KR101781935B1 - Low-melting point polyester fiber having cation dyeable - Google Patents

Abstract

The present invention relates to a low-melting point polyester composite fiber having cis-core type cation dyeability. The composite fiber is made by cation dyeable low-melting point polyester as a cis component and cation dyeable polyester as a core component. The cation dyeable low-melting point polyester is made by copolymerizing: acid components consisting of dimethyl terephthalic acid or terephthalic acid and dimethyl adipic acid or adipic acid; diol components consisting of ethylene glycol, 1,4-cyclohexane dimethanol and 1,4-buthanediol; and 5-sodium sulfoisophthalate. The cation dyeable polyester is made by copolymerizing an acid components consisting of terephthalic acid, a diol components consisting of ethylene glycol and 5-sodium sulfoisophthalate.

Description

[0001] The present invention relates to a low-melting-point polyester fiber having a cationophilic property,

The present invention relates to a low-melting-point polyester-based conjugate fiber having cationophilic properties, which is formed so that all the conjugate fibers have cationophilic properties and has a cationophilic property, .

BACKGROUND OF THE INVENTION [0002] Polyester fibers have excellent physical and chemical properties and are used in a variety of fields, mainly for clothing and industrial applications.

Polyester fibers have been variously functionalized polyester fibers since its launch since copolymerization of monomeric terephthalic acid or dimethyl terephthalate with ethylene glycol and various copolymerizable monomers as a polymerization raw material has been made possible.

A cationophilic polyester fiber has been developed as one of various polyester fibers.

Generally, polyester fibers have a poor dyeability due to their dense fiber structure. When cate- tion dyes and disperse dyes are used, there is a problem in that dyeability is deteriorated at high temperature and high pressure of 130 ° C or when a carrier agent of organic solvent is not used.

In order to solve this problem, in JP-A-6-184820 and JP-A-2000-355831, dicarboxylic acid having a sulfonic acid metal base is copolymerized as a dicarboxylic acid component, whereby a cationic dye and a disperse dye A dye-transferable polyester fiber has been proposed.

When imparting cationic flame resistance to the fibers of the cis-core type conjugate fiber among the polyester fibers, a copolymer material which improves the cationic fluorine-containing property is used to improve the dyeability.

In order to heat-treat the polyester fiber at a melting point of about 270 ° C, the polyester fiber can be heat-treated at a very high temperature, resulting in a problem of a large energy consumption. In order to solve this problem, US Patent Nos. 4,129,675 and 4,065,439 , A polyester fiber in which the melting point of a polyester fiber is lowered to 200 캜 by copolymerizing isophthalic acid, adipic acid and neopentyl glycol has been proposed.

As described above, polyester fibers having various functionalities have been developed through various kinds of copolymer materials, and there is a need to develop multifunctional polyester fibers due to the increasing needs of consumers and the advancement of the textile industry.

It is an object of the present invention to solve the problems of the prior art as described above and to provide a cation-exchange resin capable of imparting cationophilicity to a cis-core type low melting point conjugated fiber, It is an object of the present invention to provide a polyester-based composite fiber having a melting point.

It is another object of the present invention to provide a low-melting-point polyester-based conjugated fiber having cationophilic properties, in which the sheath portion and the core portion all have a cationic fluorosilvering property and thus the dyeability is greatly improved.

The present invention relates to a low-melting-point polyester-based conjugate fiber having a cis-core type cationic fluorophore, wherein the conjugate fiber is composed of a cationophilic low-melting-point polyester as a sheath component and a cationophilic polyester as a core component The cationically labile low melting point polyester is obtained by reacting an acid component consisting of dimethyl terephthalic acid or terephthalic acid and dimethyl adipic acid or adipic acid with a diol component comprising ethylene glycol, 1,4-cyclohexanedimethanol and 1,4-butanediol, And sodium 5-sulfoisophthalate, and the cationic saltable polyester is formed by copolymerizing an acid component of terephthalic acid with a diol component of ethylene glycol, and sodium 5-sulfoisophthalate. The present invention provides a low-melting-point polyester-based conjugated fiber.

