JP2009097105A - Far-infrared radiation fiber, fabric including the same and method for producing the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a far-infrared radiation fiber to exhibit pilling resistance, and to provide a fabric including the fiber and a method for producing the same. <P>SOLUTION: The far-infrared radiation fiber includes polyester (A) that is mainly composed of a dicarboxylic acid unit consisting essentially of a terephthalic acid unit and a diol unit consisting essentially of an ethylene glycol unit and is modified by using a dialkyl phosphate represented by formula (i) (wherein R<SP>1</SP>and R<SP>2</SP>are each independently a 3-8C alkyl group) and contains 0.9-1.3 mol% of phosphorus atoms derived from the dialkyl phosphate based on the whole carboxylic acid components constituting the polyester, contains 5 wt.% or more of titanium dioxide. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to a fiber having anti-pilling performance and emitting far-infrared rays, and a fabric formed using this fiber.

  Polyester fibers are superior in mechanical properties such as strength and elongation, and are also excellent in heat resistance, weather resistance, chemical resistance, and many other properties such as clothing and industrial materials. Widely used in the field. However, the high strength and high elongation characteristics of polyester fibers, on the other hand, are prone to pilling when used in clothing, especially knitted products and loose woven fabrics. It has the disadvantage of significant damage.

  And in order to prevent generation | occurrence | production of the pilling in a polyester fiber, after phosphoric acid ester is copolymerized to polyester or a phosphorus compound is added in polyester, after manufacturing a fiber using such polyester, Various methods for imparting anti-pilling properties by reducing the strength of polyester fibers by treating with polyester have been proposed (see, for example, Patent Documents 1 and 2).

On the other hand, many proposals have been made for fibers having a far-infrared radiation effect. For example, fibers made by putting a ceramic material into a fiber-forming polymer are disclosed in JP-A-60-126310, JP-A-61-1908, JP-A-62-238811, and JP-A-63-243315. Further, fibers in which far-infrared radioactive ceramic fine powder is coated on the fiber surface with a heat-resistant synthetic resin have been proposed in JP-A-60-239543 and JP-A-60-239563. However, these far-infrared radiation fibers have a sufficient anti-pilling property because it has been difficult to obtain a desired fiber due to agglomeration of ceramic fine powder and the like by the conventionally known methods for imparting anti-pilling properties. It was difficult to give. That is, pilling occurs due to long-term wearing, and the appearance of the product is remarkably impaired.
Japanese Patent Laid-Open No. 50-135351 Japanese Patent Publication No.58-18447

  The present invention solves the above-mentioned problems, and the present invention provides a fiber that exhibits anti-pilling performance and emits far-infrared rays, a fabric formed using the fiber, and a method for producing the fabric. The task is to do.

  That is, the present invention mainly comprises a dicarboxylic acid unit mainly composed of a terephthalic acid unit and a diol unit mainly composed of an ethylene glycol unit, and has the following formula (i):

（式中Ｒ^１およびＲ^２はそれぞれ独立して炭素原子数３〜８のアルキル基を表す）で表されるリン酸ジアルキルエステルを用いて変成されているポリエステル（Ａ）を含むポリエステル系の遠赤外線放射繊維であって、前記リン酸ジアルキルエステルに由来するリン原子の含有量が前記遠赤外線放射繊維構成する全ポリエステルのカルボン酸成分に対して０．９〜１．３モル％であるとともに、二酸化チタンを５重量％以上含有することを特徴とする遠赤外線放射繊維である。

(Wherein R ¹ and R ² each independently represents an alkyl group having 3 to 8 carbon atoms) and a polyester-based farther comprising a polyester (A) modified with a phosphoric acid dialkyl ester Infrared radiating fiber, the content of phosphorus atoms derived from the dialkyl phosphate is 0.9 to 1.3 mol% with respect to the carboxylic acid component of the total polyester constituting the far infrared radiating fiber, It is a far-infrared radiation fiber characterized by containing 5% by weight or more of titanium dioxide.

  Further, it is a fabric made of the far infrared radiation fiber.

  Further, it mainly comprises a dicarboxylic acid unit mainly composed of terephthalic acid units and a diol unit mainly composed of ethylene glycol units, and has the following formula (i):

（式中Ｒ^１およびＲ^２はそれぞれ独立して炭素原子数３〜８のアルキル基を表す）で表されるリン酸ジアルキルエステルを用いて変成されているポリエステル（Ａ）を含むポリエステル系の遠赤外線放射繊維であって、前記リン酸ジアルキルエステルに由来するリン原子の含有量が前記遠赤外線放射繊維を構成する全ポリエステルのカルボン酸成分に対して０．９〜１．３モル％であるとともに、二酸化チタンを５重量％以上含有する遠赤外線放射繊維からなる布帛を水の存在下に１１０℃以上の温度で熱処理することを特徴とする上記布帛の製造方法である。

(Wherein R ¹ and R ² each independently represents an alkyl group having 3 to 8 carbon atoms) and a polyester-based farther comprising a polyester (A) modified with a phosphoric acid dialkyl ester Infrared radiating fiber, wherein the content of phosphorus atoms derived from the dialkyl phosphate is 0.9 to 1.3 mol% with respect to the carboxylic acid component of all polyesters constituting the far infrared radiating fiber A method for producing the above-mentioned fabric, characterized in that a fabric comprising far-infrared radiation fibers containing 5% by weight or more of titanium dioxide is heat-treated at a temperature of 110 ° C. or more in the presence of water.

