KR0178052B1 - Process for preparing antistatic polyester fibre - Google Patents

Abstract

The present invention provides a method for producing an antistatic polyester fiber, wherein in polymerizing polyester, a single-ended blocked polyoxyalkylene amine compound of the following general formula (1) and a metal salt of the following general formula (2) It is polymerized by addition of an alkyl sulfonate compound containing a silicon dioxide with an average diameter of 50 to 500 µm and has an effect of excellent antistatic property and deep colorability.

(Wherein R ₁ : hydrogen or a hydrocarbon group, R ₂ : an alkylene group, n: an integer of 20 to 40)

(Wherein R ₃ : alkyl group, M: Na, K, Li, Mg)

Description

Manufacturing method of antistatic polyester fiber

The present invention relates to a method for producing a polyester fiber having excellent antistatic properties and excellent deep colorability.

Polyester fiber is widely used due to its excellent properties, but has high electrical resistance and high static electricity, which adversely affects workability during spinning and processing, and has a problem of discomfort to the user even when using the final product.

Conventionally, a method of copolymerizing and spinning polyethylene glycol has been proposed as a method for solving this problem, but in order to impart practical antistatic properties, a large amount of polyethylene glycol components should be copolymerized, and as a result, thermal stability and light resistance are degraded. Had a problem. In addition, a method of adding an antistatic agent composed of various polyalkylene glycol derivatives to the 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 an antistatic agent using a block copolymer of polyalkylene glycol copolymerized with polyalkylene glycol and a polyamide modified with a carboxyl group and an amine group and block polyalkylene etheramide block-polymerized as an antistatic agent It was introduced in Announcements 44-16178, 46-7213. Further, Japanese Patent Publication Nos. 48-30380, 50-107206, which use a block polyalkylene etheramide and a block polyalkylene ether ester in powder, are used in combination with an organic electrolyte. So 45-17547 was introduced. The methods listed above require a separate process and equipment for obtaining the polyalkylene ether block copolymer polymer, and have a disadvantage in that pyrolysis occurs during general polyester melt polymerization and does not easily solidify after discharge. Recently, the most widely used method is a technique using an antistatic agent in which polyoxyalkylene glycol having a molecular weight of 10000 to 30000 is mixed with a metal sulfonic acid compound, and the light resistance is poor due to the ether group component of polyoxyalkylene glycol. I have a problem. In addition, there is a lack of expressing the deep color for the use of the lining paper of clothing products.

Accordingly, the present inventors have reached the method of the present invention for solving the above problems and introducing an ether group into a polyester polymer chain which is easy to apply to a general process of polyester.

This invention relates to the manufacturing method of the polyester fiber excellent in antistatic property characterized by using the polyester superposed | polymerized by adding the single terminal blockade polyoxyalkylene amine compound of following General formula (1).

(Wherein R ₁ : hydrogen or a hydrocarbon group, R ₂ : an alkylene group, n: an integer of 20 to 40)

The present inventors have found that by using the single-ended blocked polyoxyalkylene amine compound, the vacuum line clogging phenomenon in the polycondensation reaction can be considerably alleviated. The preferred dosage is 0.5 to 7% by weight based on polyester. Preferably it is 2 to 5 weight%. In the present invention, when the compound of the general formula (1) n is less than 20, there is a weakness of the antistatic performance after washing, and thus, a considerable amount of the antistatic effect may be obtained to obtain a satisfactory antistatic effect. Deterioration occurs and is not good. In addition, when n is 40 or more, the compatibility between the polyoxyalkylene amine compound and the polyester is lost, and homogeneous mixing is not performed during the reaction.

However, the present inventors have found that when the polyester polymerization reaction is carried out using only the compound of the general formula (1), the polymerization reaction time becomes longer, resulting in a decrease in color and it is difficult to obtain a melt viscosity suitable for weaving.

Therefore, the present invention is characterized in that the alkylsulfonate compound containing the metal salt of the following general formula (2) and the silicon dioxide particles are combined with the compound of the general formula (1).

