KR0125969B1 - Manufacturing process of easy dyeable polyester fiber - Google Patents

Abstract

As a dibasic acid component, terephthalate acid is used, as a diol component, having ethyleneglicol used, while as the second diol element, 2,2'-bis[4-(2-hydroxy-2-alkylethoxy)phenyl propane is employed to produce a copolymer polyester resin. These elements are compounded to obtain a slurry, which is spun at the highest speed, 5000, by the spin draw method, 6500m/min to produce a polyester fiber with differant dyeability.

Description

Manufacturing method of dibasic polyester fiber

The present invention relates to a method for producing a dibasic polyester fiber, and in detail, terephthalic acid is used as a diacid component, and ethylene glycol and 2,2'-bis [4- (2) are used as a diol component. -Hydroxy-2-alkylethoxy) phenyl] propane or 2,2'-bis [4- (2-hydroxy-1-alkylethoxy) phenyl] propane was polymerized in a conventional manner and then 5000 It relates to a method for producing a dibasic polyester fiber characterized in that the ultra-fast spinning at 6500m / min.

In general, the microcrystalline structure in polyester differs from polyester copolymerized by adding a third component and ordinary polyester without the third component and also depends on the spinning speed. When the polyester copolymerized by adding the third component is spun at a low speed of 1500 m / min or less, the degree of crystallinity is low and the non-orientation part is large. In the case of spinning a conventional polyester without addition of the third component at a spinning speed of 1500 m / min or less, the degree of crystallinity becomes an average level, but the non-orientation part becomes large. In the case of spinning at a high speed of 5000 m / min or more of ordinary polyester without the third component added, the crystallization becomes high and the non-orientation portion becomes small.

In the case of spinning the copolyester with the third component added at a high speed of 5000 m / min or more, the degree of crystallinity is medium, but the non-orientation part is extremely small.

Disperse dyes used for dyeing the polyester fiber penetrate between the non- governmental chains in terms of polyester microstructure, the degree of crystallinity is directly related to the amount of dispersion dye penetration. If the degree of crystallinity is large, since the non-orientation part is relatively small, the disperse dye penetration amount is small, and if the degree of crystallinity is small, the opposite result is obtained. In particular, non-government is important in dyeing disperse dyes. That is, high-pressure dyeing and normal-pressure dyeing are classified according to the degree of non-precision orientation, that is, the density.

Conventional low-speed spinning elongated polyester fibers (LIDY method) of 1500 m / min or less can be dyed at 130 ° C. high temperature with a disperse dye. When spinning a conventional polyester polymer at 5000 m / min or more, it can be dyed at 120 ℃ lower than 130 ℃. Polyester fibers copolymerized using isophthalic acid, sebacic acid, etc. as diacid components, or neopentylglycol, etc., as diol components, as a third component, have low crystallinity and high non-orientation. In the well dyeing and high non-orientation in terms of high dyeing is not well offset each other can be dyed at about 125 ℃.

When the dyeing operation temperature is lowered from high pressure (130 ℃) to normal pressure (100 ℃), energy input to the dyeing process can be reduced, and especially fabrics where high temperature is a problem can be dyed at normal pressure. There is an advantage that can be prevented, the price of the existing production equipment is significantly lowered, there has been a request for a method of producing a polyester fiber that can be dyed at atmospheric pressure.

The present inventors have studied for the development of a method for producing a dichroic polyester fiber which can be dyed at normal pressure by focusing on the properties of the polyester resin, the microstructure of the polymer according to the spinning speed and the dyeing mechanism (mechanism) by the disperse dye. The present invention has been made.

That is, according to the present invention, terephthalic acid is a diacid component, ethylene glycol is a diol component, and a second diol component is added thereto to prepare a slurry by adding a compound of formula (I) or (II) It is to provide a method for producing a di-chlorinated polyester fiber characterized in that the super fast spinning at a spinning speed of 5000 to 6500m / min by the polymerization method by the spin draw method.