Since the far-infrared radiating fiber of the present invention contains 5% by weight or more of titanium dioxide, it has far-infrared radiation.
Further, the far-infrared radiating fiber of the present invention contains a polyester (A) mainly composed of a dicarboxylic acid unit mainly composed of a terephthalic acid unit and a diol unit mainly composed of an ethylene glycol unit. Therefore, polyethylene terephthalate suitable for various applications. It has the property of a system fiber and the fiber containing this.
The polyester (A) is represented by the following formula (i);

（式中Ｒ^１およびＲ^２はそれぞれ独立して炭素原子数３〜８のアルキル基を表す）で表されるリン酸ジアルキルエステルを、該リン酸ジアルキルエステルに由来するリン原子の含有量が前記遠赤外線放射繊維を構成する全ポリエステルのカルボン酸成分に対して０．９〜１．３モル％用いて変成されているので、高い抗ピリング性を発現する。
また前記二酸化チタンと前記リン酸アルキルエステルとをこのような割合で用いることで、従来遠赤外線放射繊維に高い抗ピリング性を付与しようとすると起こっていた凝集などの問題が発生しない。

(Wherein R ¹ and R ² each independently represents an alkyl group having 3 to 8 carbon atoms), the phosphoric acid dialkyl ester represented by the phosphoric acid dialkyl ester has a phosphorus atom content of Since it is modified by using 0.9 to 1.3 mol% of the carboxylic acid component of all polyesters constituting the far-infrared radiating fiber, it exhibits high anti-pilling properties.
Further, by using the titanium dioxide and the alkyl phosphate ester in such a ratio, problems such as aggregation, which have occurred when trying to impart high anti-pilling properties to far-infrared radiation fibers, do not occur.

The present invention is described in detail below.
The polyester (A) used in the present invention is a polyester modified using a phosphoric acid dialkyl ester represented by the above formula (i) [hereinafter referred to as “phosphoric acid dialkyl ester (i)”]. And, after the polyester (A) is modified with the dialkyl phosphate ester (i), after forming the fiber, or forming a fabric from the fiber, or manufacturing a product such as a sewing product from the fabric, When these fibers and fabrics are heat-treated at a temperature of 110 ° C. or higher in the presence of water, partial hydrolysis of the polyester occurs, the degree of polymerization of the polyester decreases, and good anti-pilling properties are imparted to the fibers.

In the phosphoric acid dialkyl ester represented by the above formula (i) which is a modifying component in the polyester (A), the groups R ¹ and R ² are each independently an alkyl group having 3 to 8 carbon atoms as described above. Accordingly, the groups R ¹ and R ² are alkyl groups having 3 to 8 carbon atoms selected from propyl, butyl, pentyl, hexyl, heptyl and octyl groups. The aforementioned alkyl group may be a linear alkyl group or a branched alkyl group, but is preferably a linear alkyl group. Further, the groups R ¹ and R ² may be the same alkyl group or different alkyl groups.

Specific examples of the dialkyl phosphate ester (i) include di-n-propyl phosphate, di-n-butyl phosphate, di-t-butyl phosphate, di-n-pentyl phosphate, di-n-hexyl phosphate, di- n-heptyl phosphate, di-n-octyl phosphate, (n-propyl) (n-butyl) phosphate, (n-propyl) (n-pentyl) phosphate, (n-propyl) (n-hexyl) phosphate, (n -Propyl) (n-heptyl) phosphate, (n-propyl) (n-octyl) phosphate, (n-butyl) (n-pentyl) phosphate, (n-butyl) (n-hexyl) phosphate, (n-butyl) ) (N-heptyl) phosphate, (n-butyl) (n-octyl) phosphate, (n-pepth) Til) (n-hexyl) phosphate, (n-pentyl) (n-heptyl) phosphate, (n-pentyl) (n-octyl) phosphate, (n-hexyl) (n-heptyl) phosphate, (n-hexyl) (N-octyl) phosphate, (n-heptyl) (n-octyl) phosphate, and the like. Further, in each of the phosphoric acid dialkyl esters (i) described above, one or both of the two alkyl groups forming the phosphoric acid ester is a branched alkyl group instead of an n-alkyl group. Of course, dialkyl esters can also be used.
The polyester (A) may be modified by one kind of the above-mentioned dialkyl phosphate (i), or may be modified by two or more kinds.

