KR19980051333A - Manufacturing method of polytrimethylene terephthalate stretched yarn - Google Patents

Abstract

According to the present invention, in the method for producing a stretched yarn by spinning and stretching a polytrimethylene terephthalate resin, the 5-sodiosulfo dimethyl terephthalate is 0.5 to 2.0 as the polytrimethylene terephthalate resin as compared to terephthalic acid or an ester derivative thereof. Provided is a method for producing a polytrimethylene terephthalate stretched yarn using a copolymerized polytrimethylene terephthalate resin having a mol% copolymerized intrinsic viscosity of 0.55 to 0.75, followed by spinning at a flux of 2,000 m / min or less. . By applying this method, it is possible to stably produce a drawn yarn using a low molecular weight PTT resin.

Description

Manufacturing method of polytrimethylene terephthalate stretched yarn

The present invention relates to a method for producing a stretched yarn using polytrimethylene terephthalate resin.

Recently, a resin called polytrimethylene terephthalate has begun to be commercialized in polyester, and it is being developed for various fiber applications because it has excellent elasticity and dyeing property compared to conventional polyester.

However, in the production of PTT stretched yarn, when using a resin having a molecular weight of 0.8 or more intrinsic viscosity, spun unstretched yarn or POY yarn has good strength and heat resistance, so that a stretched yarn having excellent sand quality can be easily manufactured with stable processability. In this case, however, increasing the intrinsic viscosity leads to a longer reaction time, which is disadvantageous in terms of production cost. On the other hand, low molecular weight PTT resins with an intrinsic viscosity of 0.55 to 0.75 have advantages in terms of production cost, but due to the low molecular weight, the spinning process becomes worse as the flux is increased, so the flux should be lowered as much as possible. There is a problem that the stretching process is poor, and it is quite difficult to stably obtain the stretched yarn using a low molecular weight PTT resin.

Therefore, an object of the present invention is to provide a method for stably producing a drawn yarn using a low molecular weight PTT resin without the above problems.

In the study of the present inventors for achieving the above object, unburned obtained by spinning a 0.5-2.0 mol% copolymerized PTT resin of 5-sodiosulfo dimethyl terephthalate (hereinafter referred to as DMS) at a flux of 2,000 m / min or less The use of a gentleman not only made it possible to stably produce the stretched yarn, but also found that the crystallization rate and alkali reduction were improved.

Therefore, according to the present invention, DMS is stretched after spinning PTT resin having 0.55 to 0.75 intrinsic viscosity copolymerized with 0.5 to 2.0 mol% of terephthalic acid (TPA) or ester derivatives thereof at a rate of 2,000 m / min or less. A method for producing a methylene terephthalate stretched yarn is provided.

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

According to the present invention, DMS is 0.5 to terephthalic acid (TPA) or an ester derivative thereof.

When 2.0 mol% copolymerized intrinsic viscosity 0.55 to 0.75 PTT resin was spun at 2,000 m / min or less, the change in unstretched yarn significantly decreased over time, and the weight loss rate was increased to reduce the alkalinity, thereby improving the productivity of post-processing. do.

In the present invention, the PTT resin is preferably copolymerized DMS 0.5 to 2.0 mol% compared to terephthalic acid (TPA) or its ester derivative. In this way, copolymerization of DMS, in addition to the suppression of changes over time, the weight loss rate is faster, the production speed is faster when the process is cheap, there is an advantage in reducing the production cost. If the DMS content is less than 0.5 mol%, the desired effect can hardly be obtained. If the DMS content is more than 2.0 mol%, the cost is increased and the intrinsic viscosity cannot be raised, which adversely affects physical properties.

The PTT resin may change the melt viscosity or other physical properties by copolymerizing the following compounds with DMS, if desired, to 10 mol% or less than terephthalic acid (TPA) or ester derivatives thereof.

(A) isophthalic acid or its ester derivatives

(B) HO- (CH ₂ CH ₂ -O) _n -OH, where n is from 1 to ₂₀₀

(C) HOOC- (CH ₂ ) _m -COOH (where m is 1 to 30) or ester derivatives thereof It is preferable that the intrinsic viscosity of the PTT resin used is 0.55 to 0.75. If the molecular weight is less than 0.55, the physical properties of the spinning process and the final yarn are not good because the molecular weight is less than 0.55. The process or the physical properties are good when the molecular weight is over 0.75, but the reaction time for the production of PTT resin is long, and the raw material cost increases so much that the production cost is increased. There is a disadvantage that this greatly rises.