The cationically labile low-melting-point polyester may further contain 1 to 10 mol% of the dimethyl adipic acid or adipic acid, 1 to 20 mol% of the 1,4-cyclohexanedic acid dimethanol, And the content of 1,4-butanediol is 30 to 50 mol%.

Further, the sodium 5-sulfoisophthalate copolymerized with the cationic, low-boiling point polyester having a cationic group is contained in an amount of 1 to 3 mol% based on the molar amount of the ester. Thereby providing a composite fiber.

In addition, the sodium 5-sulfoisophthalate copolymerized with the cationic phosphatizable polyester is contained in an amount of 1 to 3 mol% based on the molar amount of the ester. The low melting point polyester- Lt; / RTI >

In addition, the cross-sectional area ratio of the sheath-core of the conjugate fiber is 6: 4 to 2: 8, and provides the low melting polyester conjugate having cationophilic properties.

As described above, the low-melting-point polyester-based conjugate fiber having cationophilic properties according to the present invention contains a copolymer which imparts a cationophilic halophilic property to both the sheath portion and the core portion, have.

In addition, the cite-core type low-melting-point conjugated fiber is imparted with a cationic fluorine-containing capability, so that it has an excellent durability and can be used for various purposes.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a graph showing the surface bonding density (K / S) of a low-melting polyester conjugate fiber having cationophilic properties according to the present invention, according to the wavelength band.

Hereinafter, a preferred embodiment of the present invention will be described in detail. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted so as to avoid obscuring the subject matter of the present invention.

As used herein, the terms " about, " " substantially, " " etc. ", when used to refer to a manufacturing or material tolerance inherent in the stated sense, Accurate or absolute numbers are used to help prevent unauthorized exploitation by unauthorized intruders of the referenced disclosure.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a graph showing the surface bonding density (K / S) of a low-melting polyester conjugate fiber having cationophilic properties according to the present invention, according to the wavelength band.

The present invention relates to a low-melting-point polyester-based conjugate fiber having a cis-core type cationic salt form, a cationic salt-forming low-melting-point polyester as a sheath component and a cationic saltable polyester as a core component.

The cationic salt-imparting low-melting point polyester as the sheath component is obtained by reacting an acid component consisting of dimethyl terephthalic acid or terephthalic acid and dimethyl adipic acid or adipic acid with a diol component composed of ethylene glycol, 1,4-cyclohexanedimethanol and 1,4- And sodium 5-sulfoisophthalate.

Dimethyladipic acid and adipic acid used in the present invention have flexibility and are introduced into one of the acidic components of the copolymer polyester to increase the possibility of flow of the whole molecular chain so as not to interfere with the crystallinity of 1,4- The melting point of the non-woven fabric is lowered to facilitate processing, and the soft molecular chain existing in the main chain of the polymer improves the elasticity to improve the tear property at the time of nonwoven binding.

The content of the dimethyladipic acid or the adipic acid is preferably 1 to 10 mol% based on the mole of the ester of the cationic saltable low melting point polyester. When the content is less than 1 mol% If the content is more than 10 mol%, the crystallinity of the cationic fluorine-containing low melting point polyester is lowered and a glass transition temperature of 40 ° C. or higher can not be obtained.

On the other hand, the acid component of the remaining 90 to 99 mol% of the cationic saltable low melting point polyester is composed of dimethyl terephthalic acid or terephthalic acid.

The 1,4-cyclohexanedic acid dimethanol contained in the cationophilic low-melting point polyester is introduced as one of the diol components of the copolymer polyester as an aliphatic cyclic compound, and serves to maintain the glass transition temperature while lowering the melting point.