(Where R is one of methyl, ethyl, normal propyl, isopropyl, normal butyl or isobutyl groups)

Hereinafter, the present invention will be described in more detail.

In the present invention, terphthalic acid is used as a diacid component, 2,2'-bis [4- (2-hydroxy-2-alkylethoxy) of general formula (I) as ethylene glycol and a second diol component as diol components Copolymerized polyester resin is prepared using) phenyl] propane or 2,2'-bis [4- (2-hydroxy-1-alkylethoxy) phenyl] propane of general formula (II).

Here, these components are mixed to prepare a slurry, but the content of each monomer component is prepared according to the following formula.

In the above formula, the molar ratio is fixed at 1.1, and the excess component of diol (part at 1.1 corresponding to molar ratio of 0.1) is always ethylene glycol, and the content of the second diol component is from 8 mol% to 15 mol% with respect to terephthalic acid. Shall be. In this component ratio, the best results are obtained in the dyeing and spinning workability of 5000 to 6500 m / min. When the third diol component is less than 8 mol%, dyeing is impossible at 100 ° C., and the amorphous structure is more than 15 mol%. Since it is not only poor spinning workability but also the strength of the yarn is lowered to obtain the desired yarn.

Polyester fiber copolymerized by using isophthalic acid, sebacic acid, or the like as a diacid component or by adding neopentylglycol as a third component can be dyed at 125 ° C., but it is a dibasic polyester fiber obtained by the present invention. Since the special diacid component and the second diol component can be added and dyed at 100 ° C. under normal pressure, there is an energy saving effect, and particularly in the case of a fabric that is weak to heat, there is an advantage of preventing damage to the fabric.

In addition, the non-shrinkage rate of 7.5% is significantly larger than the 3.6% of the fiber produced by the ultra-fast spinning method generally can greatly contribute to the fabric density improvement.

The present invention is described in more detail with reference to the following Examples, but the present invention is not limited by the following Examples.

Example 1

100 parts by weight of terephthalic acid (TPA) as a diacid component, 38 parts by weight of ethylene glycol (EG) as a diol component 2,2'-bis [4- (2-hydroxy-1-isopropylethoxy) as a second diol component 20 parts by weight of phenyl] propane (10 mol% relative to terephthalic acid) is added to prepare a slurry.

In preparing the slurry, 20 parts by weight of 2,2'-bis [4- (2-hydroxy-1-isopropylethoxy) phenyl] propane, the second diol component, was added to 38 parts by weight of ethylene glycol at 50 ° C. To dissolve until the ethylene glycol solution becomes clear. After complete dissolution, 100 parts by weight of terephthalic acid is added to the solution to be mixed for good dispersion.

The slurry is added stepwise to a direct esterification tank containing 120 parts by weight of low molecular weight (oligomer) of 260 ℃, equipped with a distillation column. When the slurry is directly added to the esterification tank and the low molecular weight reaches 258 ° C., the slurry is stopped. In the direct esterification bath, the above process is repeated in conjunction with the temperature of the reaction contents.

After the slurry is added, a low-molecular weight product is prepared by performing a finishing reaction for about 30 minutes. Subsequently, the prepared low molecular weight was transferred to a polycondensation reaction tank, 400 ppm Sb ₂ O ₃ was added as a polymerization catalyst and 150 ppm triphenylphosphine as a stabilizer, and mixed at 280 ° C. for 5 minutes, followed by 1 hour under high vacuum of 0.1 mmHg or less. By reacting for about 30 minutes to prepare a high shrinkage copolymer polyethylene terephthalate resin having an intrinsic viscosity of 0.64.

The spinning adopted the ultra-fast spinning method. By using a draw roller, the so-called spin-draw method (spin-draw method), which simultaneously spins and stretches, makes the winding speed 6000m / min, spinneret diameter 0.2mm (24 holes), and makes the fineness 75 denier. Dibasic polyester fibers were prepared.

