KR100519164B1 - Deeply dyeable polyester sea-and-island type conjugated fiber and manufacturing thereof - Google Patents

Abstract

The present invention relates to a polyester islands-in-the-sea composite yarn and a method for producing the same, wherein the island component is modified to be dyed deep.

Specifically, polyester islands-in-the-sea composite yarn prepared using a deep color copolyester polymer obtained by polymerizing cyclohexane 1,4-dimethanol 1 to 10 mol% with respect to the glycol component of the entire polymer, and its components. It relates to a manufacturing method.

The polyester islands-in-the-sea composite yarn of the present invention can be manufactured using the manufacturing facilities of the conventional polyester islands-in-the-sea composite yarn, and the microfiber yarn by the island component can be dyed darker than the conventional polyethylene terephthalate fiber and has excellent fastness.

Description

Deep colorable polyester islands-in-the-sea composite yarn and its manufacturing method {Deeply dyeable polyester sea-and-island type conjugated fiber and manufacturing conjugate}

The present invention relates to a polyester islands-in-the-sea composite yarn which can be dyed in deep colors and a method for producing the same.

More specifically, a copolyester polymer obtained by polymerizing cyclohexane 1,4-dimethanol 1 to 10 mol% with respect to the glycol component of the entire polymer is used as an island component. The present invention relates to a deep color polyester islands-in-the-sea composite yarn prepared using an soluble copolyester copolymerized with sulfonic acid metal salt, isophthalic acid and polyethylene glycol, and a method for preparing the same.

Polyester island-in-the-sea composite yarn is a high value-added fiber that can manufacture high-quality papers, artificial leather, high-quality suede, etc., and various manufacturing methods have been proposed so far. Much is not known about the modification of the island component only as a method for producing the yarn.

Indeed, as a method for modifying the island component, a method of preparing deep color polyester islands-in-the-sea composite yarn using inorganic particles as disclosed in Korean Patent Application Laid-Open Publication No. 1998-055563 and high fastness as disclosed in Korean Patent Application Publication No. 2002-48331 And a method for producing a primary island-in-the-sea composite yarn.

However, the method of making a flaw on the surface of the fiber by inorganic silica or titanium dioxide may deteriorate the spinning workability during the production of ultrafine yarns due to their cohesion, etc. The primary islands-in-the-sea composite yarn made of carbon black is determined to have only one color. There is a problem that is difficult to apply to.

In particular, the polyester islands-in-the-sea composite yarn is so thin that its thickness is so thin that it is difficult to dye it with a dark color when dyed by the general polyester fiber dyeing method. Occurred.

SUMMARY OF THE INVENTION An object of the present invention is to provide a polyester islands-in-the-sea composite yarn and a method of manufacturing the same to increase the amorphous area of the island component of the polyester islands-in-the-sea composite yarn.

The present invention will be described in detail.

The present inventors made a specific polymerized product and selected it as a polymer of an island component in order to achieve the objective of this invention as mentioned above.

In the present invention, a copolymer having a structure capable of increasing the amorphous region in the polymer while increasing the fastness without causing a decrease in the glass transition temperature is used as the polymer of the island component for achieving color depth.

In this invention, the copolymerization monomer which can be used for a figure component is chosen from aromatic and alicyclic compounds, such as naphthalene dicarboxylic acid, the ethylene adduct of bisphenol A, and cyclohexane 1, 4- dimethanol.

In particular, in the present invention, cyclohexane 1,4-dimethanol was selected in consideration of the economical aspect and the shrinkage ratio when the yarn was made from yarn.

Since cyclohexane 1,4-dimethanol is a compound having an isomer of cis type and a trans type, the cyclohexane hexane 1,4-dimethanol has an advantage of increasing the amorphous region even when a smaller amount than other copolymerizing monomers is used.

In the present invention, the island component is a cyclohexane 1,4-dimethanol (Cyclohexane 1,4-dimethanol, hereinafter abbreviated as CHDM) is a copolymerization of 1 to 10 mol% compared to the glycol component of the entire polymer.