In the present invention, the reason why the polyester (A) modified with a phosphoric acid dialkyl ester in which the groups R ¹ and R ² are alkyl groups having 3 to 8 carbon atoms is used is that the groups R ¹ and R ² are This is because in the case of a methyl group or an ethyl group, the dialkyl phosphate is very easily decomposed and cannot be effectively used for modifying polyester. On the other hand, when the polyester is modified using a phosphoric acid dialkyl ester in which the groups R ¹ and R ² are an alkyl group having 9 or more carbon atoms, the polyester obtained by the modification is yellowish and the color tone is poor. It is not preferable.

  And in polyester (A), content of the phosphorus atom derived from phosphoric acid dialkyl ester (i) is 0.9-1.3 mol% with respect to the carboxylic acid component of all the polyesters which comprise a far-infrared radiation fiber. is there. That is, it is necessary that it is 0.9-1.3 mol per 100 mol of all carboxylic acid components of all polyesters constituting the far-infrared radiation fiber. When the content of phosphorus atoms derived from the dialkyl phosphate (i) is less than 0.9 mol% with respect to the total carboxylic acid component, polyester fibers and fabrics obtained by melting the polyester (A) are The anti-pilling property is not excellent. On the other hand, if it exceeds 1.3 mol%, anti-pilling properties can be imparted, but hydrolysis during the fiber production process becomes significant, resulting in a large difference between lots, and a decrease in mechanical properties of the resulting fiber. Thus, damage in the process of spinning the fiber or making it into a fabric becomes significant. Moreover, it becomes easy to receive damage, such as rubbing and tearing, while wearing a fabric.

  The polyester (A) must be mainly composed of a dicarboxylic acid unit mainly composed of a terephthalic acid unit and a diol unit mainly composed of an ethylene glycol unit. The terephthalic acid unit is 70 mol% or more, preferably 90 mol% or more, and the ethylene glycol unit is 70 mol% or more, preferably 90 mol, based on the total of all diol units and polyol units constituting the polyester (A). It is good to have more than%.

  The polyester (A) is a structural unit derived from another bifunctional compound if it is less than 30 mol%, preferably less than 10 mol%, based on all constituent units in addition to the terephthalic acid unit and the ethylene glycol unit. If necessary, one or two or more of them may be contained as copolymerized units. Structural units derived from such other bifunctional compounds include aromatic dicarboxylic acids such as isophthalic acid, phthalic acid, naphthalene dicarboxylic acid, biphenyl dicarboxylic acid, diphenyl ether dicarboxylic acid, diphenyl sulfone dicarboxylic acid, and diphenyl ketone dicarboxylic acid. Acids; Aliphatic dicarboxylic acids such as oxalic acid, malonic acid, succinic acid, adipic acid, azelaic acid, sebacic acid and dodecanedioic acid; alicyclic dicarboxylic acids such as decalin dicarboxylic acid and cyclohexanedicarboxylic acid; glycolic acid, hydroxybenzoic acid Hydroxycarboxylic acids such as acid, mandelic acid and matrolactic acid; aliphatic lactones such as ε-caprolactone; trimethylene glycol, tetramethylene glycol, 1,5-pentanediol, 1,6-hexanediol, neo Aliphatic diols such as ntile glycol, diethylene glycol, polyethylene glycol, polybutylene glycol; aromatic diols such as hydroquinone, catechol, naphthalene diol, resorcin, 1,4-bis (β-oxyethoxy) benzene; cyclohexanedimethanol, etc. Mention may be made of structural units derived from bifunctional components such as alicyclic diols.

  Further, the polyester (A) after spinning has an intrinsic viscosity [η] of 0.45 to 0.55 dl / when measured using an Ubbelohde viscometer at 30 ° C. in an equal weight mixed solvent of phenol and tetrachloroethane. g is preferable, and 0.47 to 0.53 dl / g is preferable. When the intrinsic viscosity [η] of the polyester (A) is less than 0.45 dl / g, products such as formed fibers, fabrics formed from the fibers, products formed from the fabrics, In addition, when hydrothermal treatment is performed at a temperature of 110 ° C. or higher, the anti-pilling property is obtained, but the strength of the fiber becomes too weak. Moreover, when it exceeds 0.55 dl / g, anti-pilling property is difficult to be imparted by the same treatment.