At this time, the content of the 1,4-cyclohexanedic acid dimethanol is preferably 1 to 20 mol% based on the mole of the ester of the cationophilic low melting point polyester. When the content is less than 1 mol% And a glass transition temperature of 40 DEG C or higher can not be obtained. When the content exceeds 20 mol%, the crystallinity of the copolyester is excessively lowered to exhibit a softening behavior in a wide temperature range.

The 1,4-butanediol contained in the cationic low-boiling point polyester is introduced into another one of the diol components of the cationic low-boiling polyester having a high crystallinity and remains crystalline even during copolymerization, It can be thermally adhered even at a temperature higher by 5 캜 than the melting point of the coalescence, and there is an advantage that the copolymer is hardly deformed because of the strong crystallinity at a temperature below the melting point.

The content of 1,4-butanediol is preferably 30 to 50 mol% based on the molar amount of the ester of the cationophilic low melting point polyester. When the content is less than 30 mol%, the fusion temperature is high, But it does not serve as a binder. When it exceeds 50 mol%, 1,4-butanediol becomes the main component of the diol component and the fusion temperature rises again.

On the other hand, the remaining diol component of the cationic, salt-lowering low melting point polyester is composed of ethylene glycol.

Sodium 5-sulfoisophthalate contained in the cationic salt-lowering low-melting-point polyester is a substance which is copolymerized with polyester to give a cationic salt-imparting property, and the content of sodium 5-sulfoisophthalate in the cationic salt- It is preferable that the content is 1 to 3 mol% based on the molar amount of the ester of the low melting point polyester. If the content is less than 1 mol%, a satisfactory cationophilization performance can not be obtained. If the content is more than 3 mol% - Thickening and gelation due to the charge of sodium sulfoisophthalate may occur, which may reduce the radiation processability.

The cationic saltable polyester, which is the core component, is a copolymer formed by copolymerizing an acid component of terephthalic acid with a diol component of ethylene glycol, and sodium 5-sulfoisophthalate.

The sodium 5-sulfoisophthalate contained in the cationic saltable polyester is copolymerized in order to impart the cationic salt-imparting property to the core component, and is used in an amount of 1 to 3 moles based on the mole of the ester of the cationic saltable polyester % Is preferably contained.

The cross-sectional area ratio of the cis-core of the low-melting polyester conjugate fiber having a sheath-core type cationophilic property according to the present invention is preferably from 6: 4 to 2: 8. If the cross-sectional area ratio of the sheath is too large, , Tensile strength and the like can be improved, but a strong sense of touch can be obtained when the fabric is manufactured. If the cross-sectional area ratio of the sheath is too small, the fiber fairness may be deteriorated and the physical properties may deteriorate during fabrication.

As described above, the low melting point polyester-based conjugated fiber having cationophilic properties according to the present invention has a high crystallinity and has a low glass transition temperature and a glass transition temperature of 40 ° C or higher at a temperature below the melting point Thereby delaying the rate of change of the fiber due to the low glass transition temperature in the spinning and drawing process of the conjugate fiber to prevent a decrease in productivity due to the occurrence of adhesion between adjacent fibers in the process, .

In addition, the cation and the cation are both imparted to the sheath and the core, and the dye is dyed uniformly over the whole of the fiber when dyeing with a cationic dye, so that the dyestuff can be dyed with a small amount of dye because of high dyeability.

Hereinafter, examples of the method for producing the low-melting-point polyester-based conjugated fiber having cationophilic properties according to the present invention will be described, but the present invention is not limited to the examples.

Example  1 to 3

The cationic, low-boiling point cationic polyester used as the sheath component is prepared by adding dimethyl terephthalic acid / dimethyl adipic acid (DMA) as an acid component and ethylene glycol / 1,4-cyclohexanedimethanol (CHDM) / 1 as a diol component to the ester- 4-butanediol (BD), and sodium 5-sulfoisophthalate (DMS) were added to give a cationic salt form, followed by addition of a conventional esterification catalyst at a temperature of 150 ° C., And an ester exchange reaction was carried out at a temperature of 200 ° C to prepare an oligomer. The oligomer thus obtained was fed with a conventional polycondensation catalyst, and the polycondensation reaction was carried out by raising the temperature to 260 ° C while gradually reducing the pressure to 0.1 mmHg.

