JP3223745B2 - Polyester fiber - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polyester fiber having a dry touch feeling of higher quality than conventional products.
More specifically, the present invention relates to a polyester fiber having a new texture having fine irregularities on the surface of the fiber and having minute friction characteristics.

[0002]

2. Description of the Related Art Polyester fibers are widely used for clothing because of their excellent functionality. In the blouse and lining applications in the garment field, particularly in the women's garment field, there is a strong demand for further improvement in texture in addition to the physical characteristics of polyester fibers due to the recent trend toward luxury. As a conventional texture improvement, a dry touch texture is mainly applied, and a method of alkali-treating a fiber in which inorganic particles having a relatively large particle size such as titanium dioxide are blended at a high concentration has been proposed. However, although dry touch properties can be imparted by this method, a higher quality dry touch feeling was hardly observed.

[0003] Conventionally, fine irregularities are formed on the fiber surface,
A number of techniques have been developed to increase the amount of light absorbed after dyeing to enhance color development. For example, a method has been proposed in which fibers containing a large amount of finely divided particles are reduced with alkali (Japanese Patent Application Laid-Open No. 54-120728). The main object of fine particles is silica, and in this method, 50 nm is used.
Although an innumerable unevenness having a thickness of 200 nm or less is formed on the yarn surface, the effect of improving coloration is recognized. However, since the shape of the concave portion is relatively large, a dry touch feeling is improved, but a higher quality dry touch feeling is obtained. Was rarely observed.

Other techniques for forming fine irregularities on the fiber surface are disclosed in JP-A-55-107512 and JP-A-5-107512.
Many proposals have been made in JP-A-5-107544, JP-A-55-107747, and the like, but none of them has improved color development but obtained a high-quality dry touch feeling.

Japanese Patent Application Laid-Open No. 55-51819 discloses a technique for a polyester fiber containing titanium dioxide fine particles smaller than a normal particle size. However, its purpose is to obtain a pearly luster, and there is no mention of the texture.

Japanese Patent Application Laid-Open No. 3-124852 proposes a fabric containing alumina particles.
In this case, there is a disclosure about a technique for improving the color developability by adding particles, but there is no description about a higher quality dry touch feeling.

Japanese Patent Publication No. 49-32776 proposes a fabric containing zirconium oxide particles. In this case, the purpose is to add flame retardancy to the fabric by adding particles. There is no description about the texture.

[0008]

SUMMARY OF THE INVENTION The present invention is to provide a polyester fiber having a higher quality dry touch feeling than conventional products.

[0009]

SUMMARY OF THE INVENTION The object of the present invention is to
This is achieved by a polyester fiber containing particles, which has fine irregularities on the fiber surface and a stress change Δf of a stick-slip curve of 0.030 g / d or more.

The polyester fiber of the present invention has specific particles.
And it is necessary to have many fine irregularities on its surface. Although the detailed causal relationship is not clear, these fine irregularities greatly contribute to the improvement of the high quality dry touch texture. In order to give a sufficient dry touch feeling, it is necessary to have a minute friction characteristic such as stick-slip. At this time, fine irregularities cannot be expressed under the conventional irregularity conditions.

Here, the stick-slip phenomenon is a phenomenon in which the movement of the sliding surface is intermittent, and an example of fiber stick-slip is described in a literature (Journal of the Textile Machinery Society, Vol. 39, No. 10).
(1986)). In the present invention, the stick slip is observed between the polyester fiber and the metal mirror surface or the satin finish, or between the fiber and the fiber. The polyester fibers of the present invention must have stick-slip properties. As the value, repeated stress changes in represented by Δf (g / d) in the stick-slip curve as shown in FIG. 2 to be described later 0.
030 g / d or more. Here, Δf represents a change in stress caused by repeated stick-slip. As described above, the polyester fiber of the present invention has fine irregularities on the fiber surface and unique friction characteristics.

The polyester constituting the polyester fiber of the present invention is a polymer comprising dicarboxylic acid and glycol and having thermoplasticity and fiber forming properties.

