KR880001300B1 - Polyester fibers making method - Google Patents

Abstract

Compound (I, A=C1-10 linear or branched aliphatic hydrocarbon; R=C2-4 hydrocarbon; n=1-5) 3.0-15.0 wt.% was copolymerized with terephthalic acid and ethylene glycol on the basis of conventional batch amount to give the title fiber. Thus, terephthalic acid 4300 g, ethylene glycol 1630g, antimon oxide 2.0g and 1,3-bis ( -hydroethoxy)-2,3- dimethyl propane 400g were reacted for 4 hrs for the esterification and TiO2 1.93g added then the oligomer was more reacted for 3hr AT 288≰C under 0.8 Torr to give copolyester, which was crystallized and drawn to give high shrinkable fiber.

Description

Manufacturing method of high shrink polyester fiber

The present invention relates to a method for producing a high shrink polyester fiber. Specifically, in the present invention, when terephthalic acid and ethylene glycol are reacted to prepare polyethylene terephthalate, a third resin is added to prepare a polyester resin capable of expressing high shrinkage. A method of making polyester fibers.

Conventionally, a method for producing a highly shrinkable polyester fiber is a method of imparting high shrinkage by changing the conditions for spinning in the spinning or stretching step and a method of copolymerizing a third compound as in the present invention (US Patent 3927167, Japanese Patent Laid-Open No. 78-). 134946), but in the case of the method of changing the conditions of the spinning in the spinning or stretching step, that is, the unstretched yarn is drawn at a low hot plate temperature or hot water (Japanese Patent Publication 81-27608), Changing method (Japanese Patent Laid-Open No. 81-140114) and supplying an aqueous solution of an organic solvent to the yarn during the stretching step (Korean Patent No. 85-1235), or stretching in hot water after reforming the polymer (US Patent 3549597) and the like. Due to the cumbersome condition change in the spinning or stretching process, and the attachment facility being cumbersome, there were problems in process control and manufacturing cost. In the conventional method of copolymerizing the third compound, US Patent No. 3927167 is referred to as Crystallization Retaradants.

However, when copolymerized using the above compounds, it causes complexity of equipment, such as the need to install a steam draw jet system between a feed and a draw roller. Rather, the compound added in Japanese Patent Application Laid-Open No. 78-134946 causes excessive shrinkage in post-processing processes such as sizing due to a decrease in secondary transition point (Tg) due to an increase in weight% due to high molecular weight (67 ° C). In order to obtain the required shrinkage rate, there was a problem in that the heater plate temperature was lowered.

In the present invention, the present invention has been reached as a result of intensive studies to solve the problems of the prior art and to prepare a high shrinkable polyester yarn having excellent physical properties.

Specifically, the present invention specifically describes a polyester resin having high shrinkage by spinning and stretching a polyester resin having shrinkage by adding co-polymerizing the compound of formula (1) in an esterification reaction or a condensation polymerization step. Will be obtained.

HO- (RO) _n -A- (OR) _n -OH (1)

Wherein A is a straight or branched aliphatic hydrocarbon of 1 to 10 carbon atoms, R is a hydrocarbon of 2 to 4 carbon atoms, n is a constant of 1 to 5 carbon atoms

In the present invention, the compound of formula (1) acts as a crystallization retardant in the copolyester, and the polyester fiber obtained by melt spinning and stretching such a copolyester resin has very high shrinkage and excellent physical properties. The addition amount of the compound represented by the general formula (1) is usually 3.0 to 15.0% by weight of the batch amount, more preferably 4.0 to 12.0% by weight. If the added amount is less than 3.0% by weight, the desired shrinkage cannot be obtained. If the amount is more than 15.0% by weight, the melting point of the chip and the strength of the yarn are lowered. You can get it. In addition, an anti-inflammatory agent (Tio ₂ ), a polycondensation reaction catalyst (antimony oxide), a heat stabilizer, or the like may be added when preparing the polyester according to the present invention.

