KR19990071438A - Polyester fiber having permanent antistatic property, preparation method thereof and brushed product using same - Google Patents

Abstract

The present invention relates to a polyester fiber that can exhibit a permanent antistatic property by adding to the polymerization raw material of the polyester fiber using a durable antistatic compound, and a method for producing the same and brushed products using the same, in more detail In the method for producing a polyester fiber, the step of ester-reacting terephthalic acid and ethylene glycol; Permanent charging prepared by dissolving sodium alkanesulfonate represented by the following formula (1) in ethylene glycol at 40 to 50 ℃, and adding the lysate to the reaction in a vacuum atmosphere of 265 to 290 ℃ It relates to a polyester fiber having a protective property, a method for producing the same and a brushed product using the same.

[Formula 1]

Where m is from 5 to 30.

Description

Polyester fiber having permanent antistatic property, preparation method thereof and brushed product using same

The present invention relates to a polyester fiber having a permanent antistatic property, a method for manufacturing the same, and a raised product using the same, more specifically, by using a durable antistatic compound added to the polymerization raw material of the polyester fiber permanently The present invention relates to a polyester fiber capable of exhibiting antistatic properties, a manufacturing method thereof, and a raised product using the same.

In general, polyester fiber is widely used due to its properties (strength, elongation, etc.) of synthetic fiber itself while maintaining the desirable properties of natural fiber, but due to the low electrical conductivity and hydrophobicity of synthetic fiber, The static electricity generated by the friction produced during the process of producing the ester product or the wearing of the polyester garment is not discharged and accumulates, and various types of electrostatic obstacles occur.

Therefore, in order to impart antistatic property to the polyester fiber, a compound having antistatic property must be added or copolymerized. However, when carbon black is used as a typical representative antistatic agent, there is a problem that only black products can be produced with excellent antistatic properties, and in order to impart hydrophilicity, copolymerization using polyethylene glycol as a hydrophilic compound is common. However, in order to impart hydrophilicity only with polyethylene glycol, the content of polyethylene glycol should be copolymerized at least about 5%, and as a result, the thermal stability and the light resistance of the polyester fiber are deteriorated.

In addition, a method of adding an antistatic agent composed of various polyalkylene glycol derivatives to polyester has been developed, but it has not been put to practical use due to problems in the dyeing process or loss of antistatic properties after washing. As another method, a technique using a block polyalkylene ether amide obtained by block copolymerization of a polyamide obtained by modifying a polyalkylene glycol copolymerized polyester with a polyalkylene glycol modified polyamide having a carboxyl group and an amine group is used as an antistatic agent. Nos. 44-16178 and 46-7213. Also, Japanese Patent Application Nos. 48-20380 and 50-107206 in which block polyalkylene ether amides and block polyalkylene ether esters are dispersed in polyester, and Japan special use together with block polyalkylene ether amides and organic electrolytes Sub 45-17547 was introduced. However, the methods mentioned in the above patents require a separate process and equipment for obtaining a polyalkylene ether block copolymer polymer, and a general polyester melt polymerization has a disadvantage in that pyrolysis occurs and does not easily solidify after discharge. In recent years, the most widely used method is a technique using an antistatic agent containing a polyalkylene glycol having a molecular weight of 10,000 to 30,000 and a metal sulfonic acid compound, which is a weight loss process by sodium hydroxide which is generally performed in the post-processing process of polyester fiber. There is a vulnerable problem. In addition, Korean Patent Publication No. 94-11540 discloses a method of polymerizing a polyester by adding a single-terminal blocked polyoxyalkylene amine compound represented by the following Formula a and a compound represented by the following Formula b as a copolymerization component. It discloses, but also has the disadvantage of not only deteriorating antistatic performance but also permanent.

[Formula a]

R ₁ O (R ₂ O) nNH ₂

Here, R <_1> is a hydrocarbon, R <_2> is an alkylene group, n is an integer of 20-40.

[Formula b]

Wherein R ₃ is one of H, CH ₃ , OH, CH ₂ CH ₂ OH, and M is K or Li.

In order to solve this problem, the present inventors have conducted extensive research, and have found a method of polymerizing a compound previously used as a post-treatment (temporary) antistatic agent to a polyester fiber, and the present invention was completed based on this finding. .

Accordingly, an object of the present invention is to reduce the troubles caused by the generation of static electricity during the production of polyester fibers (spinning, weaving, weaving and dyeing, etc.) by having a low cost and permanent antistatic ability, it is possible to improve the productivity and quality The present invention provides a polyester fiber having a permanent antistatic property and a method of manufacturing the same.

Another object of the present invention is to provide a brushed product prepared using the fiber.