(In the above R ₃ : Alkyl group, M: Na, K, Li, Mg)

By using the compound of the general formula (2) in parallel, there is also an effect of assisting the formation of an amorphous portion of the fibrous polymer chain together with solving the above problems. Representative examples of the compound of the general formula (2) include sodium stearyl sulfonate, sodium dodecyl sulfonate, sodium octyl sulfonate, sodium dodecylbenzene sulfonate, and dodecyl sulfonate magnesium. In the present invention, the compound of formula (2) is characterized by using 10 to 50% by weight relative to the compound of formula (1). If it is 10% by weight or less, it is difficult to obtain the above effects of the present invention, and if it is 50% by weight or more, it causes a decrease in relative intrinsic viscosity due to an abnormal increase in melt viscosity. In the present invention, in order to obtain deep colorability, 0.3 to 5% by weight of silicon dioxide particles having an average diameter of 50 to 500 µm containing water or ethylene glycol as a dispersion medium are added to the total polyester. If the average diameter of silicon dioxide is 10 µm or less, it is difficult to substantially disperse in the polymer, so that high-quality yarns are difficult to obtain.

In addition, when the content of silicon dioxide is 0.3% by weight or less, it is difficult to obtain a satisfactory deep color due to insufficient roughening structure generated during the hydrolysis process. In addition, by adding silicon dioxide, the surface area is increased due to the surface irregularities generated after the post-decomposition process, thereby making it easy to discharge the stored charge. The polyester polymer obtained in the above polymerization process is radially stretched by a conventional melt spinning method to obtain an antistatic polyester yarn. The antistatic polyester yarn of the present invention has no effect on the process and has an excellent antistatic property and excellent color depth.

An example is given and described below.

EXAMPLE

How to measure

(ηrel) is the ratio of the viscosity of the diluted polyester solution in the solvent (3: 2 mixture of phenol and tetrachloroethane) and the solvent viscosity measured at 25 ° C., and C represents the concentration of polyester in the solvent.

(2) Diethyl glycol (DEG): Pyrolyse the polyester with hydrazine hydrate and measure this by gas chromatography.

(3) Electrical resistivity: Measured by using an electrical resistance measuring instrument of TOA of Japan in a constant temperature and humidity room.

(4) Friction band voltage: Measured using a Kanebo friction belt voltage meter.

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 tank. To this oligomer was added 5 g of antimony trioxide and 300 g of a compound having the formula R ₁ : CH ₃ , R ₂ : CH ₂ CH ₂ , n = 40 in formula (1) and R ₃ : C ₁₂ H ₂₅ , M: in formula (2). 100 g of sodium dodecyl sulfonate and 200 g of silicon dioxide having an average diameter of 70 µm were added thereto, and the polyester was reacted at 280 ° C. while reducing the pressure from 760 mmHg to 1 mmHg in 1 hour. The obtained polymer was dried by a conventional method, and spun at a rate of 1000 m / min at 295 ° C. using a mold having a normal circular spherical hole of 36. The obtained non-drawn yarn was stretched at a drawing speed of 1070 m / min by a heating roller maintained at 80 ° C. and a hot plate maintained at 120 ° C. to prepare a drawn yarn of 75 d / 36f.

[Examples 2 to 4 and Comparative Examples 1 to 3]

Polymerization and sacrifice were carried out in the same manner as in Example 1, except that the compounds in Table-1 were used.

Polymers and yarns produced by the above method are summarized in Table 2 below.

Claims (1)

In polymerizing polyester, 0.5-7 weight% of single-ended block | blocked polyoxyalkylene amine compounds of following General formula (1) with respect to a polyester component, and the compound of following General formula (2) with respect to the compound of General formula (1) 10 to 50% by weight of an alkylsulfonate compound containing a metal salt and a silicon dioxide having an average diameter of 50 to 500 µm are added to 0.3 to 5% by weight based on the total polyester to produce an antistatic polyester fiber . (Wherein R ₁ : hydrogen or a hydrocarbon group, R ₂ : an alkylene group, n: an integer of 20 to 40) (Wherein R ₃ : alkyl group, M: Na, K, Li, Mg)