactive dye is used for dyeing cellulose fibers
  • the reactive dye often decomposes when the temperature of the dye bath exceeds 100 ° C.
  • the poly (methylethylene terephthalate) fiber of the present invention it is possible to perform one-step, one-bath dyeing using a cation dye or a disperse dye and a reactive dye under normal pressure.
  • the fabric thus obtained is a new sensation garment having both the dry feeling unique to cellulose and the softness derived from polytrimethylene terephthalate.
  • the polyester fiber of the present invention can be applied alone to a woven or knitted fabric, and the obtained fabric is rich in softness and exhibits excellent stretch characteristics and coloring properties. Becomes If there is no problem with staining at 100 ° C. or more, it is also possible to stain at 100 ° C. or more. Further, as a characteristic of the polyester fiber of the present invention, the amount and speed of the weight loss can be industrially controlled in spite of being a cationic dye-dyeable fiber.
  • the polyester fiber of the present invention which has been reduced in alkali content, is further softened, and has micropores of several meters on the fiber surface, so that it has a dry feeling and can be dyed clearly. Can be issued.
  • the normal pressure disperse dye dyeable poly Ester fibers also have similar alkali weight loss characteristics.
  • the polytrimethylene terephthalate-based fiber of the present invention can be used for clothing such as outer garments, underwear, lining, sports, etc., as well as for raw yarn and core, It can also be used for materials such as ground and flocks.
  • the intrinsic viscosity [7?] was measured using an oste-ward viscosity tube at 35 ° C and o-chlorophenol.
  • the loss tangent (tan 5) and the dynamic elastic modulus at each temperature were measured using Orientec's Leo Vibron in dry air at a measurement frequency of 110 Hz and a heating rate of 5 ° C / min. It was measured. From the results, a loss tangent-one temperature curve was determined, and Tmax (° C), which is the peak temperature of the loss tangent, was determined on this curve.
  • the elastic modulus was measured according to JIS-L-113.
  • the measurement was carried out in a nitrogen stream of 100 milliliters Z min at a heating rate of 20 ° C./min using a DSC manufactured by SEIKO ELECTRONICS CO., LTD.
  • the peak value of the melting peak was used as the melting point.
  • the yellowness of the obtained fiber was measured using the b value.
  • the b value was measured using a color computer of Suga Test Instruments Co., Ltd. The yellowness increases as the b value increases.
  • the sample is a one-piece knitted fabric of polyester fiber (circular knit, sheeting, gauge 28), and score roll 400 (Kao Corporation, non-ion interface) Activator)
  • the sample was a piece of polyester fiber knitted fabric (circular knit, sheeting, gauge 28), using hot water (bath ratio 1:50) containing score roll 400 at 2 g / liter. It was scoured at 70 ° C for 20 minutes and dried with a tumble dryer. Then, a heat set at 180 ° C. for 30 seconds was performed using a pin tenter.
  • the dye is Telblue 3 RSF (manufactured by Nippon Kayaku Co., Ltd., disperse dye) was used at 6% 0 wf, and dyed at a bath ratio of 1:50 at 95 ° C for 60 minutes.
  • a dispersant 0.5 g / liter of Nikki Sansol (Nikka Chemical Co., Ltd., anionic surfactant) is used, and 0.25 milliliter of acetic acid is used.
  • the pH was adjusted to 5 by adding torr Z liter and 1 g Z liter of sodium acetate.
  • the exhaustion rate was determined by measuring the absorbance A of the dye stock solution and the absorbance a of the dye solution after dyeing using a spectrophotometer, and substituting into the following formula. The value at 580 nm, which is the maximum absorption wavelength of the dye, was used as the absorbance.
  • the lightness when dyed in black was evaluated using the L value.
  • the fastness test of the dyed fiber was evaluated using a single-mouth knitted fabric dyed by the method of (6).
  • Dry cleaning fastness is JIS-L-080
  • light fastness is JIS-L-0842
  • washing fastness is JIS-L-0844
  • dry and wet friction The fastness was measured in accordance with JIS-L-08449.
  • the dry cleaning fastness was tested for liquid contamination.
  • TMG Trimethylen glycol
  • DMT dimethyl terephthalate
  • SIPP sulphoisophthalic acid Trabutylphosphonium salt
  • the rate was 22 g Zd, and the elastic recovery rate was 87%.
  • the QZR value of the drawn yarn was 0.25, which satisfied expression (1).
  • the b value of the fiber was 6.1.
  • the exhaustion rate of the cationic dye of the polyester fiber obtained in this example at 95 ° C. and 30 minutes was as large as 72%, and a very clear dyed product was obtained.
  • polymethylethylene phthalate homopolymer was obtained without using SIPP.
  • the intrinsic viscosity of the obtained polymer was 0.63.
  • This polymer chip was spun and drawn in the same manner as in Example 1 to obtain a fiber.
  • the resulting fiber has a melting point of 23 ° C, Tmax of 11 ° C, a strength of 3.6 g / d, an elongation of 35%, an elasticity of 23 g / d, and an elastic recovery of 88%. Indicated.
  • the Q / R value of this fiber was 0.26, which satisfied the expression (1).
  • the exhaustion rate of the cation dye at 95 ° C. and 30 minutes of the polyester fiber obtained in this comparative example was 6%, and it could not be dyed in a deep color.
  • a polymer was prepared in the same manner as in Example 1 except that the copolymerization ratio of SIPP was 0.3 mol%, and spinning was performed. Table 1 summarizes the test and evaluation results of the obtained fibers.
