KR0160475B1 - Process for preparing antistatic polyester fiber - Google Patents

Abstract

The present invention provides a method for producing an antistatic polyester fiber by a copolymerization method, by adding and copolymerizing a furan compound together with a polyoxyalkylene glycol compound and a non-reactive lithium sulfonate salt. It has the effect that ester fiber physical properties are maintained.

Description

Manufacturing Method of Electrostatic Wire Polyester Fiber

The present invention relates to an improved manufacturing method of polyester electrostatic yarn, which has excellent antistatic performance but does not lose the advantages of ordinary polyester fiber.

Polyester fiber is attracting much attention for clothing because it has excellent properties such as heat resistance, chemical resistance, elongation, crystallinity, and flexural strength, but in low temperature and low humidity areas, it is lining, lingerie, foundation, and other dust-free clothing in winter. In order to use it as a special functional clothing such as sportswear, there is a problem in that dust is easily adsorbed and contaminated by the generation of static electricity due to friction, and shock or discomfort to the wearer is caused. Many methods have been proposed to solve this electrostatic disturbance. For example, methacrylate or bisphenol is used for the polyoxyalkylene glycol, and there is a method of imparting an antistatic function by post-processing by plasma method, but this method has a disadvantage in that the antistatic property is sharply reduced after washing.

In order to solve this problem of washing resistance and to impart permanent antistatic properties, a method of modifying a polymer using polyalkylene glycol and sodium alkyl sulfonate introduced in Japanese Patent Laid-Open Nos. 52-47071 and 52-47072 is disclosed. This has been used a lot lately. Sodium alkyl sulfonate has the advantage of introducing an ionic group into the polymer to facilitate charge transfer and to express excellent antistatic performance by synergy with a copolymer of polyalkylene glycol. However, sodium alkylsulfonate is poor in dispersibility inside the polymer and causes a pack pressure increase during spinning. In addition, sodium metal salts may remain inside the spinning nozzles, resulting in poor spinning and shorter pack replacement cycles, resulting in poor spinnability and poor dispersibility in the polymers, which can lead to poor dyeing.

The present invention solves this problem and will be described in more detail as follows.

The present invention relates to a method for producing an antistatic polyester fiber characterized by using a polyester prepared by adding a furan compound together with a polyoxyalkylene glycol compound and a non-reactive alkylsulfonic acid lithium salt.

In the present invention, the polyoxyalkylene glycol compound is a compound of the following general formula (1) having a number average molecular weight of 2,000 to 3,000 and copolymerized at the terminal of the polyester main chain in an amount of 0.01 to 3.5% by weight relative to the total amount of polyester in the polycondensation period. .

If the input amount is 0.01% by weight or less, the antistatic property is extremely low, when the 3.5% by weight or more, the basic physical properties of the yarn is lowered.

(Herein, an alkyl group having R ₁ : C ₁ to C ₁₃ or H,

R ₂ : alkylene group having from C ₂ to C ₁₆ ,

n: integer from 20 to 150)

In the present invention, the non-reactive lithium sulfonate salt preferably uses non-reactive lithium polyalkyl sulfonate of the following general formula (2), the amount of which is 0.01 to 2% by weight relative to the total polyester.

(Herein, R ₃ : C ₃ ~ C ₂₆ Alkyl group or C ₇ ~ C ₃₀ An aryl group)

At this time, if the amount of lithium polyalkyl sulfonate is too high, the content of diethylene glycol (DEG) increases, so that when the polymer is discharged at the same melt viscosity, the intrinsic viscosity becomes high, and the elongation is too low in the object property. It is difficult to have a low viscosity. Therefore, preferable addition amount is 0.01-2 weight%.

The furan compound used together with the two compounds in the present invention is specifically 5-nitro-2-praldehyde diacetate (a), 5-nitro-2-praldehyde semicarbaron (b), 5-nitro-2pre Anacroline (c), 5-nitro-2-pranacrylic N- (5-nitro-2-propylidene) hydrazide (d), 5-nitro-2-proic acid, 5-nitro-2 -Praldehyde, and the like, and its content is preferably 0.001 to 1% by weight compared to polyester. If it is 0.001 weight% or less, antistatic property will fall, and if it is 1 weight% or more, it will cause a viscosity increase and a radiation failure.

The present invention can also increase the thermal stability by adding 200 ~ 400ppm Sb ₂ O ₃ as a catalyst during the polycondensation and adding 10 ~ 200ppm of the phosphorus compound as described below and reacting for 2 hours.