The physical properties and the dyeing properties of the prepared dibasic polyester fibers are evaluated and shown in Table 1 below.

Example 2

Instead of using 2,2'-bis [4- (2-hydroxy-2-isopropylethoxy) phenyl] propane as the second diol component, 2,2'-bis [4- (2-hydroxy It is dibasic in the same manner as in Example 1 except that 20 parts by weight of -2-isopropylethoxy) phenyl] propane (10 mol% based on terephthalic acid) were added to prepare a dibasic polyethylene terephthalate having an intrinsic viscosity of 0.65. To prepare a polyester fiber and to evaluate the physical properties and dyeing properties of the prepared di-chloride polyester fiber is shown in Table 1 below.

Comparative Example 1

A slurry is prepared by adding 90 parts by weight of terephthalic acid as a diacid component, 10 parts by weight of isophthalic acid (10 mol% based on the total diacid components) and 38 parts by weight of ethylene glycol as the diol component. Subsequently, a polyethylene terephthalate resin having an intrinsic viscosity of 0.62 was prepared in the same manner as in Example 1, ultrafast spinning was used to prepare a dibasic polyester fiber, and the physical properties and dyeing characteristics of the prepared dibasic polyester fiber were evaluated. Shown together.

Comparative Example 2

A slurry was prepared from 100 parts by weight of terephthalic acid, 38.5 parts by weight of ethylene glycol, and 6.4 parts by weight of neopentyl glycol (10 mol% based on terephthalic acid) to prepare a polyethylene terephthalate resin having an intrinsic viscosity of 0.65 in the same manner as in Example 1. To prepare a dyestuff polyester fiber and to evaluate the physical properties and dyeing properties of the prepared dyestuff polyester fiber shown in Table 1 together.

Comparative Example 3

Polyethylene terephthalate was prepared in the same composition as in Comparative Example 2, and the yarn was stretched at a spinning speed of 120 m / min according to a conventional method to prepare a dyestuff polyester yarn, and evaluated the physical properties and dyeing characteristics of the prepared dyestuff polyester fiber. It is shown together in Table 1 below.

[Comparative Example 4]

A slurry was prepared from 41 parts by weight of terephthalic acid and 41 parts by weight of ethylene glycol without adding a second diol component. A polyethylene terephthalate resin having an intrinsic viscosity of 0.65 was prepared in the same manner as in Example 1, and ultra-fast spinning was used to prepare a dibasic polyester fiber. And to evaluate the physical properties and dyeing properties of the prepared chlorinated polyester fibers are shown in Table 1 together.

[Comparative Example 5]

Polyethylene terephthalate was prepared in the same composition as in Comparative Example 4, followed by spinning in a conventional manner at a spinning speed of 1200 m / min, to prepare a dyestuff polyester yarn, and to evaluate the physical properties and dyeing characteristics of the prepared dyestuff polyester fiber. It is shown together in Table 1 below.

TABLE 1

(1) mol% represents terephthalic acid.

(2) Disperse dyes (normally dyestuffs for polyester fiber and preparation conditions) Adsorption amount: temperature rising to 10 ℃ / min, leveling for 30 minutes after reaching temperature

Claims (2)

Terephthalic acid was used as a diacid component, ethylene glycol was used as a diol component, and as a second diol component, a compound of the following general formula (I) or (II) was added to prepare a slurry, which was then synthesized by a conventional method. After the spin-draw method, a method for producing a dye-resistant polyester fiber characterized in that the ultra-fast spinning at a spinning speed of 5000 to 6500m / min. (Where R is one of methyl, ethyl, normal propyl, isopropyl, normal butyl or isobutyl groups) The method for producing a dibasic polyester fiber according to claim 1, wherein the compound of the general formula (I) or (II) is added in an amount of 8 to 15 mol% based on terephthalic acid.