  • the copolymerization ratio of the ester-forming sulfonate compound is less than 0.5 mol%, and the dye exhaustion rate of the dye at 95 ° C and 30 min at 30 ° C is 30%. Can't do it (Comparative Example 3)
  • Example 1 In the same manner as in Example 1, a fiber was prepared through polymerization and spinning with a copolymerization ratio of SIPP of 6 mol%. Table 1 summarizes the test and evaluation results. During the spinning of this polymer, thread breakage occurred frequently and the spinnability was poor. When the fiber was dyed at 95 ° C, the yarn shrank and became hard, and a fabric with a good texture could not be obtained. Further, the dry cleaning fastness of the obtained fabric was lower than that of Example 1.
  • Example 1 the stretching ratio was 3.3 times.
  • the orientation of the obtained fiber was too advanced, and T max exceeded 115 ° C.
  • the exhaustion rate of the cationic dye was 45%.
  • fluff was frequently generated in the obtained fiber.
  • Example 2 Polymerization and spinning were carried out in the same manner as in Example 1 except that the temperature of the hot roll was 25 ° C. Many yarn breaks occurred during drawing, and fibers could not be obtained continuously. Polymerization and spinning were performed in the same manner as in Example 1 except that the temperature of the hot roll was set at 80 ° C. At the time of drawing, the yarn was fused to the hot roll, and single yarn breakage occurred frequently, and the obtained fiber was full of fluff. U% was 3.2, which was bad.
  • Example 2 Polymerization and spinning were carried out in the same manner as in Example 1 except that the temperature of the hot plate was 70 ° C. Fibers were obtained without problems such as yarn breakage and fluffing. However, the obtained fiber had a low elastic recovery of 55% and a QZR value of 0.49, which did not satisfy the expression (1).
  • Polymerization / spinning was performed in the same manner as in Example 1 except that the temperature of the hot plate was set at 200 ° C. The fiber was cut at the hot plate and could not be drawn.
  • Polymerization / spinning was performed in the same manner as in Example 1 except that the draw ratio was 2.3 times and the temperature of the hot plate was 180 ° C. Fibers were obtained without problems such as yarn breakage and fluffing. However, the obtained fiber had a low elastic recovery rate of 48%, a QZR value of 0.52, and could not satisfy the expression (1).
  • Spinning was performed using poly (ethylene terephthalate) fiber obtained by copolymerizing 2.5% by mole of 5-sodium sulfoisophtalic acid.
  • the obtained fiber had a strength of 4.2 g Zd, an elongation of 30%, an elasticity of 100 g / d, an elastic recovery of 31%, a QZR value of 3.2, and a Tmaxl of 31 ° C. Show, Katyo The exhaustion rate of the dye at 95 ° C. and 30 minutes was 36%.
  • Example 1 was repeated without using cobalt acetate and trimethyl phosphite. In this case, there was no change in the fiber properties, but the b value of the fiber was 11.2, which turned yellow.
  • Example 2 The polymer obtained in Example 2 was dried to a water content of 50 ppm, melted at 285 ° C, and spinned into a single array having 0.23 mm diameter and having 36 holes. Extruded through mouth. The extruded molten multifilament is passed through a heat retaining area with a length of 5 cm and a temperature of 100 ° C, and then quenched by blowing air at a wind speed of 0.4 m / min to obtain a solid multifilament. I changed it to a comment.
  • this solid multifilament was heated to 60 ° C, and the first roll was at a speed of 210 m / min, and the rotary speed was heated to 133 ° C, 4300 m / min Then, hot stretching and heat setting were performed between the second rolls, and then the film was wound at 418 m / min.
  • the obtained fiber was made into a double yarn and made 75 d / 72 f.
  • the obtained fiber has a strength of 3.1 g Zd, an elongation of 41%, a U% of 0.7%, an elasticity of 22 gZd, a sexual recovery rate of 89%, a Q / R of 0.25,
  • the exhaustion rate of the cationic dye at Tmax 109 ° C, 95 ° C, and 30 minutes was 98%, and the b value was 6.5.
  • a warp knitted fabric was formed using the polyester fiber of Example 1 and a loyal force of 210 denier (polyurethane stretch fiber manufactured by Asahi Kasei Kogyo Co., Ltd.).
  • the knitting gauge is 28 G
  • the polyester fiber is 108 mm / 480 course of polyester fiber
  • stretch fiber strength is 12 mm / 480 course
  • driving is performed.
  • the density was 90 courses Z inch.
  • the mixing ratio of the polyester fiber was set to 75.5%.
  • the obtained greige was subjected to relax scouring for 90 minutes and a dry heat set at 160 ° C for 1 minute.
  • Disperse TL Non-ionic activator manufactured by Meisei Chemical Co., Ltd.
  • KYARILL BLACK BS-ED cationic dye manufactured by Nippon Kayaku Co., Ltd.
  • Using a liter add 50 g of sodium sulfate and 15 g / liter of sodium carbonate, and dye by adding a dye to an aqueous solution whose pH has been adjusted to 11. Liquid. Staining was performed at 95 ° C. for 1 hour at a staining concentration of 8% 0 wf and a bath ratio of 1:50.
  • Granup P manufactured by Sanyo Kasei Kogyo Co., Ltd., non-ionic surfactant 1 g Z liter, bath ratio 1: 50, 80 ° C. for 10 minutes.
  • finishing was performed by a conventional method.
  • the obtained dyed product had an L value of 11.2, which was sufficiently dyed.
  • the dyeing fastness of the dyed materials is from the washing fastness class 5, the wet rub fastness class 5, and the light fastness class 4.
  • the dyed knitted fabric was soft, rich in stretch, and had an excellent texture with tightness and waist.
  • Example 9 The same operation as in Example 9 was repeated using the polyester fiber of Example 2.
  • the L value of the obtained dyed product was 10.9, indicating that it was sufficiently dyed.