When it exceeds 10 mol%, the shrinkage ratio becomes too large when the fiber is made from the above fiber, and in particular, when it is higher than 30 mol%, it becomes an amorphous polymer which can hardly be used for fibers.

If it is less than 1 mol%, the object of the present invention, which is an increase in the amorphous region, cannot be achieved.

Since the dissolution rate in the alkaline solution should be very fast, the bishydroxy ethyl isophthalate containing a soluble copolyester polymer, ie, a metal sulfonate salt, disclosed in Korean Patent Application No. 2003-0026652. When the component is polymerized, 1 to 6 mole% of the dieside component in the polymer is added, 0.01 to 5% by weight of the isophthalic acid component is added, and the polyalkylene glycol having an average molecular weight of 1,000 to 20,000 is polymerized. A water-soluble copolyester was added to copolymerize 3 to 15% by weight.

In the present invention, a TPA polymerization method using terephthalic acid (hereinafter abbreviated as TPA) as a raw material was used as a polymerization method of copolyester. In general, as the polymerization method of copolyester, a polymerization method using TPA as a raw material and a method using dimethyl terephthalate as a raw material are known, but from the viewpoint of economics in the production of polymers, a method using TPA as a raw material is much more advantageous. .

However, in the polymerization method of the copolyester containing CHDM, the unreacted TPA is non-soluble and non-meltable, so that the oligomer filter or the polymer filter of the polymerizer occurs, or the pack pressure rise rate increases during spinning. There is a problem that workability is degraded.

Therefore, the amount of unreacted TPA should be minimized. For this purpose, the esterification time should be increased or the esterification temperature should be increased.

However, increasing the esterification time or increasing the esterification temperature is not good because it increases the amount of DEG, a side reaction product, which impairs the thermal stability of the polymer. Therefore, it is better to lower the G value (the ratio of the number of moles of ethylene glycol and CHDM combined to the number of moles of terephthalic acid) to suppress DEG production. Therefore, in the present invention, the G value is set to 1.10 to 1.50. If the G value is within the above range, the content of DEG in the polymer during polymerization may be 0.7 to 2.0% by weight, thereby increasing the amorphous region aimed at by the present invention, and at the same time, it will not cause thermal property deterioration. Problems in the process hardly occur.

Since the copolyester polymer according to the present invention is intended for the fiber for clothing, it is possible to inject Anatase Type Titanium Dioxide like conventional polyester.

The amount of Super Bright is not added at all according to the intended use of the fiber, Bright is 200 to 500 ppm compared to the polymer, Semi-Dull is 1,000 to 5,000 ppm, 10,000 to 40,000 ppm for full-dull.

In addition, in order to increase the specific gravity of the copolyester or to improve the transparency and friction characteristics, barium sulfate may be added in an amount of 5 wt% or less with respect to the copolyester polymer according to the purpose.

Examples of the polycondensation catalyst include antimony-based catalysts such as antimony trioxide and antimony acetate, germanium-based catalysts such as germanium dioxide, and titanium-based compounds such as tetrabutyl titanate and tetraisopropyl titanate. Can be used.

Their input amount is 0.01 to 5% by weight relative to the polymer.

The physical properties of the following Examples and Comparative Examples were measured by the following method.

1. IV: A solution containing 60/40 weight ratio of phenol and 1,1,2,2-tetrachloroethane, measured at 30 ° C. using a Uvelode viscometer.

2. Melting temperature (Tm) and glass transition temperature (Tg): Using a DSC 7 of Perkin Elmer, the temperature was raised to 10 ℃ / min and analyzed as a peak within the melting range.

3. Dyeing property: The prepared yarns were treated with 1.2 wt% NaOH solution for 20 minutes to completely remove the soluble part, and then dyed at 130 ° C with Kuralon Navy Blue, and the color intensity of the dyed fabric was measured using a spectrophotometer. K / S was calculated.