The cationophilic polyester used as the core component was prepared in the same manner as above but terephthalic acid as an acid component, ethylene glycol as a diol component and sodium 5-sulfoisophthalate (DMS) were used.

Using the sheath and core components prepared above, 75D / 36F low melting point polyester conjugate fibers according to the present invention having cationophilic properties were prepared by a conventional method for producing conjugate fibers.

In Examples 1 to 3, the content of dimethyl adipic acid (DMA), 1,4-cyclohexanedic acid dimethanol (CHDM), 1,4-butanediol (BD), sodium 5-sulfoisophthalate (DMS) The content of each of the copolymer materials is shown in Table 1 based on the molar amount of the ester of the cationophilic low-melting-point polyester or the cationophilic polyester.

Comparative Example  One

The polyester-based conjugated fiber was prepared in the same manner as in the above example, but was produced without using a copolymer material in the sheath and core.

Comparative Example  2

Polyester composite fibers were prepared in the same manner as in Example 1 except that the core component was prepared without using sodium 5-sulfoisophthalate (DMS).

Comparative Example  3

The polyester-based composite fiber was prepared in the same manner as in Example 1, except that 5-sulfoisophthalic acid sodium (DMS) was not used in the sheath component.

◈ Evaluation experiment of examples and comparative examples

The melting point, glass transition temperature, adhesion, and dyeing characteristics of Examples 1 to 3 and Comparative Examples 1 to 3 prepared above were evaluated and shown in Table 1.

The melting point / glass transition temperature was measured by measuring the sheath component, and the adhesive strength was measured using a composite fiber of Examples 1 to 3 and Comparative Examples 1 to 3 as short fibers, followed by a heat fusion process as a nonwoven fabric, The dyeing characteristics were measured by dyeing the composite fibers with a circular blue dye (1 owf%) at 110 ° C for 30 minutes using an IR stainer after circular knitting. The evaluation results of Examples 1 to 3 and Comparative Examples 1 to 3 are shown in Table 1.

[Assessment Methods]

* Melting point / glass transition temperature and softening behavior measurement

: Measured using a thermal differential scanning calorimeter (Perkin Elmer, dsc-7). When there is no heat absorption peak, that is, when no melting point exists, the softening behavior is measured using a dynamic thermal property measuring device (Perkin Elmer, DMA-7)

* At room temperature adhesion and high temperature adhesion measurement

: The prepared thermally fused bonded nonwoven fabric was fixed at a density of 2 g / 100 cm 2, and the room temperature adhesive strength was measured at 25 ° C. at room temperature by the method of ASTM D 1424, and the high temperature bonding strength was measured at 100 ° C. (dry heat)

* Maximum dyeing temperature: After dyeing for 30 minutes by temperature up to 80 ~ 130 ℃,

* Surface Dyeing Concentration (K / S)

○ Measurement of surface dyed density (K / S) by dyed circular knitted fabric using a contact type spectrophotometer (Bench-top Spectrophotometer)

- Contact type spectrophotometer: Manufacturer X-rite, Model Color-Eye 7000A

- High-resolution spectroscopic color measurement equipment that outputs the spectral distribution and the tristimulus value by measuring the reflection spectrum of the surface or the transmission spectrum of the transparent semitransparent object in a contact manner

○ The reflectance of each wavelength band is measured and the K / S value is obtained from the surface reflectance of the maximum absorption wavelength as the apparent color density (durability) by the following Kubelka-Munk equation

K / S = (1 - R) ² / 2R

K: absorption coefficient

S: scattering coefficient

R: reflectance

FIG. 1 shows surface contamination concentrations according to the wavelength ranges of Example 1, Comparative Example 2, and Comparative Example 3.

