KR19980046795A - Manufacturing method of polyester yarn - Google Patents

Abstract

According to the present invention, carbon black is reacted by adding oxidized carbon black having a surface oxygen content of 2% or more surface treated with nitric acid so as to be 0.05% to 10.0% by weight relative to the polyester polymer. It is to prepare a polyester primary yarn having excellent dispersibility and spinning workability and having a dark black color after spinning.

Description

Manufacturing method of polyester yarn

The present invention relates to a method for preparing polyester yarn, and more particularly, by adding oxidized carbon black surface-treated with nitric acid during the polymerization reaction or from the polymerization reaction to the fiber formation, the carbon black content is reacted. The present invention relates to a novel production method of polyester primary yarn having high spinning and stretching workability.

Polyester polymers obtained by adding carbon black at the time of polymerization or in the process from polymerization to fiber formation by the conventional method and fabrics produced therefrom have a reddish color compared to those after dyeing with black dyes and have insufficient dyeability. .

Moreover, due to coagulation of carbon black or poor dispersibility of carbon black during polymerization, coarse carbon black particles are undispersed in the polymer and coarse particles are formed, resulting in clogging of the filter and filament rupture during the spinning step. It does not have good spinning ability, the spinning pressure rises sharply during spinning, not only trimming occurs during stretching, but also it has low affinity with the polymer, so the strength and elongation are low even after the fiber is manufactured.

Japanese special offices 49-87 and 49-792 disclose the combined use of copper phthalocyanine green to remove red shade and prevent aggregation. Japanese special offices 35-835 and 35-78 Although combination use of copper phthalocyanine blue has been disclosed, the polyester fibers produced by these disclosed methods have not prevented visible red shades. As a solution to this, Japanese Patent Laid-Open Publication No. 60-45689 and U.S. Patent No. 3,992,218 disclose a dope dyeing method using a turbid concentrate, but the liquid colorant reduces the content of carbon black and thereby causes the carafe in polyester fibers. There was another drawback, such as a low black content.

Accordingly, the present invention has been made to overcome the above-mentioned disadvantages, and more preferably at the stage of the polymerization reaction or at the stage from the polymerization reaction to the fiber formation, more preferably the surface with nitric acid during the polyester ester reaction of terephthalate acid and ethylene glycol. The present invention provides a method for producing a good dispersibility of carbon black in a polymer, excellent spinning ability, and dark brown after spinning, by adding the treated oxidized carbon black to react.

In the present invention, the oxidized carbon black is oxidized to the carbon black surface with nitric acid, wherein oxygen on the carbon black can form various functional groups such as carboxyl, lactone, phenol, and quinone. This increases the adsorption amount of the polymer on the carbon black surface and increases the acidity of the carbon black by the steric hindrance effect of the adsorbed polymers, thereby changing the pH of the carbon black from 8.3 to 2.7.

In the present invention, the oxidized carbon black, which is characteristically added, preferably has a surface oxygen content of 2% or more and more preferably 3% or more. If the amount of surface oxygen is less than 2%, the formation of coarse particles is seriously caused due to the lack of adsorption on the surface of carbon black, and the carbon black causes coagulation among them, which causes a problem of significantly lowering object properties.

The amount of oxidized carbon black that is characteristically added in the present invention is preferably 0.05% to 10% by weight, more preferably 0.1% to 5.0% by weight based on the polyester polymer. If it is 0.05% by weight or less, the black effect after the production of the primary yarn is insufficient, and if it is 10% by weight or more, the radiation workability is remarkably deteriorated due to poor polymerization reaction and deterioration of physical properties due to excessive addition of carbon black.

In the present invention, the method of adding the oxidized carbon black surface treated with nitric acid may be any step of the transesterification step, the polymerization step and the spinning step, but most preferably the transesterification step. 5-20% by weight of carbon black, premixed and sand milled to form a fully dispersed slurry of carbon black, and the slurry is then oxidized with respect to the polyester polymer in a prepolymer having a conventional transesterification reaction. This black is added to 0.05 to 10% by weight to cause a polycondensation reaction.

Polyester raw yarn prepared according to the invention is excellent in the dispersion of the carbon black, the polyester polymerization process is well progressed and good spinning work is to provide a high-quality polyester raw yarn having a dark black.

Hereinafter, the present invention will be described in detail in Examples and Comparative Examples, but the scope of the present invention is not limited by the following Examples. The matters necessary before entering this example and a comparative example are as follows.

[Dispersibility of Particles in Polymer]

The polymer was measured 10 times at a magnification of 4,000 times using a transmission electron microscope (Transmission Eletronic Microscope). At this time, the dispersibility evaluation of the particles in the polymer was evaluated by the number of particles having an average particle size of 10㎛ or more.

[Extreme Viscosity Measurement]

The polymer was dissolved in a 3: 2 mixed solution of phenol: 1,1,2,2-tetrachloroethane and measured at 250 ° C.

[Examples 1-3]

Use carbon black surface treated with nitric acid so that the surface oxygen concentration becomes 2.0%, 3.0%, and 4.0%, respectively, add 90% by weight of ethylene glycol to 10% by weight of oxidized carbon black, and then stir for 1 hour with a stirrer. Each premixed ethylene glycol slurry was prepared, followed by sand milling each premixed ethylene glycol slurry for at least 5 hours to prepare a slurry in which carbon black fine particles were uniformly dispersed in ethylene glycol. Separately, 100% by weight of terephthalate acid and 180% by weight of ethylene glycol and 0.040% by weight of antimony trioxide were subjected to transesterification and removal of the theoretical amount of water, followed by addition of a carbon black dispersion slurry surface-treated with nitric acid. It was set as 1,2,3. The resulting polymer was polycondensed at 270 ° C. for 30 minutes at atmospheric pressure, for 15 minutes under reduced pressure of 30 mmHg and for 150 minutes under high vacuum, and then the resulting polymer was pelletized by a general method.

After drying in the usual manner, the spinning speed was set to 186d / 36f undrawn yarn at 2,000 / min, and then drawn to 2.5d / 36f at a draw ratio of 2.5.

The physical properties of the undrawn and drawn yarns were measured and shown in Tables 1-1 and 2.

[Comparative Examples 1 and 2]

The same procedure as in Example 1 was carried out, except that the surface oxygen content of the oxidized carbon black was 0.6% in Comparative Example 1 and 1.2% in Comparative Example 2, and the overall physical properties of the undrawn and drawn yarns were evaluated. 1,2 is shown.

[Table 1-1] General Properties of Undrawn Artists

[Table 1-2] General Properties of Drawing Agents

As can be seen from the above examples and comparative examples, the oxidized carbon black surface-treated with nitric acid of the present invention is added and reacted to exhibit excellent dispersibility and radioworkability of the carbon black.

Claims (3)

Polyethylene, characterized in that the polycarbonate is prepared by adding and dispersing oxidized carbon black surface treated with nitric acid to ethylene glycol to make an ethylene glycol slurry, followed by transesterification, followed by polycondensation, followed by spinning and stretching. Manufacturing method of ester original yarn. The method of claim 1, The oxidized carbon black surface treated with nitric acid has a surface oxygen content of 2% or more. The method according to claim 1 or 2, The oxidized carbon black surface-treated with nitric acid is added to 0.05% to 10.0% by weight based on the polyester polymer.