Hereinafter, the present invention will be described in detail with reference to Examples. However, the scope of the present invention is not limited by this embodiment.

<Examples 1-3, Comparative Examples 1-2>

As the sea component, bishydroxy ethyl isophthalate containing a metal sulfonate salt is 5 mol% of the dieside component in the polymer, isophthalic acid component is 2% by weight of the dieside component in the polymer, and a polyalkylene having a molecular weight of 4000 A polymer having an intrinsic viscosity of 0.55 dl / g prepared by copolymerizing glycol to 6 wt% of the polymer was used, and a (co) polyester polymer having physical properties shown in Table 1 was used as a component of the figure.

Using spinning conditions as shown in Table 1, spinning was carried out at a spinning speed of 2800 m / min, followed by drawing ratio of 1.74 to prepare island-in-sea composite yarns having 37 islands of 75 denier and 36 filaments. Table 1 shows.

The prepared yarns were treated in a 1.2 wt% NaOH solution for 20 minutes to completely remove the soluble part, and then dyed at 130 ° C. with Kuralon Navy Blue. The color intensity of the dyed fabric was measured at 500 nm using a spectrophotometer. The comparison is shown in Table 1.

<Table 1>

division Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 CHDM content (mol%) 3 6 9 5 30 G value * 1.20 1.20 1.20 1.80 1.20 Intrinsic viscosity (dl / g) 0.631 0.628 0.617 0.627 0.572 DEG content (% by weight) 1.28 1.34 1.46 2.46 1.78 Compound ratio (weight ratio) 70:30 76:24 70:30 74:24 70:30 Strength (g / d) 3.76 3.72 3.59 3.63 - Elongation (%) 38 40 37 41 - K / S ** 106 112 119 110 -

G value: (EG + CHDM) / TPA molar ratio

** Converted to 100 as the apparent color concentration of general polyethylene terephthalate.

The polyester islands-in-the-sea composite yarn of the present invention maintains the inherent mechanical properties of the polyester yarn as it is, and has the advantage that the fine fine fibers, which are the island components remaining after the sea component is dissolved, can be dyed thick during dyeing.

In addition, the polyester islands-in-the-sea composite yarn according to the present invention has excellent thermal properties, good flammability, and excellent fastness.

Claims (4)

A polyester island-in-the-sea composite yarn comprising a deep color copolyester polymer obtained by copolymerizing cyclohexane 1,4-dimethanol 1 to 10 mol% with respect to the glycol component of the entire polymer. Polyester island-in-the-sea composite yarn. The sea component is a bishydroxy ethyl isophthalate component containing a metal sulfonate salt containing 1 to 6 mol% of the dieside component in the polymer, wherein the isophthalic acid component is selected from the dieside component in the polymer. A deep color polyester islands-in-the-sea composite comprising a copolyester polymer obtained by copolymerizing a polyalkylene glycol having an average molecular weight of 0.01 to 5% and a molecular weight of 1,000 to 20,000 at 3 to 15% by weight relative to the polymer. four. The method of claim 1, wherein the island component is characterized in that the molar ratio (G value) of the diol to the total dieside is 1.10 to 1.50 and the content in the polymer of the diethylene glycol produced as a side reaction is 0.7 to 2.0% by weight. Deep color polyester islands-in-the-sea composite yarn. In preparing the polyester islands-in-the-sea composite yarn, the island component is one obtained by copolymerizing cyclohexane 1,4-dimethanol with respect to the glycol component of the entire polymer, and the sea component is a metal sulfonate salt. The bishydroxy ethyl isophthalate component containing 1 to 6 mol% of the dieside component in the polymer during polymerization, the isophthalic acid component is added to 0.01 to 5% by weight of the dieside component in the polymer, the average molecular weight is 1,000 to A method for producing a deep color polyester islands-in-the-sea composite yarn comprising 20,000 polyalkylene glycols prepared by incorporating 3 to 15% by weight relative to a polymer.