The polyester is preferably a polyester having ethylene terephthalate as a main repeating unit,
It is particularly preferred that 80 mol% or more is ethylene terephthalate. When it is in the range of 20 mol% or less, a copolymer component generally used, for example, dicarboxylic acid represented by adipic acid, isophthalic acid, 5-sodium sulfoisophthalic acid, or polyethylene glycol, butanediol, neopentyl glycol Use of a glycol represented by such a method is acceptable.

[0014] In addition, the polyester fiber of the present invention, the double
Manufacture of titanium oxide, zirconium oxide or polyester
Sometimes formed from catalyst and / or polyester oligomer
Containing polyester insoluble particles. like this
When a specific particle is contained, a micro powder touch feeling is obtained even in a high quality dry touch. For titanium dioxide, the average particle size of the primary particles and the range of 50 ～120Nm
There is a need to, 60~100nm is more preferable. It is preferable that the particles are dispersed in the state of primary particles in the polyester fiber, but they may be partially secondary-agglomerated. By setting the average particle size of the primary particles in the range of 50 to 120 nm,
This is preferable because the fine irregularities on the fiber surface are controlled and the texture becomes micropowder touch.

The content of titanium dioxide is 1.2 to 10
It must be in the range of weight%, more preferably 1.2
8 wt%, more preferably 1.2 to 6%.
The content becomes micropowder touch feeling by the said range and spinnability also that Do good.

The structure of titanium dioxide may be any one of anatase type, rutile type and both types, but anatase type is preferred. Further, titanium dioxide may contain a small amount of an element such as iron, potassium, phosphorus, aluminum, silica, and manganese, for example, as an oxide. In particular, it is preferable to contain or coat alumina or silica because the particle dispersibility is improved. The average particle size of titanium dioxide may be obtained by adjusting the average particle size at the time of synthesis, or titanium oxide having a particle size equal to or larger than the particle size according to the present invention may be physically or mechanically obtained. It may be crushed and adjusted to an arbitrary particle size.

[0017]

[0018]

In the case of zirconium oxide particles, they can be easily obtained by heating zirconic acid or thermally decomposing zirconium salts. The average particle size of the zirconium oxide particles may be prepared so as to have a predetermined particle size at the time of synthesis, or zirconium oxide particles having a particle size not less than the particle size according to the present invention are physically and mechanically pulverized. It may be prepared to an arbitrary particle size. The average primary particle size of the zirconium oxide particles must be in the range of 5 to 200 nm . It is preferably dispersed in a state of primary particles in the port Riesuteru fibers in, partially 2
Next aggregation may be performed. The average primary particle size is 5 to 200 n.
By setting the range of m, the fine irregularities on the fiber surface are controlled, and the texture becomes micropowder touch.

The content of the zirconium oxide particles is as follows:
It is necessary to be in the range of 1.0 to 6 % by weight . The containing organic amount becomes micropowder touch feeling by the said range and spinnability also that Do good.

Catalysts and polyesters during polyester production
Field of polyester-insoluble particles formed from oligomers
In this case, it is preferable to use a copolymerized polyester,
Preferred copolymerization components include alkali metal salt-containing compounds typified by 5-sodium sulfoisophthalic acid . The insoluble polyester here refers to an insoluble particle in a solvent capable of dissolving the polyester, such as ortho-chlorophenol. In particular, it is preferable to contain lithium-based insoluble particles because the powder has a micro powder touch feeling.

As a specific example of the production of the polyester fiber of the present invention, the case where titanium dioxide is used will be described below. That is, after dry-blending titanium dioxide fine particles having a specific particle size and polyester powdered in advance, 2
A master pellet is prepared by melt-kneading using a shaft extruder. After blending the master pellet and polyethylene terephthalate containing substantially no particles in a pellet state, a melt spinning method may be used as it is. Alternatively, titanium dioxide and polyester may be directly melt-kneaded with an extruder and melt-spun without pelletizing.