  The production method of the polyester (A) is not particularly limited, and any polyester that satisfies the above-described requirements can be used. Preferably, the polyester (A) is produced as follows. That is, a raw material mainly composed of a dicarboxylic acid component mainly composed of terephthalic acid or an ester-forming derivative thereof and a diol component mainly composed of ethylene glycol, and containing other bifunctional compounds as described above as required. Then, an esterification reaction or a transesterification reaction is performed to produce a prepolymer (first stage reaction), and then the prepolymer obtained by the first stage reaction is heated under reduced pressure to cause a polycondensation reaction. In producing the final polyester (second stage reaction), the dialkyl phosphate described above at any point between the end of the first stage reaction and the end of the second stage reaction. By adding (i) to the reaction system, the polyester (A) can be produced smoothly. The production method of the polyester (A) is described in detail in the above-mentioned Japanese Patent Application Laid-Open No. 61-47818 relating to the applicant's application, and the polyester (A) used in the present invention is described in the method described therein. It can be manufactured similarly.

  For the far-infrared radiation effect, the standard set by the Far-Infrared Association is a standard. That is, the far-infrared spectral emissivity by the FT-IR method exceeds the integrated spectral emissivity by 5% or more in the wavelength range of 4 to 20 μm as compared with the unprocessed product, or the total radiation in an arbitrary section of the wavelength range. The standard is that the rate is at least 10% higher than that of the unprocessed product.

  Examples of the fine particles for emitting far-infrared rays include titanium dioxide, silicon dioxide, zircon, manganese oxide, iron oxide, cobalt oxide, nickel oxide, and chromium oxide. However, titanium dioxide and silicon dioxide are desirable in consideration of the price of raw materials, the ease and cost of pulverization, and the good state that the dispersion state in the polyester polymer does not affect the spinning. The far-infrared radiation fiber of the present invention needs to contain 5% by weight or more of titanium dioxide. Further, when titanium dioxide is used alone as fine particles for emitting far-infrared rays, it is preferably 5 to 10% by weight, and more preferably 6 to 8% by weight. If the content of titanium dioxide is less than 5% by weight, the amount of far-infrared radiation is small and the standard set by the far-infrared ray association is not reached. Also, if the content exceeds 10% by weight, the content of titanium dioxide is large, so that titanium dioxide tends to agglomerate, causing problems such as clogging of the polymer filter during spinning or breaking the yarn during spinning. It becomes easy and is not preferable.

  Adding more silicon dioxide increases the effect of far-infrared radiation. It is necessary to contain silicon dioxide in an amount of 0.5% by weight or more, preferably 0.6 to 3% by weight, based on the polyester (A). When the content is less than 0.5% by weight, even if added to titanium dioxide, the effect is small in the far infrared ray measurement method. When the content exceeds 3% by weight, as in the case of titanium dioxide, agglomeration of silicon dioxide is likely to occur, and troubles such as clogging of the polymer filter during spinning or breakage during spinning are preferable. Absent.

The method for mixing the polyester (A) with titanium dioxide or silicon dioxide is not particularly limited as long as the fine particles can be mixed uniformly and melt-spun. For example,
(1) Titanium dioxide dispersed in ethylene glycol or the like is added before the start of the esterification reaction, and a prepolymer is produced by performing an esterification reaction or a transesterification reaction (the first stage reaction), and then the first stage The prepolymer obtained by the first reaction is heated under reduced pressure to undergo a polycondensation reaction to produce a final polyester (second stage reaction). A method of adding the above-described dialkyl phosphate (i) to the reaction system at an arbitrary time until the completion of the stage reaction.
(2) A prepolymer was produced by performing an esterification reaction or a transesterification reaction (first stage reaction), and then titanium dioxide dispersed in ethylene glycol or the like was added, and then obtained by the first stage reaction. The resulting prepolymer is heated under reduced pressure to undergo a polycondensation reaction to produce a final polyester (second stage reaction). After the completion of the first stage reaction, the second stage reaction is carried out. A method of adding the above-mentioned dialkyl phosphate (i) to the reaction system at an arbitrary time until the completion.
(3) A method in which, when the chip is remelted in the obtained polyester (A), titanium dioxide and silicon dioxide are added to obtain a chip in which fine particles are uniformly dispersed, and this chip is used for melt spinning.
(4) A method in which the chip is remelted in the obtained polyester (A), titanium dioxide and silicon dioxide are added, and after the fine particles are uniformly dispersed, the polymer is directly used for melt spinning.
(5) Polyester (A) and polyester (B) chips containing titanium dioxide or silicon dioxide are produced separately, then blended and remelted to produce chips in which both polyesters are uniformly mixed. And using the chip for melt spinning.
(6) Polyester (A) and polyester (B) chips containing titanium dioxide or silicon dioxide are produced separately, blended and remelted, and both polyesters are uniformly mixed and melt-spun directly. Method used for.
(7) Polyester (A) and a polyester (B) chip containing titanium dioxide or silicon dioxide are melted individually, and each melt is uniformly mixed in a mixing section provided upstream of the melt spinning apparatus. Direct melt spinning method.
(8) Polyester (A), polyester (B) containing titanium dioxide and polyester (C) containing silicon dioxide are produced separately, blended and remelted, A method of producing uniformly mixed chips and using the chips for melt spinning.
(9) Polyester (A), polyester (B) containing titanium dioxide, and polyester (C) containing silicon dioxide are produced separately, blended and remelted to obtain three types of polyester. A method in which the mixture is uniformly mixed and directly used for melt spinning.
(10) Polyester (A), polyester (B) containing titanium dioxide, and polyester (C) chips containing silicon dioxide are individually melted, and each melt is provided on the upstream side of the melt spinning apparatus. A method in which the mixture is uniformly mixed and directly melt-spun.
And so on.
In short, if the polyester (A) is uniformly mixed with titanium dioxide and silicon dioxide, an appropriate method can be used at any time during the melt spinning after the completion of polymerization of the respective polymers. Adopt it.