* Wash fastness: measured according to KS K ISO 105 C06 (washing temperature 40 ± 2 ℃, washing time 30 minutes, 0.4% ECE standard detergent, 0.1% sodium borate)

division Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Sheath
Copolymerized feed composition
(mol%) DMA 8 8 8 - 8 8 BD 40 40 40 - 40 40 CHDM 6 6 6 - 6 6 DMS 1.8 1.8 1.8 - 1.8 - Core
Copolymerized feed composition
(mol%) DMS 1.5 1.5 One - - 1.5 Sheath: Core ratio 4: 6 2: 8 4: 6 4: 6 4: 6 4: 6 Melting point (캜) 165 160 162 256 163 165 Glass transition temperature (캜) 43 48 45 75 45 48 Adhesion Adhesion at room temperature (kg) 4.1 3.4 4.4 0 4.1 4 High Temperature Adhesion (kg) 2.3 2.2 2.3 0 2.1 2.2 Dyeing properties Maximum Fertilization Temperature 110 110 110 130 110 110 Surface soil concentration 27.2 26 23.5 2.0 11 4.3 Wash fastness 5th grade 5th grade 5th grade 2nd grade 5th grade 5th grade

As shown in Table 1, Examples 1 to 3, which are low-melting-point polyester conjugated fibers having cationophilic properties according to the present invention, have a melting point of about 160 to 165 ° C, a glass transition temperature of 40 ° C or more, And it can be seen that it has an excellent measurement value in terms of adhesion.

In addition, the surface adhesion concentration (K / S) in the dyeing characteristics was much higher than those of Comparative Examples 2 and 3 in which Examples 1 to 3 had catechin fluoride solely in the sheath component and Comparative Example 3, .

As shown in Table 1 and FIG. 1, since the concentration of the surface dyes in the Examples is higher than that in Comparative Examples 2 and 3, the content of sodium 5-sulfoisophthalate (DMS) It can be deduced that the workability is increased and the rate of saltation with the cationic dye increases. When the cationic salt-imparting property is imparted to both the sheath and core components, the dyeing performance is remarkably improved.

Claims (5)

In a low-melting-point polyester-based conjugate fiber having a cis-core type cationic salt-
Wherein the conjugate fiber is formed of a cationophilic low melting point polyester as a sheath component and a cationophilic polyester as a core component,
The cationically labile low-melting-point polyester comprises an acid component consisting of dimethyl terephthalic acid or terephthalic acid and dimethyl adipic acid or adipic acid, a diol component comprising ethylene glycol, 1,4-cyclohexanedimethanol and 1,4-butanediol, and 5- And sodium sulfoisophthalate,
The cationic saltable polyester is formed by copolymerizing an acid component of terephthalic acid with a diol component of ethylene glycol and sodium 5-sulfoisophthalate,
Sodium 5-sulfoisophthalate copolymerized with the cationic, low-boiling point polyester is contained in an amount of 1 to 3 mol% based on the molar amount of the ester, and 5-sulfoisophthalic acid copolymerized with the cationic- Sodium is contained in an amount of 1 to 3 mol% based on the molar amount of the ester to form a low melting polyester conjugate fiber,
The cationic salt-forming low-melting-point polyester has a melting point of 160 to 165 ° C, a glass transition temperature of 40 ° C or higher, and a low melting point polyester-based conjugate fiber has a surface binding concentration (K / S) Wherein the low melting point polyester-based conjugated fiber has a cationophilic property. The method according to claim 1,
The cationically labile low-melting-point polyester comprises 1 to 10 mol% of the dimethyl adipic acid or adipic acid, 1 to 20 mol% of the 1,4-cyclohexanedic acid dimethanol, And the content of 4-butanediol is 30 to 50 mol%. delete delete The method according to claim 1,
Wherein the cross-sectional area ratio of the sheath-core of the composite fiber is 6: 4 to 2: 8.

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