In order to achieve the above object, the present invention provides a method for producing a polyester fiber, comprising the steps of ester-reacting terephthalic acid and ethylene glycol; Dissolving sodium alkane sulfonate represented by Formula 1 in ethylene glycol at 40 to 50 ° C., and polymerizing by adding the lysate to the reaction product under a vacuum atmosphere of 265 to 290 ° C. Is done.

Where m is from 5 to 30.

The brushed product of the present invention for achieving the above another object is subjected to a conventional knitting process, dyeing process, presetting process, brushing process, shearing process, drying process and tenter processing process using the fiber. Are manufactured.

Looking at the present invention in more detail as follows.

First, in the present invention, 1 mol of terephthalic acid and 2 to 3 mol of ethylene glycol are subjected to an initial ester reaction at 225 to 250 ° C. under pressure (2.5 to 5.0 kg / cm 2) in the presence of a catalyst, and the esterification rate is about 80 to 95%. Complete the reaction. After the esterification reaction, a pretreatment process for treating water or impurities is performed before proceeding with the polymerization reaction. First, the pressure is removed to remove the pressure from 2.5 to 5.0 kg / cm 2 or less at 0.5 kg / cm 2 or less, and then the pressure is increased while the pressure is reduced by an ejector. The end point of the pretreatment process is determined by the reaction temperature and reaction time. This reaction is a conventional process, and any known method may be used.

Then, when slowly approaching the atmospheric pressure while slowly releasing the vacuum of the reactor, sodium alkanesulfonate represented by the formula (1) dissolved in ethylene glycol at a concentration of 20 to 40% of 0.5 to 5% by weight of the final product (polymer) Nitrogen gas is added to the positive amount. After that, the mixture is mixed well so that the mixture with the polymer having a low viscosity. The addition point of the melt is very important in the present invention because the sodium alkanesulfonate represented by the formula (1) may be volatilized or aggregated during the polymerization reaction. In addition, when the solubility of sodium alkanesulfonate in ethylene glycol is less than 20%, the antistatic performance is lowered, and when it exceeds 40%, it is separated from ethylene glycol.

After the addition of the lysate is completed, the reactant is transferred to the next reactor by vacuum for polymerization. At this time, the temperature is raised (265 to 290 ° C.) while gradually applying the vacuum step to perform the reaction under high vacuum. The reaction is terminated when the target viscosity, eg, relative viscosity (IV), is about 0.630. The polyester polymer obtained in the above polymerization process is radially stretched by a conventional melt spinning method to obtain an antistatic polyester yarn.

Meanwhile, the present invention selects an antistatic agent represented by Chemical Formula 1 from various known antistatic agents for the purpose of preventing static electricity generated during the production of garments and industrial products of various synthetic fibers, and by dissolving and polymerizing them, its characteristics To maximize the performance.

Sodium alkanesulfonate represented by the formula (1) used as an antistatic agent in the present invention is used for the purpose of suppressing the generation of static electricity between fibers and fibers (F / F) and fibers and metals (F / M), the average carbon number A compound having a molecular weight of 12 to 17 and an average molecular weight of 240 to 350 is preferable in view of compatibility and antistatic effect with the polyester fiber structure, and the compound is used at 0.5 to 5% by weight based on the final product (polymer). At this time, when the added amount is less than 0.5% by weight, the physical properties (strength, elongation, etc.) of the fiber are excellent, but the function of the antistatic fiber cannot be exhibited due to the decrease in the antistatic performance, and when it exceeds 5% by weight, the antistatic performance is excellent. Care should be taken because problems such as trimming and laping can occur during spinning, and fiber breaks due to overuse.

On the other hand, it is possible to manufacture a brushed product of the polyester knit with a dyed processed product using a general polyester yarn. Also known as Polar fleece (Polar fleece), the polyester brushed fleece is a material that is used in a variety of sportswear, general clothing, various accessories, bedding as well as light and excellent thermal insulation. However, as mentioned above, this product generates a lot of static electricity, which is a disadvantage of synthetic fibers, and becomes a problem not only when wearing clothes but also when processing the fabric.

This problem is solved by manufacturing a polyester yarn having permanent antistatic property in the present invention. The brushed product manufactured by using the antistatic polyester yarn according to the present invention is manufactured through a knitting process → dyeing → presetting → brushing → shearing → tumbler drying → tenter processing → rolling process.

1. Knitting Process

First, the antistatic polyester yarn of the present invention is knitted with a circular knitting machine (10-200 feeder, 10-60 inch, 10-28 gauge) at a speed of 5-100 rpm.