Wherein R ₄ to R ₆ : H or an alkyl group

In the present invention, the method of copolymerization is carried out by adding a mixed slurry of terephthalic acid and ethylene glycol to a polyethylene terephthalate oligomer polymerization tank and preparing an oligomer, and then adding the three-component compound of the present invention to the predetermined amount together with additives such as a catalyst. Since the polymerization is carried out according to the usual reaction conditions after the addition, the detailed description is omitted and replaced by the examples. Such polyester antistatic yarn according to the present invention is excellent in antistatic performance without compromising the inherent properties of the polyester fiber can be widely used in clothing and functional clothing.

EXAMPLE

How to measure

(1) Diethylene glycol (DEG) amount: Pyrolyse the polyester with hydrazine hydrate and measure this by gas chromatography.

(2) Resistivity: Measured in a constant temperature and humidity room using an electrical resistance meter manufactured by TOA Japan.

(3) Friction band voltage, half-life: Measured using a Kanebo friction belt voltage meter.

* The specific resistance, friction voltage, and half-life were measured at 20 ± 2 ℃ and 40 ± 2RH% humidity.

Example 1

While maintaining a polymerization tank containing 10 kg of polyethylene terephthalate oligomer at 260 ° C., a slurry in which 8645 g of terephthalic acid and 3875 g of ethylene glycol were well mixed was added over 6 hours to prepare 20 kg of oligomer, and then 10 kg was transferred to another polymerization furnace. 5 g of antimony trioxide, Compound C ₁₂ H ₂₅ O (C ₂ H ₄ O) ₄₀ H, and Compound C ₁₂ H ₂₅ SO ₃ Li 10 g, and 5-nitro- of general formula (2) were added to the oligomer. 5 g of 2-praldehyde diacetate (a) was added and then reacted at 280 ° C. to prepare a polyester of the present invention. After drying the obtained polymer in a conventional manner, the undrawn yarn obtained by spinning was drawn at a drawing speed of 1070 m / min by a heating roller maintained at 80 ° C. and a hot plate kept at 120 ° C. to prepare a drawn yarn of 75 d / 36f. .

EXAMPLES 2-6 AND COMPARATIVE EXAMPLES 1-3

The composition ratio of the copolymerization components is shown in Table-1, and Examples 2 to 3 and Comparative Example 1 used (a) as the furan compound, Example 4 is (b), Example 5 is (c), and Example 6 It carried out by the method similar to Example 1 except having used silver (d). In addition, Comparative Examples 2 and 3 were carried out in the same manner as in Example 1, changing the composition of only the compounds of the general formulas (1) and (2) without addition of the furan compound.

Claims (3)

After preparing a oligomer by adding a mixed slurry of terephthalic acid and ethylene glycol to a polymerization tank containing a polyethylene terephthalate oligomer, 5-nitro-2-praldehyde diacetate, together with a polyoxyalkylene glycol compound and a non-reactive alkylsulfonate lithium salt, 5-nitro-2-praldehyde semicarbaron, 5-nitro-2-pranacroline, 5-nitro-2-prannacrylic N- (5-nitro-2-propylidene) hydrazide, At least one furan compound selected from 5-nitro-2-proic acid and 5-nitro-2-praldehyde is added in an amount of 0.001 to 1% by weight based on the total amount of polyester to copolymerize polyester, and the copolymerized polyester is dried, followed by melt spinning. Method for producing an antistatic polyester fiber comprising the step of stretching. The method of claim 1, wherein the polyoxyalkylene glycol compound is a compound of the general formula (1) having a number average molecular weight of 2,000 to 3,000, antistatic properties, characterized in that added to 0.01 to 3.5% by weight relative to the total amount of polyester Method for producing polyester fiber. (Herein, an alkyl group having R ₁ : C ₁ to C ₁₃ or H, R ₂ : alkylene group having from C ₂ to C ₁₆ , n: integer from 20 to 150) The method of claim 1, wherein the non-reactive lithium lithium sulfonate salt is a non-reactive lithium polyalkyl sulfonate of the general formula (2), the addition amount of the antistatic polyester fiber, characterized in that 0.01 to 2% by weight relative to the total amount of polyester Manufacturing method. (Herein, an alkyl group of R ₃ : C ₃ ~ C ₂₆ or An aryl group C ₇ ~ C ₃₀₎