  • the dyeing fastness of this dyed product was 5 for washing fastness, 5 for wet rub fastness, and 4 to 5 light fastness.
  • the dyed material was soft, rich in stretchiness, and had an excellent texture with a firm and firm feel.
  • Example 9 The same knit as in Example 9 was knitted using the polymethylene terephthalate fiber prepared in Comparative Example 1.
  • the obtained greige was subjected to relax scouring at 90 ° C for 2 minutes and subjected to a dry heat set at 160 ° C for 1 minute.
  • To dye in a dark color use Dynix Black BG-FS (Disperse Dye, manufactured by Dystar Japan) 8% 0 wf, and add 0.5 g / In the presence of a little, the pH was adjusted to 6 with acetic acid, and the cells were stained at a bath ratio of 1:30 at 95 ° C for 60 minutes.
  • the wet rub fastness of the obtained dyed product was of the second grade, and the release of the disperse dye contaminating the stretch fiber was observed.Similar to Example 9 using the fiber prepared in Comparative Example 9 Was repeated.
  • the resulting fabric was clearly hard and was dyed only in a light color with an L value of 21.
  • a warp knitted fabric of nylon 6 fiber and Roy force spun by the usual method was prepared in the same manner as in Example 9, and was prepared by using Callon Black BGL (manufactured by Nippon Kayaku Co., Ltd.). Dye) at 7% 0 wf at 100 ° C. for 60 minutes. The lightfastness of the obtained dyed fabric was 2 to 3.
  • a 75-dZ36f polyester fiber obtained in the same manner as in Example 1 was used for warp and a 75-d / 44-f cuprammonium rayon for the weft, to give a plain weave (140-w / 25.4 mm, weft 80 / 25.4 mm).
  • This plain fabric was scoured by a conventional method. After washing with water, 180 ° C, 3
  • one-step one-bath dyeing with a cationic dye and a reactive dye was performed without using a carrier.
  • the cation dyes used were KYRILLIL BLACK BS-ED (Cation dyes, manufactured by Nippon Kayaku Co., Ltd.) and Dori Maleble X-SGN (Sand Co., Ltd., reactive dyes). .
  • the dispersant used was Dispar TL (manufactured by Meisei Chemical Co., Ltd.) at a rate of 1 g / liter, 50 g of sodium sulfate and 15 g / liter of sodium carbonate. The dye was added to the aqueous solution whose pH was adjusted to 11 to obtain a dye solution.
  • Staining was performed at 100 ° C. for 1 hour at a concentration of 2% 0 wf and a bath ratio of 1:50. After staining, the granules were soaked in Granup P (manufactured by Sanyo Chemical Industry Co., Ltd.) at 1 g / liter and a bath ratio of 1:50 at 80 ° C. for 10 minutes. staining After that, finishing was performed by a conventional method. The obtained dyed product was uniformly dyed and was a clear dyed product. K / S was 24.3. In addition, despite the fact that the alkali weight reduction treatment performed with ordinary polyester fibers was not performed, the fabric was full of soft texture and dryness, and had an excellent texture that cannot be obtained with conventional fabrics. The dry cleaning fastness was grade 5, the wet friction fastness was grade 5, and the light fastness was grade 4.
  • Example 2 Using 75 d / 36 f polyester fiber obtained in the same manner as in Example 1, a plain woven fabric was prepared using the same weft and warp yarns, and dyed. Although the obtained fabric did not have a dry feeling, it was extremely soft and the fabric showed a stretch property of about 7% in the weft direction.
  • Example 1 The fiber obtained in Example 1 was copolymerized and spun in the same manner as in Example 1, and copolymerized with 3% by mole of polyethylene terephthalate fiber and sodium 5-naphthalomisophthalate.
  • a weight loss test was carried out using a single-knit fabric (circular knit, sheeting, gauge 28) prepared from the prepared polyethylene terephthalate fiber. After knitting, the knitted fabric is scoured at 70 ° C for 20 minutes using warm water containing score roll 400 at 2 g / liter, dried with a tumble dryer, and then dried. A heat set at 180 ° C. for 30 seconds using a pin tenter was used.
  • Alkali weight reduction processing was carried out by placing the bite knitted fabric in a 6% by weight aqueous solution of sodium hydroxide boiled for 20 minutes.
  • the alkali weight loss rate was evaluated by dividing the weight of the knitted fabric reduced by the weight loss by the weight of the original knitted fabric.
  • the weight loss rates of the single-port knitted fabric of the fiber obtained in Example 1 and the single-port knitted fabric of polyethylene terephthalate fiber were 25.4% by weight and 10.3% by weight, respectively.
  • the polyester fiber of the present invention exhibits a weight loss rate close to that of polyethylene terephthalate fiber. did.
  • Example 12 In the same manner as in Example 12 using a one-piece knitted fabric obtained by knitting polyethylene terephthalate fiber obtained by copolymerizing sodium 5 sodium sodium sulfophthalate at 3 mol% in the same manner as in Example 12 When the weight was reduced, the knitted fabric was completely decomposed, dissolved and disappeared. Therefore, in the case of polyethylene terephthalate fiber obtained by copolymerizing 3% by mole of sodium 5-sodium sulfoisophtalate, it is practically impossible to reduce the weight loss rate because the rate of weight loss is too fast. It is possible.
  • a fiber was prepared by copolymerizing 2 mol% of dimethyl sodium 5-dimethylsophthalate and 5 wt% of dimethyl ethyl adipate.
  • the physical properties of the fiber are as follows: melting point: 220 ° C, strength: 3.6 g / d, elongation: 34%, elasticity: 22 g Zd, elastic recovery: 90%, and R value of 0.2 It was five.