The ester reaction of the present invention is carried out at 230 to 260 ° C. and 1.2 to 2.0 atm for 3 to 4 hours, that is, when the ester reaction rate reaches 93 to 98%, about 50 to 60% of the oligomer is transferred to the polycondensation reaction tank to achieve 260 to After the polycondensation reaction is carried out for 2.5 to 4 hours while maintaining the temperature of 290 ° C. and the final vacuum at 0.5 to 2.0 Torr, the polymer is chipped to prepare a highly shrinkable polyester resin. The prepared polyester resin is crystallized at a temperature of 120 to 160 ° C. under a nitrogen stream, and then dried at 170 to 180 ° C. for 10 to 12 hours to pass an injection machine at 250 to 290 ° C., and 800 to 1200 <m in a conventional spinning block. Melt spin at a winding speed of> / min. In this way, the melt-stretched unstretched yarn is thermally stretched at a feed ratio of 75 ± 2 ° C. and a hot plate of 120 to 130 ° C. at a draw ratio of 2.5 to 4.0 times, thereby producing a highly shrinkable polyester fiber. The physical properties (IV, terminal group) and color of the polyester resin thus prepared were very good, and the shrinkage and physical properties of the polyester yarn were also very good.

The present invention will be described in more detail with reference to the following Examples.

Example 1

A slurry was prepared by adding 400 g of 1,3-bis (beta-hydroethoxy) -2 and 2-dimethylpropane to a mixture of 4300 g of terephthalic acid, 1630 g of ethylene glycol, and 2.0 g of antimony oxide in a small polymerization reactor equipped with a stirrer, a condenser, and a distillation tube. After the reaction, the reaction is carried out for 4 hours while being uniformly added to the ester and the reaction tank. At this time, the additionally produced water was flowed out of the system to promote the esterification reaction.After the completion of the esterification reaction, titanium dioxide 1.93g was added as a quencher, and the oligomer was transferred to a condensation polymerization tank. After the addition, the temperature was raised to 288 ° C and the final vacuum was 0.8 Torr (Torr) for 3 hours. The copolyester resin thus prepared was crystallized at 120 to 160 ° C., dried at 180 ° C. for 12 hours, and spun at a speed of 1000 m / min at a spinning block at 290 ° C., followed by stretching (extension ratio 3.0).

Example 2

Slurry was added to a mixture of 4300 g of terephthalic acid, 1630 g of ethylene glycol and 2.0 g of antimony oxide in the same small polymerization unit as in Example 1 by adding 470 g of 1, 5-bis (beta-hydroethoxy) -3 and 3-dimetalpentane. Thereafter, in the same manner as in Example 1, esterification and condensation polymerization were carried out to chip, spin, and stretch.

Comparative Example 1

4300 g of terephthalic acid, 1690 g of ethylene glycol, and 1.86 g of antimony oxide were mixed and slurried in the same small polymerizer as in Example 1, and then subjected to esterification condensation polymerization in the same manner as in Example 1 for chipping, spinning, and stretching.

Comparative Example 2

In the same small polymerization apparatus as in Example 1, 4300 g of terephthalic acid, 1630 g of ethylene glycol, 2.0 g of antimony oxide, and 400 g of isophthalic acid were mixed and slurried, followed by esterification and condensation polymerization in the same manner as in Example 1, and then chipped and spun. , Stretched.

TABLE 1

Claims (1)

In preparing polyester fiber by reacting terephthalic acid with ethylene glycol, a method for producing a highly shrinkable polyester fiber characterized in that the compound of the following general formula (1) is usually added in an amount of 3.0 to 15.0 wt% based on the batch amount. HO- (RO) _n -A- (OR) _n -OH (1) Wherein A is a straight or branched aliphatic hydrocarbon having 1 to 10 carbon atoms, R is a hydrocarbon having 2 to 4 carbon atoms, n is a constant of 1 to 5 carbon atoms.