  The polyesters (B) and (C) must be mainly composed of dicarboxylic acid units mainly composed of terephthalic acid units and diol units mainly composed of ethylene glycol units. 70 mol% or more, preferably 90 mol% or more of terephthalic acid units based on the total carboxylic acid component constituting, and ethylene glycol based on the total of all diol units and polyol units constituting polyesters (B) and (C) The unit should be 70 mol% or more, preferably 90 mol% or more.

  Polyesters (B) and (C) are derived from other bifunctional compounds as long as they are less than 30 mol%, preferably less than 10 mol%, based on all constituent units in addition to terephthalic acid units and ethylene glycol units. If necessary, one or more structural units may be contained as copolymerized units.

  The melt spinning is not particularly limited, and may be performed using a conventionally known melt spinning method and melt spinning apparatus when producing ester fibers from a polyester polymer. Various conditions such as the melt spinning temperature, the cooling condition after spinning, and the spinning speed of the spun fiber are not particularly limited. For example, it is preferable to perform melt spinning at a take-up speed of about 500 to 6000 m / min using a melt spinning temperature of about 270 to 300 ° C.

  For each of polyesters (A) and (B) and (C), inorganic fine particles, fragrance, antibacterial agent, flame retardant, deodorant, dye / pigment, matting agent, antistatic agent (antistatic) Agent), an antioxidant, a light stabilizer, and the like, may contain one or more optional additives.

The cross-sectional shape of the fiber is not particularly limited, and an atypical cross section can be appropriately selected according to the purpose other than circular. Although not limited, as an atypical section in the present invention, for example, a hollow shape, a Y shape, a T shape, a cross shape, a flat shape, a 3-8 leaf shape, a 3-8 octagon shape, a dogbone shape, an elliptic shape The cross-sectional shape such as
Further, the single fiber fineness and the total denier number of the polyester fiber are not particularly limited, and a monofilament or multifilament having an arbitrary single fiber fineness can be produced smoothly.

  Polyester fibers are produced by the above-described series of processes. The polyester fibers obtained thereby can be directly circulated and sold as they are without heat treatment in the presence of water, or can be drawn, crimped, entangled. After processing such as processing and taslan processing, it can be distributed and sold, and the form at that time is also made of filament yarn, staple, sliver, spun yarn, knitted fabric, woven fabric, non-woven fabric, etc. Any form, such as a product obtained, may be sufficient. And in that case, the anti-pilling property can be imparted by heat-treating them at a temperature of 110 ° C. or higher in the presence of water on the side where those fibers, yarns, fabrics, products, etc. are purchased. .

  Further, the polyester fiber obtained by the above melt spinning is subjected to drawing, crimping, entanglement processing, taslan processing, or the like, before making the fabric, or after applying the above processing, After producing a final product such as a sewn product from a fabric or the like, it may be heat treated at a temperature of 110 ° C. or higher in the presence of water to impart anti-pilling properties, and then distributed and sold.

  In order to impart anti-pilling properties by heat-treating polyester fibers, staples made thereof, sliver, yarn, fabric, products, etc., it is necessary to perform heat treatment in the presence of water. When the heat treatment is performed in the presence of water, the partial hydrolysis of the polyester fiber necessary for imparting anti-pilling property and the accompanying decrease in fiber physical properties cannot be expressed. In addition, the heat treatment temperature needs to be 110 ° C. or higher, and if it is less than 110 ° C., water treatment efficiency is effective for imparting anti-pilling properties and prevention of significant physical property deterioration of the polyester fiber. The heat treatment in the presence is preferably performed at a temperature of 120 to 180 ° C. Further, this heat treatment is performed until the tensile strength of the polyester fiber after heat treatment is in the range of 3.4 to 5.8 cN for a single fiber and the tensile elongation is in the range of 12 to 18%. From the viewpoint of imparting properties and mechanical properties of the polyester fiber after heat treatment, the tensile strength is in the range of 3.7 to 4.2 cN for a single fiber, and the tensile elongation is in the range of 14 to 16%. Is more preferable.