2. Dyeing Process

The knitted fabric was added with disperse dyes and dispersants in a high temperature dyeing machine, the pH was adjusted to 4-5 with acetic acid, and then dyed at 100-135 ° C. for about 50 minutes, followed by addition of sodium hydrosulfite and NaOH. 10 minutes to 30 minutes at 60-90 ° C for reduced washing to increase the fastness, and two times water-washing to add the softening agent, followed by 5-20 minutes at 40-50 ° C. In this case, in the case of a fabric knitted with a general polyester yarn, in addition to the softener, an antistatic agent should be added together to prevent static electricity occurring in the final product. However, in the case of the fabric using the permanent antistatic polyester yarn of the present invention, it is not necessary to add the antistatic agent. Dehydrate after finishing softening.

3. Presetting process

The finished fabric is pre-set in a tenter at a speed of about 10 to 60 m / mim at 140 to 170 ° C.

4. Raising process

Using a brush, the brush is brushed 2-3 times on the loop side and 3-4 times on the other side. At this time, in the case of a fabric made of a general polyester yarn causes a fairly severe static electricity during the brushing process, the static electricity does not occur when using a permanent antistatic yarn.

5. Sharing process

A shaling process is performed to prevent tangles of the raised products and to even the surface of the fabric. Using a shearing machine, cut 0.1 to 1.0 cm apart.

6. Tumbler drying process

In the tumbler drying step, the fabric is treated at 80 to 140 ° C. for 5 to 60 minutes to suppress peeling, form a surface shape, and fix the surface.

7. Tenta processing process

After the drying process, the fabric is subjected to a tena processing, and the temperature is performed at a speed of 10 to 60 m / min at 160 to 210 ° C. to impart thermoplasticity to stabilize the form so as not to increase or decrease.

The antistatic polyester knitted brushed product thus prepared may manufacture military blankets, general blankets, bedding, sportswear, general clothing, accessories, or home interior accessories.

Hereinafter, the present invention will be described in more detail with reference to Examples and Comparative Examples, but the scope of the present invention is not limited to the following Examples.

Example 1

In the presence of SB ₂ O ₃ catalyst, 1 mole of terephthalic acid and 2 moles of ethylene glycol are subjected to an initial ester reaction at 210 ° C. and 4.0 kg / cm 2 to complete the reaction at about 90%. Then, the pressure is removed from the 4.0kg / ㎠ to 0.5kg / ㎠ or less, and when depressurization is completed, the pressure is reduced by the ejector while simultaneously heating the reactor and maintaining at about 240 ℃ for 4 hours to remove impurities in the reactor .

When the vacuum of the reactor is slowly released to normal pressure, sodium alkanesulfonate (an compound having an average carbon number of 15), an additive antistatic agent made of 31% ethylene glycol solution, is pushed into nitrogen gas at 1% by weight based on the polymer. . After that, the mixture is mixed well so that the mixture with the polymer having a low viscosity. After the addition is complete, the reaction product is transferred to the next reactor by vacuum, and then the reaction is completed at 280 ° C. under high vacuum. When the relative viscosity was 0.630, the reaction was terminated, cut into chips, transported, and then a spinning process was performed.

Example 2

Except for changing the addition amount of sodium alkanesulfonate to 2% by weight based on the polymer in Example 1 was carried out in the same manner as in Example 1.

Example 3

Except for changing the addition amount of sodium alkanesulfonate to 5% by weight based on the polymer in Example 1 was carried out in the same manner as in Example 1.

Examples 4-7

Except for changing the average carbon number of sodium alkanesulfonate in Example 1 to 5, 10, 20 and 30, respectively, it was carried out in the same manner as in Example 1.

Comparative Example 1

The same procedure as in Example 1 was conducted except that sodium alkanesulfonate was added together with various raw materials in Example 1.

Comparative Example 2

The same procedure as in Example 1 was conducted except that the antistatic agent for addition in Example 1 was not added.

Comparative Example 3

The addition was carried out in the same manner as in Example 1 except that the antistatic agent for addition in Example 1 was changed to a carbon block so that the addition amount was 1.2% by weight based on the polymer, and the conditions were added under the conditions during the spinning process. .

The mechanical properties of the fibers prepared by polymerization and spinning by the methods of Examples 1 and 2 and Comparative Examples 1 to 3 are shown in Table 1 below.