  • the exhaustion rate of the cationic dye at 95 ° C and 30 minutes of the polyester fiber obtained in this example was 95%, and the exhaustion rate of the disperse dye at 95 ° C and 60 minutes. Showed high dyeability at 95% for both cationic dyes and disperse dyes at normal pressure.
  • the dry cleaning fastness of the one-necked knitted fabric after dyeing did not show any fading of the dyed material, and the cation dye and the disperse dye were in the 4th to 5th class of liquid contamination.
  • the light fastness (four to five grades), dry / wet friction fastness (five grades), and washing fastness (five grades) of the fibers were also good.
  • Example 2 The fiber obtained in Example 2 was cut to obtain a short fiber having a fiber length of 39 mm. .
  • a 20 d / 2 f filament obtained in the same manner as in Example 2 was used as a core, and the short fibers were arranged in a sheath.
  • the filament mixture was 11 wt%.
  • Yarn was obtained.
  • the composite yarn was woven into a warp (weaving density: 144, Z25.4 mm) and weft (weaving density: 77, Z25.4 mm) woven fabrics, and was woven according to the method of Example 9. Staining was performed at ° C.
  • the KZS of the dyed fabric was dyed deep at 25.3.
  • the obtained fabric was excellent in tension, waist, and resilience.
  • Example 2 The polymer obtained in Example 2 was subjected to solid-state polymerization in nitrogen at 200 ° C. for 24 hours to obtain a polymer having an intrinsic viscosity of 1.0.
  • the spinning was carried out in the same manner as in Example 1, and the strength was 4.0 (5, elongation 32%, 11% 1.0%, elastic modulus 23 g Zd, elasticity recovery rate 91%, QZR value A fiber having physical properties of 0.25, T maxll O ° C, and b value of 4.3 was obtained.
  • 4G 1,4-butanediol
  • DMT 130 parts by weight 1,4-butanediol
  • titanium tetrabutoxide 1.3 parts by weight
  • the intrinsic viscosity of the obtained polymer was 0.8.
  • the 4G component in the polymer measured by using NMR was 4.1% by weight.
  • a spinning temperature of 265 ° C and a spinning speed of 1200 were used using a spinning hole having 36 round cross-section holes (diameter: 0.23 mm).
  • An undrawn yarn was prepared by spinning at m / min.
  • the obtained undrawn yarn is hot-rolled 60. C, a hot plate was applied at 140 ° C, a draw ratio of 2.9 times, and a draw speed of 600 mZmin was used to obtain a drawn yarn of 50 d / 36 f.
  • Fiber properties are as follows: melting point: 2 24 ° C, Tma x 98 ° C, strength 3.6 g Zd, elongation 40%, U% 1.2%, elastic modulus 23 g / d, elastic recovery 83%, b value 4.5 .
  • the QZR value of this fiber was 0.28, thereby satisfying the expression (1).
  • the exhaustion rate of the polyester fiber of this example at 95 ° C. and 60 minutes by the disperse dye was 78%, indicating a high exhaustion rate.
  • Example 13 Polymerization / spinning was performed in the same manner as in Example 16 except that the ratio of TMG to 4G was changed. The results are shown in Table 2. The proportion of the 4G component was less than 1.5% by weight and the Tmax of the fiber was 106 ° C. The exhaustion rate by the disperse dye at 95 ° C and 6 minutes was low, and it was not possible to dye in a dark color.
  • Polymerization / spinning was performed in the same manner as in Example 16 except that the ratio of TMG to 4G was changed.
  • Table 2 shows the physical properties and evaluation results of the obtained fibers.
  • the ratio of the 4G component was 10.3% by weight.
  • the Tmax of the fiber was 85 ° C or less, and the exhaustion rate was high, but the dry cleaning fastness was very low at class 1.
  • Hexamethylen glycol (hereinafter abbreviated as 6G) was used in place of 4G, and polymerization and spinning was performed in the same manner as in Example 16 except that the ratio of TMG to 6G was changed.
  • Table 2 shows the test and evaluation results of the obtained fibers.
  • the proportion of the 6G component of the polymer was 8.7% by weight.
  • the Tmax of this fiber was 85 ° C or less, and when dyed at 95 ° C for 60 minutes, the exhaustion rate exceeded 70%.
  • the ruggedness was very poor at 1st grade.
  • the melting point of the fiber was as low as 210 ° C., and when processing such as false twisting was performed, the yarn was fused to the heater and processing could not be performed.
  • Example 16 Polymerization was carried out in the same manner as in Example 16 except that cyclohexanedimethanol (hereinafter abbreviated as C6-12G) was used instead of 4G and the ratio of TMG to C6-2G was changed. ⁇ Spinning was performed. The results are shown in Table 2. The ratio of the C 6 -2G component was 12.6% by weight. However, the elastic modulus of this yarn was 24 g Zd, the elastic recovery was 34%, and the QZR value was 0.71, which did not satisfy the expression (1). The fabric obtained from this yarn had poor elastic recovery. The Tmax of the fiber was 62 ° C. When dyed at 95 ° C for 60 minutes, the fabric shrank and became hard.
  • C6-12G cyclohexanedimethanol
  • Example 17 Polymerization spinning was carried out in the same manner as in Example 16 except that ethylene glycol (hereinafter abbreviated as 2G) was used instead of 4G and the ratio of TMG to 2G was changed. The results are shown in Table 2.
  • the obtained polymer is colored yellow, and the obtained fiber is also colored yellow with a b value of 18.3, and should be used for uses such as inner whiteners that require whiteness. Can not be done.
  • a warp knitted fabric was prepared using the polyester fiber of Example 16 and a 210 denier Roy force (polyurethane-based stretch fiber manufactured by Asahi Kasei Corporation).