  In performing heat treatment in the presence of water, a polyester fiber obtained from the polyester (A), a thread made from the polyester, a sliver, a staple, a fabric, a sewing product, and the like are immersed in hot water of 110 ° C. or higher for a predetermined time. It is good to carry out, and it is usually carried out by putting water in a pressure device to bring the temperature of the water to 110 ° C. or higher and immersing it in it. As described above, the heat treatment in the presence of water for imparting anti-pilling properties may be performed at any stage up to the final product such as fiber, staple, sliver, yarn, fabric, and sewing product. In particular, it is convenient in terms of the process to use the hot hot water treatment received in the dyeing process in combination as a heat treatment for imparting anti-pilling properties.

  EXAMPLES Hereinafter, although an Example demonstrates this invention concretely, this invention is not limited at all by this. In addition, each evaluation in an Example was performed with the following method.

[Far-infrared spectral emissivity]; Using FT-IR, how much the integrated spectral emissivity was higher than that of the unprocessed product in a wavelength range of 4 to 20 μm was measured.

[Measurement of tensile strength and tensile elongation of fiber after hydrothermal treatment];
JIS L 1050 7.7.1 Tensile strength and elongation were measured according to the standard time method. The tester used was a constant-speed load type tester (capacity 20 g), the sample holding interval was 20 mm, and the tensile speed was 20 gf / min. In addition, the value of tensile strength was represented by the load (gf) when a sample cut | disconnects.

[Evaluation of fabric pilling];
Evaluation was performed according to JIS L 1076 6.1A method (method using an ICI type tester).

Example 1
(1) Polyester (A) polyethylene terephthalate chip having di-n-butyl phosphate units converted to phosphorus atoms at a ratio of 2.5 mol% with respect to the total carboxylic acid component, and polyester (B) dioxide Polyethylene terephthalate chips containing 10% by weight of titanium are blended in a weight ratio of polyester (A) / polyester (B) = 40/60, and after drying, blended in a melting apparatus provided upstream of the melt spinning apparatus. After melting the product, it is supplied to a melt spinning apparatus, melt-spun at 280 ° C. from a spinneret having a spinning hole, taken at 1000 m / min, and then stretched 2.5 times at 70 ° C. To give a mechanical crimp by cutting to a fiber length of 38 mm, and a phosphorus atom: 1.0 mol%, titanium dioxide; 6.0 wt% of a polyester fiber Far-infrared radiation fibers were produced as staples.

(2) The staple obtained in (1) above was treated by immersing it in hot water at a temperature of 130 ° C. for 60 minutes, then taken out, dried, and its tensile strength and tensile elongation were measured by the above method. They were 4.1 cN and 14.2%, respectively.
(3) Using the staple obtained in (1) above, a spun yarn (30 count) is produced by a conventional method, and a 1/1 plain woven fabric is woven by using the spun yarn by a conventional method, and the fabric is desized. After scouring and dyeing (dye bath temperature of 120 ° C.), the pilling property was evaluated by the above method. As a result, it was grade 5, excellent anti-pilling property, and good fabric with softness and bulkiness. (Fabric).
(4) When the integral spectral emissivity of the polyester fabric obtained in (3) above was measured in the wavelength range of 4 to 20 μm using FT-IR, it was 74.1%. Since it was 5.9% higher than 68.2% of Comparative Example 1 not containing titanium dioxide, a good far-infrared radiation effect was seen.

(Example 2)
In the same manner as in Example 1, far-infrared radiation fibers and fabrics were obtained and tested.

(Example 3)
In the same manner as in Example 1, far-infrared radiation fibers and fabrics were obtained and tested.

Example 4
(1) Polyester (A) polyethylene terephthalate chip having di-n-butyl phosphate units converted to phosphorus atoms in a proportion of 2.6 mol% with respect to the total carboxylic acid component, and polyester (B) dioxide A polyethylene terephthalate chip containing 15% by weight of titanium and a polyethylene terephthalate chip containing 6% by weight of silicon dioxide as polyester (C) are polyester (A) / polyester (B) / polyester (C) = 50 / After blending at a weight ratio of 40/10 and drying, the blended material was melted by a melting device provided upstream of the melt spinning device, and then supplied to the melt spinning device. From a spinneret having a spinning hole, 280 ° C. Spin at a speed of 1,000 m / min, and then stretch 2.5 times at 70 ° C. To provide a mechanical crimp, cut to a fiber length of 38 mm, and far infrared as a staple of polyester atoms of phosphorus atoms; 1.3 mol%, titanium dioxide; 6.0 wt%, silicon dioxide; 0.6 wt% Radiant fibers were produced.