In this manufacturing method, it is preferable that the discharge | discharge discharge | release at the time of spinning shall be 2,000 m / min or less. The unstretched yarn manufactured at such a low discharge rate does not lose its stretchability when drawn within 5 days. This seems to be because the crystallization rate of the resin is accelerated by the DMS component and the physical properties obtained during and immediately after spinning hardly change thereafter. When the discharge speed exceeds 2,000 m / min, there is a disadvantage that a lot of trimming occurs during spinning while excessive tension is applied during spinning.

Features and other advantages of the present invention as described above will become more apparent from the embodiments described below. Of course, the following examples are only intended to aid understanding of the present invention and are not intended to be limiting. Unless specifically defined in the following Examples and Comparative Examples, parts represent parts by weight. Physical properties shown in the following Examples and Comparative Examples are measured by the following method.

◎ Intrinsic Viscosity (IV): After dissolving at 120% ortho-chlorophenol at 1% concentration, it was measured using a Ubelrod viscometer in a 30 ° C thermostat.

◎ Alkali weight loss rate: Two 75/36 filament yarns were spun and re-assembled in a reshaping machine, and then the weight loss rate was measured by weight change before and after immersion in 98T: 5% NaOH solution for 30 minutes.

Example 1

500 parts of dimethyl terephthalate (DMT), 9.2 parts of DMS (1.2 mol% compared to DMT), 330 parts of 1,3-propylene glycol (hereinafter referred to as 1,3-PG) in a reactor equipped with a stirrer and an outlet condenser, tetra 1 part of butyl titanate and 0.1 part of sodium acetate are added, and the temperature of the reactor is gradually raised to 220 ° C. At this time, the produced methanol is discharged to the outside of the system for transesterification. When the discharge of methane is completed, 1 part of trimethyl phosphate is added as a stabilizer and stirred for 10 minutes. Here, the internal temperature is raised from 220 ℃ to 260 ℃ and the pressure is gradually reduced to 0.1mmHg from normal pressure to remove 1,3-PG, reacting until the desired intrinsic viscosity is reached, ejected and cut into chips. .

The PTT resin chip thus prepared was dried at 150 ° C. for 6 hours in a vacuum dryer, and then spun using a conventional spinning machine to prepare 210De ′ 36 filament undrawn yarn. Spinning conditions were spinning temperature 260 ℃, spinning speed 1,20m / min, cooling wind temperature 25 ℃, nozzle size 0.3mm. The undrawn yarn thus prepared was stretched three times under the conditions of a hot roller temperature of 65 ° C., a hot plate temperature of 160 ° C., and a stretching speed of 400 m / min using a conventional drawing machine. The conditions and results of this example are summarized in Table 1.

EXAMPLE 2 AND COMPARATIVE EXAMPLES 1-13

The same procedure as in Example 1 was repeated except that the intrinsic viscosity, DMS content, and flux of the PTT resin were changed as shown in Table 1 below.

Example 3

The same procedure as in Example 1 was repeated except that 10 parts of dimethyl isophthalate was added to the reaction.

Example 4

The same procedure as in Example 1 was repeated except that 10 parts of diethylene glycol was added and reacted at the beginning of the reaction.

Example 5

The same procedure as in Example 1 was repeated except that 10 parts of adipic acid was added and reacted at the beginning of the reaction.

* DMS content: mol% compared to DMT

As can be seen from Table 1, according to the present invention it is possible to stably produce the drawn yarn using a low intrinsic viscosity PTT resin.

Claims (2)

In the method for producing a stretched yarn by radially stretching the polytrimethylene terephthalate resin, 5-sodiosulfo dimethyl terephthalate is copolymerized 0.5 to 2.0 mol% of terephthalic acid or its ester derivative as the polytrimethylene terephthalate resin A method for producing a polytrimethylene terephthalate stretched yarn comprising using a copolymerized polytrimethylene terephthalate resin having an intrinsic viscosity of 0.55 to 0.75 and spinning it at a speed of 2,000 m / min or less. The method according to claim 1, wherein the copolymerized polytrimethylene terephthalate resin is copolymerized with at least one or more of the following components together with 5-sodiosulfo dimethyl terephthalate component by 10 mol% or less relative to terephthalic acid or its ester derivatives. Method of polytrimethylene rephthalate drawn yarn (A) isophthalic acid or its ester derivatives (B) HO- (CH ₂ CH ₂ -O) _n -OH, where n is from 1 to ₂₀₀ (C) HOOC- (CH ₂ ) _m -COOH, where m is 1-30, or ester derivatives thereof