Examples of the method for forming fine irregularities on the surface of the polyester fiber of the present invention include a plasma treatment, a laser treatment, and an alkali weight reduction treatment, and the alkali weight reduction treatment is preferred. As the alkali, a compound such as NaOH, KOH, or LiOH can be used as an aqueous solution. Its concentration is 0.5-10
% Is preferred.

The cross-sectional shape of the polyester fiber of the present invention is not limited to a round shape, but may be a polygonal shape, an H-shaped shape, a Π-shaped shaped cross-section, or the like, and the thread form may be either a filament or a staple. The fabric form can be appropriately selected depending on the purpose, such as a woven fabric, a knitted fabric, and a nonwoven fabric.

In addition, the polyester fibers of the present invention include:
As long as the object of the present invention is not impaired, particles such as calcium carbonate, silicon dioxide, talc and organic crosslinked particles may be blended. Also, as long as the effects of the present invention are not impaired,
Various stabilizers, flame retardants, antistatic agents, hydrophilic agents and the like can be optionally used.

[0026]

The present invention will be described below in detail with reference to examples. The measuring method used in the examples is as follows.

(A) Average particle diameter of particles: Determined by an electron micrograph of the particles.

(B) Alkali weight reduction processing: The knitted tube was treated with a 3% aqueous solution of caustic soda at 98 ° C. until the desired weight reduction rate was reached. All weight loss rates are weight ratios.

(C) Stick-slip characteristics: As shown in FIG. 1, a cylindrical knitted fabric knitted with 26G having fine irregularities formed on the surface of a fixed cylinder by alkali weight reduction as shown in FIG. The load 1
(10 g) and a very slow speed (4 mm /
Minutes). At this time, if the device has the stick-slip characteristic, a stress elongation curve as shown in FIG. 2 is obtained. Therefore, an average Δf is obtained from the waveforms at the five points.

(D) Texture: The micropowder touch was evaluated by sensory evaluation by 5 persons, and 0 or 1 persons recognized ×, 2 or 3 persons △, four persons ○, 5 persons
In the case of all the persons, it was evaluated as ◎, and only ◎ was judged as passed .

Example 1 The primary particles have an average particle size of 70 nm and 2 parts by weight of anatase type titanium dioxide fine particles containing 3.0% of aluminum in terms of alumina and 98 parts by weight have an intrinsic viscosity of 0.65.
Was mixed with an extruder to obtain polyester pellets containing 2.0% by weight of titanium dioxide fine particles.

This pellet was spun by a usual melt spinning method and then drawn to obtain a drawn yarn of 75 denier and 24 filaments without breaking. This was made into a tubular knitted fabric, and a 20% weight reduction process was performed with a 3% by weight aqueous solution of sodium hydroxide. There were many very fine irregularities on the surface of the fiber after the weight reduction processing.

A part of the tubular knitted fabric was disassembled and the stick-slip between the fibers was measured to determine Δf. The results are summarized in Table 1. The result of the sensory evaluation was that the powder had micro powder touch properties and had a good texture.

Examples 2 to 4 and Comparative Examples 1 to 13 A knitted material was obtained in the same manner as in Example 1 except that the content of titanium dioxide and the reduction rate of alkali were changed. As shown in Table 1, Examples 2 to 12 had stick-slip characteristics and had a micro powder touch feeling.

On the other hand, for Comparative Examples 1 to 13 , Δf
Was less than 0.030 g / d and did not have a good micropowder touch texture. Further, when the amount of particles exceeded 10% by weight as in Comparative Example 13 , yarn breakage occurred during spinning, and evaluation could not be performed.

[0036]

[0037]

[Table 1]

[0038]

[0039]

[0040]

The pellets were spun by a conventional melt spinning method and then drawn to obtain a drawn yarn of 75 denier and 24 filaments without breaking. This was made into a tubular knitted fabric, and a 20% weight reduction process was performed with a 3% by weight aqueous solution of sodium hydroxide. There were many very fine irregularities on the surface of the fiber after the weight reduction processing. By disassembling a part of the tubular knitted fabric and measuring the stick slip between the fibers, the Δf
I asked. The results are summarized in Table 3. As a result of the sensory evaluation, the powder had micropowder touch properties and had a good texture.