Item Thickness (denia) Strength (g / d) Elongation (%) Example 1 74.5 4.74 33.4 Example 2 74.5 4.73 33.4 Example 3 74.2 4.72 33.4 Example 4 74.1 4.70 33.3 Example 5 74.0 4.70 33.1 Example 6 74.0 4.70 33.0 Example 7 74.0 4.70 33.1 Comparative Example 1 74.0 4.70 33.2 Comparative Example 2 73.9 4.67 33.1 Comparative Example 3 73.8 4.65 33.1

<How to measure>

Strength and elongation: measured according to KS K 0409 (1985)

In addition, the friction band voltage (KS K 0555 B method) of the fibers prepared according to Example 1 and Comparative Example 2 was measured and the results are shown in Table 2 below.

division Example 1 Comparative Example 2 After washing three times 30volt 1460volt After 50 washes 60volt - 3 times after dry cleaning 40volt 1640volt After 50 dry cleans 70volt -

Note) Test conditions: 20 ℃, 65% RH, 450rpm, cotton cloth

Washing condition: KS K 0465, normal cycle, 40 ± 3 ℃, drying clothesline

Dry cleaning condition: KS K 0474

As can be seen from Tables 1 and 2, the polyester fiber yarns according to the present invention (Examples 1 and 2) have a significant difference in the frictional belt voltage values without deterioration in strength and elongation compared to conventional Comparative Examples 2 and 3. In addition to showing a permanent antistatic properties. Especially in the case of the comparative example 3, since the antistatic agent fell out and shows the same tendency as the comparative example 2, durability could not be expected.

On the other hand, in the case of Comparative Example 1 in which the addition time of the antistatic agent of the present invention is different than the conventional products (Comparative Examples 2 and 3), the friction voltage value is improved, but sodium alkanesulfonate tends to volatilize or aggregate during polymerization. There was a problem in the production process such as spinning, weaving, weaving, dyeing and processing. However, in the case of the present invention, no adverse effect was found on the production process.

Example 8

The antistatic polyester yarn prepared in Example 1 was knitted at a speed of 5 to 100 rpm with a circular knitting machine (10 to 200 feeder, 10 to 60 inch, 10 to 28 gauge). The knitted fabric was added with 10% by weight of disperse dye (LG, N / B S-2GL) and 0.3% by weight of dispersant (East South Synthetic, Revogen DC) in a high temperature dyeing machine, and adjusted to pH 4-5 with glacial acetic acid. Then, after dyeing at about 130 ℃ for about 50 minutes, 2 g / L sodium hydrosulfite and 1.0 g / L of NaOH was added to reduce washing at about 80 ℃ for about 20 minutes to improve the fastness, After washing with water twice, 3% by weight of a softening agent (Sino-Japanese emulsification, JD-402-1) was added and treated at 40 to 50 ° C. for about 15 minutes, followed by drying. Finished fabric is pre-set in a tenter at a speed of about 40m / mim at about 150 ℃. After brushing the loop side 3 times and the opposite side 4 times using a brush, cut about 0.5cm by using a shearing machine. The fabric is treated at about 100 ° C. for about 30 minutes to suppress peeling, form a surface, and adhere. After the drying process, the fabric was tenanted at a speed of about 40 m / min at about 180 ° C.

As a result of measuring the friction band voltage (KS K 0555 B method) of the military blanket prepared by the conventional method using the fabric thus prepared, it was almost the same as Table 2 above.

As described above, the present invention suppresses the static electricity generated during friction between polyester fiber, fiber (F / F) fiber and metal (F / M), so that the production of P / E textile industry (spinning, weaving, weaving) , Dyeing, etc.) It reduces the troubles caused by the generation of static electricity and improves productivity and quality, thereby eliminating static electricity at an affordable price.

Claims (7)

A method for producing a polyester fiber, comprising the steps of: ester-reacting terephthalic acid with ethylene glycol; Dissolving the sodium alkanesulfonate represented by the formula (1) in ethylene glycol at 40 to 50 ℃, and the step of polymerizing by adding the lysate to the reaction in a vacuum atmosphere of 265 to 290 ℃ Method for producing a polyester fiber having a permanent antistatic property. [Formula 1] Where m is from 5 to 30. The method of claim 1, wherein the sodium alkanesulfonate is dissolved in ethylene glycol at a concentration of 20 to 40% and added. The method according to claim 1, wherein the amount of sodium alkanesulfonate added is 0.5 to 5% by weight based on the final product. The method of claim 1, wherein the sodium alkanesulfonate has an average carbon number of 12 to 17 and an average molecular weight of 240 to 350. A permanently antistatic polyester fiber produced by the method of claim 1. Using the fiber according to claim 5 having a permanent antistatic properties prepared through the usual knitting process, dyeing process, presetting process, brushing process, shearing process, drying process and tenter processing process Raising products. The brushed product of claim 6, wherein the brushed product is military blankets, general blankets, bedding, sportswear, general clothing, accessories, or home interior accessories.