(2) The staple obtained in (1) above was treated by immersing it in hot water at a temperature of 130 ° C. for 60 minutes, then taken out, dried, and its tensile strength and tensile elongation were measured by the above method. They were 3.5 cN and 13.5%, respectively.
(3) Using the staple obtained in (1) above, a spun yarn (30 count) is produced by a conventional method, and a 1/1 plain woven fabric is woven by using the spun yarn by a conventional method, and the fabric is desized. After scouring and dyeing (dye bath temperature of 120 ° C.), the pilling property was evaluated by the above method. As a result, it was grade 5, excellent anti-pilling property, and good fabric with softness and bulkiness. (Fabric).
(4) When the integral spectral emissivity of the polyester fabric obtained in (3) above was measured in the wavelength range of 4 to 20 μm using FT-IR, it was 75.9%. Since it was 7.7% higher than 68.2% of Comparative Example 1 not containing titanium dioxide, a good far-infrared radiation effect was seen.

(Comparative Example 1)
(1) Polyester (A) polyethylene terephthalate chip having di-n-butyl phosphate units converted to phosphorus atoms at a ratio of 2.5 mol% with respect to the total carboxylic acid component, and polyester (B) dioxide Polyethylene terephthalate chips that do not contain titanium are blended at a weight ratio of polyester (A) / polyester (B) = 40/60, and after drying, the blend is melted in a melting device provided upstream of the melt spinning device. Then, it is supplied to a melt spinning apparatus, melt-spun at 280 ° C. from a spinneret having a spinning hole, taken up at 1000 m / min, and then stretched 2.5 times at 70 ° C. Shrinkage was applied, and the fiber length was cut to 38 mm, and a polyester fiber staple of phosphorus atom: 1.0 mol%, titanium dioxide: 0 wt% was obtained. Manufactured.
(2) The staple obtained in (1) above was treated by immersing it in hot water at a temperature of 130 ° C. for 60 minutes, then taken out, dried, and its tensile strength and tensile elongation were measured by the above method. They were 4.2 cN and 14.5%, respectively.
(3) Using the staple obtained in (1) above, a spun yarn (30 count) is produced by a conventional method, and a 1/1 plain woven fabric is woven by using the spun yarn by a conventional method, and the fabric is desized. After scouring and dyeing (dye bath temperature of 120 ° C.), the pilling property was evaluated by the above method. As a result, it was grade 5, excellent anti-pilling property, and good fabric with softness and bulkiness. (Fabric).
(4) When the integral spectral emissivity of the polyester fabric obtained in (3) above was measured in the wavelength region of 4 to 20 μm using FT-IR, it was 68.2%. The difference from this value was evaluated as a raw material standard for far-infrared radiation effect.

(Comparative Example 2)
In the same manner as in Comparative Example 1, fibers and fabrics were obtained and evaluated.

(Comparative Example 3)
(1) Polyester (A) polyethylene terephthalate chip having di-n-butyl phosphate units converted to phosphorus atoms in a proportion of 2.0 mol% with respect to the total carboxylic acid component, and polyester (B) as dioxide Polyethylene terephthalate chips containing 10% by weight of titanium are blended in a weight ratio of polyester (A) / polyester (B) = 40/60, and after drying, blended in a melting apparatus provided upstream of the melt spinning apparatus. After melting the product, it is supplied to a melt spinning apparatus, melt-spun at 280 ° C. from a spinneret having a spinning hole, taken at 1000 m / min, and then stretched 2.5 times at 70 ° C. To give a mechanical crimp, cut to a fiber length of 38 mm, phosphorus atom; 0.8 mol%, titanium dioxide; 6.0% by weight of polyester fiber Staples were manufactured.

(2) The staple obtained in (1) above was treated by immersing it in hot water at a temperature of 130 ° C. for 60 minutes, then taken out, dried, and its tensile strength and tensile elongation were measured by the above method. They were 6.0 cN and 20.0%, respectively.
(3) Using the staple obtained in (1) above, a spun yarn (30 count) is produced by a conventional method, and a 1/1 plain woven fabric is woven by using the spun yarn by a conventional method, and the fabric is desized. After scouring and dyeing (temperature of dyeing bath 120 ° C.), the pilling property was evaluated by the above method. As a result, it was a woven fabric that was second grade and inferior in pilling property.