Examples 5 to 9 and Comparative Examples 14 to 31 Fabrics which were subjected to weight reduction processing in the same manner as in Example 1 except that the content, particle diameter and alkali weight loss of zirconium oxide particles were changed. As shown in Table 3, Examples 5 to 9 had a stick-slip property and a high quality micro powder touch feeling after alkali weight reduction processing. On the other hand, for Comparative Examples 14 to 31 , Δf
It was less than 0.030 g / d and did not have a micro powder touch feeling. Further, when the amount of particles exceeded 10% by weight as in Comparative Example 31 , yarn breakage occurred during spinning, and evaluation could not be performed.

[0043]

[Table 2] Example 10 Dimethyl terephthalate (97 mol% of all acid components), 5
-Dimethyl sodium sulfoisophthalate (3 of the total acid component)
Mol%), ethylene glycol (molar ratio to dimethyl terephthalate 2.0) and lithium acetate dihydrate (0.03% by weight to dimethyl terephthalate)
Into a transesterification can and melted at 135 ° C.
The temperature was raised to 25 ° C. over 4 hours, and methanol generated by the transesterification was distilled out of the system (reaction rate: 95% or more). Further, 0.03% by weight of lithium acetate dihydrate (vs. dimethyl terephthalate) and 0.12% by weight of trimethyl phosphate (vs. dimethyl terephthalate) were added and reacted for 30 minutes. Let out. 0.03% by weight of antimony trioxide
After adding (vs. dimethyl terephthalate), the mixture was transferred to a polymerization vessel and heated from 240 ° C. to 290 ° C. over 1 hour and 30 minutes. At the same time, the pressure was reduced from normal pressure to 1 mmHg. Further, the mixture was polymerized for 3 hours to obtain a polyester having an intrinsic viscosity of 0.55. The polyester contained 0.18% by weight of insoluble particles. The polyester was converted into a fiber in the same manner as in Example 1 and then knitted into a tubular knitted fabric to reduce alkali (20).
%)did. There were many very fine irregularities on the surface of the fiber after the weight reduction processing. When the stick-slip property was measured, Δf was 0.052 g / d, and the powder had a micro powder touch feeling.

[0044]

The polyester fiber obtained by the present invention has a high quality dry touch feeling, is excellent in wearing comfort, and can be used for a wide range of applications. In particular, blouses,
It is extremely practical for sportswear and lining.

[Brief description of the drawings]

FIG. 1 is a schematic view of a method for measuring the stick-slip property of the polyester fiber of the present invention.

FIG. 2 is an example of a stress-elongation curve diagram of a stick-slip of the polyester fiber of the present invention.

[Explanation of symbols]

 1. Load 2. 2. polyester fiber sample Fixed cylinder 4. Rotating roller 5. Tension gauge

──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-58-104215 (JP, A) JP-A-60-71768 (JP, A) JP-A-55-107512 (JP, A) JP-A-58-104 4818 (JP, A) JP-A-3-124852 (JP, A) JP-A-56-101913 (JP, A) JP-A-5-171014 (JP, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) D01F 1/00-6/94 D06M 11/38

Claims (2)

(57) [Claims] 1. The primary particles have an average particle size of 50 to 120 n.
polyester fiber containing 1.2 to 8.0% by weight of titanium dioxide fine particles having fine irregularities on the fiber surface and having a stress change Δf of a stick-slip curve of 0.
A polyester fiber having a weight of 030 g / d or more. 2. The average particle diameter of primary particles is from 5 to 200 nm.
Polyester fiber containing 1.0 to 6% by weight of zirconium oxide particles, having fine irregularities on the fiber surface,
And the stress change Δf of the stick-slip curve is 0.03
A polyester fiber having a weight of 0 g / d or more.