  • the knitting gauge of this knitted fabric is 28 G, the loop length is 1800 mm / 480 course for polyester fiber, and 11 mm / 480 course for stretch fiber.
  • the implantation density was 90 courses Z inch.
  • the mixing ratio of the polyester fiber was set at 75.5%.
  • the obtained greige was subjected to relax scouring at 90 ° C for 2 minutes and subjected to a dry heat set at 160 ° C for 1 minute.
  • 8% owf of Dianix Black BG-FS Disperse Dye manufactured by Daiichi Yuichi Japan Co., Ltd.
  • 0.5 g / liter of Nikka Sun Salt 1200 as a dyeing aid.
  • the pH was adjusted to 6 with acetic acid, and the cells were stained at a bath ratio of 1:30 at 95 ° C for 60 minutes.
  • the black lightness L value of the obtained dyed product was 11.7, which was sufficient for coloring.
  • the dyed product has a washing fastness of 5, a wet rub fastness of 4, and a light fastness of 4, and has a soft, stretchy, tight, and firm feel.
  • a warp-knitted fabric of nylon 6 fiber spun by a conventional method and Roy force was prepared in the same manner as in Example 22 and calo black BGL (Nippon Kayaku Co., Ltd.) was used as the acid dye.
  • calo black BGL Nippon Kayaku Co., Ltd.
  • the L value of the obtained dyed product was 12.3.
  • the lightfastness of this fabric was 2 to 3.
  • a plain woven fabric (weaving density 1 40 lines Z25.4 mm, Latitude 80 lines / 25.4 mm). This plain fabric was scoured and made into a mass by a conventional method. The mercerization process was performed at room temperature by immersion in a 75% sodium hydroxide aqueous solution.
  • the dye was added to the aqueous solution in which H was adjusted to 11 to obtain a dye solution.
  • Dyeing was performed at 95 ° C. for 1 hour at a dye concentration of 2% owf and a bath ratio of 1:50.
  • the sample was rubbed with Granup P (manufactured by Sanyo Chemical Co., Ltd., nonionic surfactant) at 1 g / liter and a bath ratio of 1:50 at 80 ° C. for 10 minutes.
  • the obtained dyed product was uniformly dyed, had a soft texture, had a dry feeling, and had a good texture not seen in conventional fabrics.
  • the dyed product had a K / S of 22.7, a dry cleaning fastness of 3 to 4, a wet rub fastness of 4, and a light fastness of 4.
  • Example 24 Using a 75 d / 36 f polyester fiber obtained in the same manner as in Example 16, a similar plain woven fabric was prepared using the same weft and warp yarns and dyed. Although the obtained fabric had no dry feeling, the fabric was extremely soft and showed a stretch property of about 7% in the weft direction. (Example 24)
  • a twist of 300 TZm was applied to the polyester fiber of Example 16 and glued with a roller. Then, the warp was used, and diacetate (100 d / 150 f) was used for the weft.
  • a plain woven fabric 120 warps / 25.4 mm, weft 80 warp Z25.4 mm was woven.
  • Nippon Kayaku Polyesterable RSRS manufactured by Nippon Kayaku Co., Ltd.
  • Nyakuhon Kabushiki Kaisha RD 200 (Nippon Kayaku) as a disperse dye for diacetate (Manufactured by Sharp Corporation).
  • the dye concentration was 5% owf for each step, and one-step single-bath dyeing was carried out at 95 ° C in the presence of a dispersant with weak acidity. After staining, soda ash 1 g Z liter, nonionic detergent 0.5 g Z liter 70 in a weak alkaline bath. C. Soaking was performed for 20 minutes.
  • the K / S of the obtained dyed product was excellent, 22.2.
  • the dyed product had a dry cleaning fastness of 3 to 4th grade, a light fastness of 4th grade, a soft texture and excellent clarity.
  • Transesterification was carried out at 220 ° C using 117 parts by weight of DMT, 130 parts by weight of dimethyl isophthalate, 1.3 parts by weight of TMG 763 parts, and 1.3 parts by weight of titanate laboxide. Thereafter, 0.01 part of trimethyl phosphate was further added, and polycondensation was performed at 260 ° C. at a reduced pressure of 0.5 t 0 rr to obtain a polymer. The intrinsic viscosity of the obtained polymer was 0.8.
  • the isophthalic acid component in the polymer measured by NMR was 6.2% by weight.
  • a spinning temperature of 265 ° C and a spinning speed of 1200 were used using a spinning hole having 36 round cross-section holes (diameter: 0.23 mm).
  • An undrawn yarn was prepared by spinning at m / min. Then, the obtained undrawn yarn was heated at a hot roll of 60 ° C, a hot plate of 140 ° C, Stretching was performed at a draw ratio of 2.9 and a draw speed of 600 m / min to obtain a drawn yarn of 50 d / 36 f.
  • the physical properties of the fiber are as follows: melting point: 21.9 ° C, Tmax: 100 ° C, strength: 3.5 g / d, elongation: 43%, U%: 1.0%, elastic modulus: 24 gd, elastic recovery
  • the b value was 7.6%
  • the b value was 7.6.
  • the Q / R value of the fiber was 0.29, which satisfied Expression (1).
  • the polyester fiber of this example had an exhaustion rate of 81% with a disperse dye at 95 ° C for 60 minutes, indicating a high exhaustion rate.
  • the dry-cleaning fastness of the one-necked knitted fabric after dyeing did not show any fading of the dyed material, and the liquor contamination was grade 3.
  • the dyeing fastness of the dyed product was good in light fastness (grade 4 to 5), dry / wet rub fastness (grade 5), and wash fastness (grade 5).