(Comparative Example 4)
(1) Polyester (A) polyethylene terephthalate chip having di-n-butyl phosphate units converted to phosphorus atoms in a proportion of 2.8 mol% with respect to the total carboxylic acid component, and polyester (B) dioxide Polyethylene terephthalate chips containing 12% by weight of titanium are blended in a weight ratio of polyester (A) / polyester (B) = 50/50, and after drying, blended in a melting apparatus provided upstream of the melt spinning apparatus. After melting the product, it is supplied to a melt spinning apparatus, melt-spun at 280 ° C. from a spinneret having a spinning hole, taken at 1000 m / min, and then stretched 2.5 times at 70 ° C. To give a mechanical crimp, cut to a fiber length of 38 mm, phosphorus atom; 1.4 mol%, titanium dioxide; 6.0 wt% of polyester fiber Staples were manufactured.
(2) The staple obtained in (1) above was treated by immersing it in hot water at a temperature of 130 ° C. for 60 minutes, then taken out, dried, and its tensile strength and tensile elongation were measured by the above method. They were 3.3 cN and 11.0%, respectively.
(3) Using the staple obtained in (1) above, a spun yarn (30 count) is produced by a conventional method, and a 1/1 plain woven fabric is woven by using the spun yarn by a conventional method, and the fabric is desized. After scouring and dyeing (dye bath temperature 120 ° C.), the pilling property was evaluated by the above method, and it was grade 5 and excellent in anti-pilling property. The tear damage was great and it was not ready for use.

(Comparative Example 5)
(1) Polyester (A) polyethylene terephthalate chip having di-n-butyl phosphate units converted to phosphorus atoms at a ratio of 2.5 mol% with respect to the total carboxylic acid component, and polyester (B) dioxide Polyethylene terephthalate chips containing 10% by weight of titanium are blended in a weight ratio of polyester (A) / polyester (B) = 40/60, and after drying, blended in a melting apparatus provided upstream of the melt spinning apparatus. After melting the product, it is supplied to a melt spinning apparatus, melt-spun at 280 ° C. from a spinneret having a spinning hole, taken at 1000 m / min, and then stretched 2.5 times at 70 ° C. To give a mechanical crimp by cutting to a fiber length of 38 mm, and a phosphorus atom: 1.0 mol%, titanium dioxide; 6.0 wt% of a polyester fiber Staples were manufactured.
(2) The staple obtained in (1) above was treated by immersing it in hot water at a temperature of 100 ° C. for 60 minutes, then taken out and dried, and its tensile strength and tensile elongation were measured by the above method. They were 6.6 cN and 22.0%, respectively.
(3) Using the staple obtained in (1) above, a spun yarn (30 count) is produced by a conventional method, and a 1/1 plain woven fabric is woven by using the spun yarn by a conventional method, and the fabric is desized. After scouring and dyeing (temperature of dyeing bath 100 ° C.), the pilling property was evaluated by the above-mentioned method. As a result, it was a woven fabric (fabric) that was first grade and inferior in anti-pilling property.

  Table 1 below shows the physical properties after hydrothermal treatment of the fibers, the pilling properties after dyeing of the fabric, the distant properties when the dialkyl phosphate content, titanium dioxide content, and silicon dioxide content are changed. The infrared radiation effect was summarized.

Claims (5)

It consists mainly of a dicarboxylic acid unit mainly composed of terephthalic acid units and a diol unit mainly composed of ethylene glycol units, and has the following formula (i):

(Wherein R ¹ and R ² each independently represents an alkyl group having 3 to 8 carbon atoms) and a polyester-based farther comprising a polyester (A) modified with a phosphoric acid dialkyl ester Infrared radiating fiber, wherein the content of phosphorus atoms derived from the dialkyl phosphate is 0.9 to 1.3 mol% with respect to the carboxylic acid component of all polyesters constituting the far infrared radiating fiber A far-infrared radiating fiber containing 5% by weight or more of titanium dioxide. The far-infrared radiating fiber according to claim 1, wherein the far-infrared radiating fiber contains 0.5% by weight or more of silicon dioxide. The fabric which consists of a far-infrared radiation fiber in any one of Claims 1-2. It consists mainly of a dicarboxylic acid unit mainly composed of terephthalic acid units and a diol unit mainly composed of ethylene glycol units, and has the following formula (i):

(Wherein R ¹ and R ² each independently represents an alkyl group having 3 to 8 carbon atoms) and a polyester-based farther comprising a polyester (A) modified with a phosphoric acid dialkyl ester Infrared radiating fiber, wherein the content of phosphorus atoms derived from the dialkyl phosphate is 0.9 to 1.3 mol% with respect to the carboxylic acid component of all polyesters constituting the far infrared radiating fiber The fabric comprising a far-infrared radiation fiber according to claim 3, wherein the fabric comprising the far-infrared radiation fiber containing 5% by weight or more of titanium dioxide is heat-treated at a temperature of 110 ° C or higher in the presence of water. Production method. From the far-infrared radiation fiber according to claim 4, wherein the far-infrared spectral emissivity according to the FT-IR method is more than 5% higher than that before heat treatment in the wavelength range of 4 to 20 µm. The manufacturing method of the fabric which becomes.