KR940007689B1 - Process for preparation of polyester fiber - Google Patents

Abstract

This relates to a manufacturing method of polyester fiber which has better dyeing and drape properties and enhanced touch feeling. In the manufacturing polyester by ethylene glycol and dimethylterephthalate, the compd. of formula (I) 1-5 wt.% and dimethylisophthalic acid 5.8 wt.% are added in the early reaction. The above dimethylisophthalic acid has a role to enhance the noncrystalline zone of polyester molecula and to enhance the touch feeling.

Description

Method for producing polyester fiber

The present invention gives a micro crater after reducing the alkali on the surface of the fiber to give excellent dyeing and drape compared to the general polyester fiber, and at the same time to change the molecular structure of the polymer yarns generated after salt processing The present invention relates to a method for producing a polyester fiber by using a shrinkage property to improve the feel of the fiber. More specifically, the present invention relates to a method of preparing a polyester resin by reacting ethylene glycol and dimethyl terephthalic acid to prepare a polyester resin, and drying, melting, spinning, and stretching the same. In preparing the polyester fiber, 1 to 5% by weight of the compound of the following general formula (I) is added based on the amount of chips and 5 to 8% by weight of the dimethyl isophthalic acid on the basis of the amount of chips. It relates to a method for producing a polyester fiber characterized in that the reaction by addition.

Wherein R ¹ is a monovalent organic group, Y is a hydroxyl group, M is an alkaline earth metal such as manganese, zinc, cobalt, nickel, n ₁ is an integer of 0 or 1, and R ² and R ³ are carbon atoms 1 It is a compound containing the aliphatic hydrocarbon of -8, n <_2> is an integer of 1 or 2.

Polyester fibers have various uses, but the crystal regions in the molecular structure have reduced dyeing properties, which makes it difficult to produce high value-added products requiring deep color, silk-like, and drape. As a method of improving the disadvantages of such polyester fibers, Korean Patent Publication Nos. 88-12803 and 88-7833, Japanese Patent Laid-Open Nos. 59-21720, 60-59171, 61-152816, 61-160476, 61-258018, 62 As described in -152816 and the like, there are a method of imparting concavities and convexities to a yarn surface by a plasma treatment, an internal particle method of adding an additive to produce particles during a polymerization reaction, or an external particle method of adding an inorganic particle. However, the plasma treatment method has uniform unevenness ( Since it is difficult to form and expensive equipment is inevitable, there is a problem such as a rise in manufacturing cost.Inner particle method is difficult to control the amount and size of particles produced according to the process conditions during polymerization. This is large, the external particle method using the silica-based inorganic particles shorten the exchange cycle of the spin (PACK) due to the agglomeration of particles during the polymerization reaction, there is a disadvantage that the workability is poor because a lot of trimming occurs.

Accordingly, an object of the present invention is to provide a method for producing a polyester fiber, which provides excellent dyeing and drape properties as well as improved feel compared to polyester fibers.

In order to achieve the above object as well as another object that can be easily expressed in the present invention by adding a compound of the general formula (I) described above to give fine roughness on the surface of the fiber after alkali reduction to give dyeing and drape Dimethyl isophthalic acid was added to increase the amorphous region in the polyester molecule, giving shrinkage characteristics in the weaving and dyeing steps, thereby improving the feel.

The present invention is described in more detail as follows.

First, in preparing a polyester by reacting ethylene glycol and dimethyl terephthalic acid, the compound of the following general formula (I) is prepared before the polymerization reaction, and is charged in an amount of 1 to 5% by weight based on the chip amount at the beginning of the transesterification reaction, and polyester Dimethylisophthalic acid is added in 5 ~ 8% by weight based on chip amount to increase the amorphous region within the molecule and give shrinkage characteristics in the weaving and salt processing steps, and then the temperature of the reaction tube is changed to 240 ° C from the condensation polymerization tube. After the transfer, the mixture was decompressed and reacted at -760torr for 3 hours to prepare chips.

Wherein R ¹ is a monovalent organic group, Y is a hydroxyl group, M is an alkaline earth metal such as manganese, zinc, cobalt, nickel, n ₁ is an integer of 0 or 1, and R ² and R ³ are carbon atoms 1 It is a compound containing the aliphatic hydrocarbon of -8, n <_2> is an integer of 1 or 2.

In the above process, the transesterification reaction was controlled at 95-98%. The addition amount of the compound of the general formula (I) is preferably 1 to 5% by weight based on the chip amount, when the addition of less than 1% by weight does not exhibit the effect of addition, when it exceeds 5% by weight of the dye by aggregation of the particles The effect drops.