  • Example 25 was repeated, except that the copolymerization ratio of dimethyl isophthalate was changed. Table 3 shows the test and evaluation results of the obtained fibers. In Comparative Example 19, the copolymerization ratio was too low, resulting in inferior dyeability of the fibers. In Comparative Example 20, the copolymerization ratio was too high, resulting in a decrease in dry cleaning fastness.
  • Example 25 Dimethyl isophthalate 6.2 219 0.80 3.5 43 24 82 0.29 100 1.0 81 3 7.6
  • Example 26 Dimethyl isophthalate 5.2 224 0.81 3.5 43 24 75 0.43 102 0.8 75 4 7.5
  • Example 27 Isophthalic acid Dinutyl 7.4 216 0.75 3.4 42 20 83 0.25 96 1.0 91 3 7.3
  • Example 28 Dimethyl succinate 4.0 222 0.80 3.5 42 22 85 0.28 92 1.1 85 38.2
  • Example 29 Dimethyl adipate 5.3 222 0.77 3.5 41 23 90 0.23 89 1.2 96 3 9.6
  • Example 30 di- / chill sebacate 7.8 210 0.80 3.0 44 22 86 0.19 85 1.1 96 3 9.5
  • Example 31 1,4-six ⁇ -hexane 6.0 220 0.80 2.2 42 23 87 0.21 85 1.2 90 3 9.0
  • Example 29 was repeated without using trimethyl phosphite. Although the fiber properties of the obtained fiber did not change, the b value of the fiber was 12.3, which turned slightly yellow.
  • a warp knitted fabric was prepared using the polyester fiber of Example 25 and a loyal force of 210 denier (polyurethane stretch fiber manufactured by Asahi Kasei Corporation).
  • the knitting gauge is 28 GG
  • the loop length is 1800 mm / 480 course of polyester fiber
  • the stretch fiber strength is 11 mm / 480 course
  • the driving density is 9 0 course Z inch.
  • the mixing ratio of polyester fiber was set at 75.5%.
  • the obtained greige was relaxed and scoured at 90 ° C for 2 minutes, and dried and set at 160 ° C for 1 minute.
  • the pH was adjusted to 6 with acetic acid in the presence of 0.5 g Z-liter, and staining was carried out at a bath ratio of 1:30 at 95 ° C for 60 minutes.
  • the black lightness L value of the obtained dyed product was 11.3, which was sufficient for color development. Washing fastness of the dyed product was class 5, wet rub fastness was class 4, and light fastness was class 4. In addition, the dyed product was soft and rich in stretch feeling, and had a firm and waisted texture.
  • Transesterification was carried out at 220 ° C using DMT 130 parts by weight, TMG 112 1 parts by weight, titanyl tributoxide 1.3 parts by weight, and cobalt acetate 0.01 parts by weight. Thereafter, 69 parts by weight of polyethylene glycol having an average molecular weight of 1000 and 0.01 part by weight of phosphoric acid were added, and the mixture was decompressed at 260 ° C under a pressure of 0.5 t0 rr. The polymer was obtained by polycondensation. The intrinsic viscosity of the obtained polymer was 0.82. The copolymerization ratio of polyethylene glycol having an average molecular weight of 1,000 was 5% by weight. After drying the obtained polymer chip, a spinning temperature of 26 ° C. and a spinning speed of 1 using a spinning hole having 36 round cross-section holes (0.23 mm) were used.
  • An undrawn yarn was prepared by spinning at 200 m / min. Next, the obtained undrawn yarn was drawn at a hot roll of 50 ° C, a hot plate of 140 ° C, a draw ratio of 2.9 times, and a drawing speed of 60 Om / min. /
  • a 36 f drawn yarn was obtained.
  • the physical properties of the fiber are as follows: Melting point: 23 ° C, Tmax: 92 ° C, strength: 3.1 g / d, elongation: 43%, U%: 1.1%, elastic modulus: 20 g Zd, elasticity The recovery rate was 89% and the b value was 8.2. In addition, the QZR value of the fiber was 0.22, thereby satisfying the expression (1).
  • Example 33 The same operation as in Example 33 was repeated, while changing the copolymerization ratio of polyethylene glycol. Table 4 shows the results. In Comparative Example 23, the copolymerization ratio was too low and the dyeability was insufficient, and in Comparative Example 24, the copolymerization ratio was too high and the dry cleaning fastness was poor. Also the whiteness of the fiber Also fell.
  • PEG polyethylene glycol
  • Example 33 A warp knitted fabric was prepared using the polyester fiber of Example 3 and a loyal force of 210 denier (polyurethane-based stretch fiber manufactured by Asahi Kasei Corporation).
  • the gauge is 28 G
  • the loop length is 108 mm / 480 course of polyester fiber
  • the stretch fiber strength is 112 mm / 480 course
  • the driving density is 9 0 course Z 25.4 mm.
  • the mixing ratio of the polyester fibers was set at 75.5%.
  • the obtained greige was relaxed and scoured at 90 ° C for 2 minutes, and dried and set at 160 ° C for 1 minute.
  • 8% owf of Dyanix Black BG-FS (manufactured by Dyster Japan) and 0.5 g of Nitukasan Sonoret 1200, which is a dyeing aid, with 0.5 g of Z-Little The pH was adjusted to 6, and staining was carried out at a bath ratio of 1:30 at 95 ° C for 60 minutes.
  • the black lightness L value of the obtained dyed product was 11.0, and the color was sufficiently developed.
  • the washing fastness of the fiber was grade 5, the wet rub fastness was grade 4, and the light fastness was grade 4.
  • the dyed fabric had a soft and stretchy feel, and had a tight and waisted texture.
  • Polymethylene terephthalate having an intrinsic viscosity of 0.9 and polybutylene terephthalate having an intrinsic viscosity of 1.0 are mixed at a ratio of 94.8: 5.2 and extruded as it is. Then, in the same manner as in Example 17, polymethylene terephthalate fiber obtained by copolymerizing 5.2% by weight of 1,4-butanediol was obtained.
  • the obtained fiber is almost equivalent to the fiber of Example 17 and has a strength of 3.6 g d, an elongation of 43%, a U% of 0.7%, an elasticity of 23 g / d, and an elastic recovery.
  • Example 43 Weaving a plain woven fabric (40 warp yarns) using the 75 d Z 36 f polyester fiber obtained in Example 1 as a warp yarn and a 75 d / 44 mm copper ammonia rayon as a weft yarn / 25.4 mm, latitude 80 lines ⁇ 25.4 mm).
  • This plain fabric was scoured by a conventional method. After washing with water and pre-setting at 80 ° C. for 30 seconds, one-step one-bath dyeing with a cation dye and a reactive dye was performed without using a carrier.
  • Cryacryl Black BS-ED (Cation Dye manufactured by Nippon Kayaku Co., Ltd.) and Drimaremble X-SGN (Reactive Dye manufactured by Sand Co., Ltd.) were used.
  • DISPER TL Dispersant manufactured by Meisei Chemical Co., Ltd.
  • the dye was added to the aqueous solution whose pH was adjusted to 11 to obtain a dye solution.
  • Dyeing was carried out at 100 ° C. for 1 hour at a dye concentration of 2% owi and a bath ratio of 1:50. After staining, the sample was soaked at 80 ° C. for 10 minutes at 1 g / liter, Granup P (manufactured by Sanyo Chemical Industries, Ltd.) at a bath ratio of 1:50. After dyeing, finishing was performed by a conventional method.
  • the obtained dyed product was uniformly dyed, was excellent in wet rub fastness, dry cleaning fastness, and light fastness, and was a clear dyed product.
  • the texture was full of soft texture and dry feeling, and was an excellent texture that cannot be obtained with conventional woven fabrics.
  • the same plain woven fabric was woven and dyed using 75 d / 36 f polyester fiber obtained in the same manner as in Example 1, using the same warp and weft. Although the obtained fabric did not have a dry feeling, it was extremely soft and the fabric exhibited a stretch property of about 7% in the weft direction.
  • Example 43 when dyeing was performed at a temperature of 130 ° C., the reactive dye was decomposed, and the fabric was darkened.
  • Example 4 Weaving a plain fabric using the 75 d / 36 f polyester fiber obtained in Example 1 for warp and weft (140 warp / 3.54, warp 80 / 2.54 ) did. After scouring the plain fabric by a conventional method, the alkali weight was reduced by 20% using a 10% aqueous sodium hydroxide solution. Thereafter, the same pre-setting and staining as in Example 43 were performed, and finally a final set was performed at 180 ° C. for 30 seconds.
  • the obtained fabric showed a soft and dry feeling that was not seen before, and also showed a stretch property of about 7% in the weft direction.
  • the poly (methylen terephthalate) fiber of the present invention can be dyed at ordinary pressure with either a dye or a disperse dye or both dyes to a color density (shades) practically required.
  • the polymethylene terephthalate-based fiber of the present invention has an Ossian de-air property similar to general-purpose polyester fibers such as polyethylene terephthalate fiber, dimensional stability, yellowing resistance, and the like. It is a fiber material that has a dry feel and a workability for reducing weight, and has flexibility similar to nylon fibers.
  • the polytrimethylene terephthalate fiber of the present invention can be used for heat-resistant fibers such as stretch fibers typified by polyurethane elastic fibers, wool, silk, and acetate. It is a suitable fiber material for the production of fast-dyed fabrics mixed with low-strength fiber materials and cellulosic fibers dyed at normal pressure.
  • a robust dyeing fabric can be manufactured by a simple dyeing method using a general-purpose normal-pressure dyeing facility without impairing the properties of the fiber. It is an industrial utility to be noted.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
  • Polyesters Or Polycarbonates (AREA)
  • Materials For Medical Uses (AREA)
  • Nonwoven Fabrics (AREA)

Abstract

Fibre de polyester préparée à partir d'un polyester préparé par copolymérisation de terephtalate de polytriméthylène avec un troisième constituant qui est un composé de sulfonate formant un ester, mis en application selon un rapport de comonomère de 0,5 à 5 % molaire. La température de crête de la perte tangente de la fibre est de 85 à 115 °C et le rapport entre le module d'élasticité, Q (g/d) et la récupération élastique, R (%), de la fibre répond à 0,18 ≤ Q/R ≤ 0,45. On peut teindre cette fibre en profondeur à la pression atmosphérique et elle permet de teindre rapidement des textiles préparés par mélange de cette fibre avec un matériau fibreux faiblement résistant à la chaleur, tel qu'une fibre étirée, de la laine, de la soie et une fibre d'acétate caractérisée par une fibre élastique de polyuréthanne. On peut effectuer la teinture de ce textile mélangé à la pression atmosphérique, de sorte que les propriétés du matériau fibreux mélangé faiblement résistant à la chaleur sont moins susceptibles de se détériorer en cours de teinture. On peut soumettre cette fibre de polyester à un traitement alcalin de perte de poids, son toucher à sec est doux et riche et elle autorise une large palette de coloration.