In addition, if the amount of dimethylisophthalic acid to be added is less than 5.0% by weight, there is a problem that the shrinkage characteristic does not appear after processing, and if it exceeds 8.0% by weight, a bridge occurs during drying due to an increase in the amorphous region in the polymer. There was a problem.

The chip prepared by the above-described method was dried and spun at 1300 to 3000 m / min, stretched at a range of 1.5 to 3.5 times at a stretching temperature of Tg + 50 ° C., and heat-set to 90 to 140 ° C. At this time, if the stretching temperature is outside the Tg + 50 ℃ range, there is a problem that the trimming and salt spots occur, if the heat setting temperature is out of the above range can not achieve the target shrinkage.

The following examples illustrate the invention in more detail, but do not limit the scope of the invention.

Example 1

Dimethylphthalic acid and ethylene glycol were added in a ratio of 1: 2, 5% by weight of dimethylisophthalic acid and 0.0045% by weight of antimony trioxide were added at the beginning of the transesterification reaction. When the temperature of the reaction tube was 160 ° C, R ₁ = -CH ₃ , Y = -OH, R ₂ = -CH _2- , , M = Mn, n ₁ and n ₂ is 1% by weight of the compound of the general formula (I) 1 is transferred to the condensation polymerization tube at 240 ℃, and the pressure of the condensation polymerization tube is gradually reduced to -7600torr state It is made to react to 285 degreeC for 3 hours.

The prepared chip was dried to a moisture content of 50 ppm or less using a hot air dryer, and then spun at 1500 m / min to prepare 30 denier / 12 filaments.

Process conditions and the object properties at this time are listed in Table 1.

Example 2

A yarn was prepared in the same manner as in Example 1, except that 7% by weight of dimethylisophthalic acid was used. Process conditions and properties are listed in Table 1.

Example 3

A yarn was prepared in the same manner as in Example 1, except that 1 wt% of the compound of Formula (I) was used. Process conditions and properties are listed in Table 1.

Comparative Example 1

A yarn was prepared in the same manner as in Example 1, except that 5 wt% of the compound of Formula (I) was used. Process conditions and properties are listed in Table 1.

Comparative Example 2

A yarn was prepared in the same manner as in Example 1, except that 9% by weight of dimethylisophthalic acid was used. Process conditions and properties were described.

Comparative Example 3

A yarn was prepared in the same manner as in Example 1, except that the compound of Formula (I) was added at the beginning of the polycondensation polymerization. Process conditions and properties are listed in Table 1.

TABLE 1

(Physical measurement method)

I. Intrinsic viscosity

According to ASTM-D1601 method, 2 g of chips were stirred and dissolved (120 ± 30 ° C) in 258 ml of OCP (O-chlorophenol) and measured with an Ostwalt viscometer.

II. Terminal group

According to JIS-K6715 method, the chip is dissolved in benzyl alcohol and measured with 0.04N NaOH.

III. D-EG

According to the CTS-203CP method, 1.5 g of a chip is dissolved in mono ethanol amine and measured by gas chromatography (manufactured by Shimadtu).

Ⅳ. Tg and Tm

DuPont's Model 990, Differential Scanning Analyzer

Ⅴ. Shrinkage

Measured by JIS-L1013 method.

(Evaluation standard)

Ⅵ. Depth

Measured with a colorimeter (made by DENSHOKU), the lower the L value, the better the dyeability.

Alkali weight loss was measured by 23% NaOH solution and dyed by high temperature and high pressure method.

Claims (2)

In preparing a polyester fiber by reacting ethylene glycol and dimethyl terephthalic acid, and drying, melting, spinning, and stretching the same, a compound of the following general formula (I) To 1 to 5% by weight based on the amount of the chip and dimethyl isophthalic acid 5 to 8% by weight based on the amount of the chip by the reaction method for producing a polyester fiber. Wherein R ¹ is a monovalent organic group, Y is a hydroxyl group, M is an alkaline earth metal such as manganese, zinc, cobalt, nickel, n ₁ is an integer of 0 or 1, and R ² and R ³ are carbon atoms 1 It is a compound containing the aliphatic hydrocarbon of -8, n <_2> is an integer of 1 or 2. The method for producing a polyester fiber according to claim 1, wherein the stretching temperature is Tg + 50 占 폚 and the draw ratio is 1.5-3.5 times to heat-set in the range of 90-140 占 폚.