PCT/JP1998/003660 1997-08-18 1998-08-18 Fibre de polyester et textile prepare au moyen de cette fibre WO1999009238A1 (fr)

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US09/485,938 US6652964B1 (en) 1997-08-18 1998-08-18 Polyester fiber and fabric prepared therefrom
KR1020007001596A KR100359347B1 (ko) 1997-08-18 1998-08-18 폴리에스테르 섬유 및 그것을 사용한 포백
JP51302799A JP3226931B2 (ja) 1997-08-18 1998-08-18 ポリエステル繊維及びそれを用いた布帛
EP98937854A EP1006220A4 (fr) 1997-08-18 1998-08-18 Fibre de polyester et textile prepare au moyen de cette fibre

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001044345A1 (fr) * 1999-12-15 2001-06-21 Asahi Kasei Kabushiki Kaisha Polytrimethylene terephtalate modifie
US6316586B1 (en) 2000-08-15 2001-11-13 E. I. Du Pont De Nemours And Company Copolyether composition and processes therefor and therewith
US6479619B1 (en) 2001-03-15 2002-11-12 E. I. Du Pont De Nemours And Company Sulfoisophthalic acid solution process therewith
US6706852B2 (en) 2002-07-02 2004-03-16 E. I. Du Pont De Nemours And Company Partially ester-exchanged SIPM and process therewith
WO2011048888A1 (fr) * 2009-10-20 2011-04-28 帝人ファイバー株式会社 Fibres de polyester, procédé pour la production de fibres de polyester, tissu, produit en fibres, et article moulé en polyester
WO2012178094A1 (fr) 2011-06-23 2012-12-27 E. I. Du Pont De Nemours And Company Nanoparticules modifiées, leur préparation et leur utilisation pour améliorer l'aptitude d'un substrat fibreux à la teinture par un colorant cationique

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US6331264B1 (en) 1999-03-31 2001-12-18 E. I. Du Pont De Nemours And Company Low emission polymer compositions
US6576340B1 (en) 1999-11-12 2003-06-10 E. I. Du Pont De Nemours And Company Acid dyeable polyester compositions
US6312805B1 (en) 2000-02-11 2001-11-06 E.I. Du Pont De Nemours And Company Cationic dyeability modifier for use with polyester and polyamide
CN1193120C (zh) * 2000-07-14 2005-03-16 帝人株式会社 聚酯纤维
US6331606B1 (en) 2000-12-01 2001-12-18 E. I. Du Pont De Nemours And Comapny Polyester composition and process therefor
WO2009079499A1 (fr) * 2007-12-18 2009-06-25 Shell Oil Company Fibre polymère contenant un ignifuge, son processus de production, et matériau contenant de telles fibres
KR101125253B1 (ko) * 2011-10-28 2012-03-21 주식회사 지클로 음이온 고분자 염과 셀룰로오스로 조성되는 스킨-코어 섬유 및 이의 제조방법

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JPH08269820A (ja) * 1995-04-04 1996-10-15 Asahi Chem Ind Co Ltd 易染性の改質ポリエステル繊維およびその製造方法

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JPH05302211A (ja) * 1992-04-21 1993-11-16 Kuraray Co Ltd 易染性ポリエステル繊維
JPH0770856A (ja) * 1993-09-02 1995-03-14 Toyobo Co Ltd ポリエステル被覆弾性糸
JPH08269820A (ja) * 1995-04-04 1996-10-15 Asahi Chem Ind Co Ltd 易染性の改質ポリエステル繊維およびその製造方法

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* Cited by examiner, † Cited by third party
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WO2001044345A1 (fr) * 1999-12-15 2001-06-21 Asahi Kasei Kabushiki Kaisha Polytrimethylene terephtalate modifie
EP1245604A1 (fr) * 1999-12-15 2002-10-02 Asahi Kasei Kabushiki Kaisha Polytrimethylene terephtalate modifie
EP1245604A4 (fr) * 1999-12-15 2003-01-29 Asahi Chemical Ind Polytrimethylene terephtalate modifie
US6645619B2 (en) 1999-12-15 2003-11-11 Asahi Kasei Kabushiki Kaisha Modified polytrimethylene terephthalate
CN1322182C (zh) * 1999-12-15 2007-06-20 旭化成株式会社 共聚聚对苯二甲酸亚丙基酯纤维及其制品
US6316586B1 (en) 2000-08-15 2001-11-13 E. I. Du Pont De Nemours And Company Copolyether composition and processes therefor and therewith
US6479619B1 (en) 2001-03-15 2002-11-12 E. I. Du Pont De Nemours And Company Sulfoisophthalic acid solution process therewith
US6706852B2 (en) 2002-07-02 2004-03-16 E. I. Du Pont De Nemours And Company Partially ester-exchanged SIPM and process therewith
WO2011048888A1 (fr) * 2009-10-20 2011-04-28 帝人ファイバー株式会社 Fibres de polyester, procédé pour la production de fibres de polyester, tissu, produit en fibres, et article moulé en polyester
JP5758807B2 (ja) * 2009-10-20 2015-08-05 帝人フロンティア株式会社 ポリエステル繊維およびその製造方法および布帛および繊維製品
US9334608B2 (en) 2009-10-20 2016-05-10 Teijin Frontier Co., Ltd. Polyester fiber, method for producing the same, cloth, textile product, and polyester formed article
WO2012178094A1 (fr) 2011-06-23 2012-12-27 E. I. Du Pont De Nemours And Company Nanoparticules modifiées, leur préparation et leur utilisation pour améliorer l'aptitude d'un substrat fibreux à la teinture par un colorant cationique

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DE69837169D1 (de) 2007-04-05
DE69837169T2 (de) 2008-01-03
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KR100359347B1 (ko) 2002-10-31
EP1489206B1 (fr) 2007-02-21
EP1006220A4 (fr) 2001-10-31
KR100359149B1 (ko) 2002-11-01
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KR20010022988A (ko) 2001-03-26

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