KR940004693B1 - Method of preparing polyester fiber having an excellent dipersibility of particles and antibacterial ability - Google Patents

Abstract

mixing and dispersing the liquid-type polyester-based dispersing agent, which is the condensation polymerization product of the aliphatic or aromatic dicarboxylic acid and 2 valence alcohol and whose molecular weight is 200-5,000, with the antibacterial agent which is multiporous inorganic particles made of silica and alumina and the surface of which is exchanged by cuprous or silver ion, with the dispersant's amount of 0.5-5 times the antibacterial agent to make an antibacterial mixture; adding the mixture during the fiber spinning process in a way that the antibacterial agent adheres to the final fiber product by weight of 0.3-5 wt.%.

Description

Manufacturing method of polyester fiber excellent in particle dispersibility and antibacterial property

The present invention relates to a method for producing a polyester fiber having excellent particle dispersibility and antimicrobial properties by adding an antimicrobial agent of inorganic particles to the fiber, and more specifically, a liquid that is a condensation product of an aliphatic or aromatic dicarboxylic acid and a dihydric alcohol. The surface of the polyester dispersant is substituted with metal ions and mixed and dispersed 0.5-5 times in weight ratio with respect to the inorganic antimicrobial agent composed of silica and alumina. It relates to a method for producing a polyester fiber excellent in particle dispersibility and antimicrobial prepared by injection.

When polyester fiber is used as sportswear, socks, etc., microorganisms multiply and cause odor and harmful diseases.

In order to solve the above problems, many attempts have been made to impart antimicrobial function to fibers. For example, Japanese Patent Application Laid-Open No. 1-42288 discloses a method of preparing a slurry by adding an antimicrobial additive to the reaction monomer in a polymerization process. Although this method has a disadvantage in that the additives aggregate or react with the catalyst during the polymerization reaction, the antimicrobial agent is distributed inside the fiber cross-section during the production of hemp and the antimicrobial properties are reduced.

In addition, Japanese Patent Application Laid-Open No. 54-38951 is made of ion-exchangeable polyester fibers and treated with aqueous solutions such as copper and silver salts to give them antimicrobial properties. The problem is that it gets worse.

Accordingly, an object of the present invention is to produce an antimicrobial polyester fiber in the spinning process by mixing a dispersant and an antimicrobial agent in the spinning process to uniformly disperse the antimicrobial agent on the fiber surface to improve the workability in the fiber manufacturing process, antibacterial It is to provide a method for producing this excellent polyester fiber.

In order to achieve the above object, in the present invention, the antimicrobial agent of inorganic particles is first mixed and dispersed in a liquid polyester type dispersant, and then the mixture is spun by adding a predetermined amount to the molten polyester resin during spinning to disperse the antimicrobial inorganic particles. Due to the difference in viscosity between the melt polyester and the dispersant mixture containing the antimicrobial agent, it was possible to prepare a polyester fiber excellent in the antimicrobial property, the antimicrobial agent is mostly present on the fiber surface.

The present invention is described in detail as follows.

In the present invention, in the preparation of the antimicrobial polyester fiber, the liquid polyester type dispersant is mixed 0.5 to 5 times by weight with respect to the antimicrobial agent and the first mixed dispersion and then the mixture is introduced into the melt extruder during the spinning process to the antimicrobial agent to the final fiber Is added so as to adhere 0.3 to 5wt% and stretched by a conventional method to prepare a polyester fiber. Various additives for improving dyeing properties, antistatic properties, etc. may be used in the production of the polyester fiber of the present invention.

The dispersing agent used in the present invention is a liquid polyester present in liquid form at room temperature, and aliphatic or aromatic dicarboxylic acid and ethylene such as adipic acid, sebacic acid, azelaic acid, glutamic acid, terephthalic acid, isophthalic acid, phthalic acid and phthalic anhydride, etc. A condensate with a dihydric alcohol such as glycol, propylene glycol, butylene glycol, etc., and a molecular weight of 200 to 5,000 is appropriate. At this time, when the molecular weight is less than 200 or larger than 5,000, the dispersibility is poor, and workability such as elongation and radioactivity is poor.

Since the liquid polyester type dispersant used in the present invention has a lower viscosity than ordinary polyester, when the fiber is formed through a spinneret, the antimicrobial agent may be uniformly distributed on the surface of the fiber to sufficiently exhibit antimicrobial activity.

In addition, when the amount of the dispersant is mixed at less than 0.5 times by weight relative to the antimicrobial agent, the antimicrobial agent is not sufficiently sprayed on the propellant, and when mixed with more than 5 times, the physical properties such as strength and elongation may be achieved. It is significantly lower than general fibers and does not have practicality.

Meanwhile, the anti-regulator used in the present invention is a porous inorganic particle composed of silica and alumina, in which metal ions such as copper ions and silver ions are substituted on the surface thereof, and 0.3 to 5 wt% of the final fiber is preferably used. If the wt% is less than the antimicrobial effect is not effective antimicrobial effect, when used in more than 5wt% the workability during the manufacturing process of the fiber is reduced and there is no economic advantage.

Another method for producing polyester fibers having excellent particle dispersibility and antimicrobial properties of the present invention is to apply a liquid dispersant to the surface of the chip in a homomixer and then mix the antimicrobial agent to make a master batch chip in the compounding process in the spinning process There is a method of adding a certain amount into the melt extruder. In addition, the fiber may be made of a cis-core structure or a side-by-side structure by a composite spinning technique, and it is preferable that the antimicrobial-containing part is located on the sheath portion or the side of the fiber cross section on the side.

[Antibacterial Test Method]

Test standard The antibacterial effect was tested with Staphylococcus aureus (standard AATCC No. 6538) by the AATCC-100 Test Method. After inoculating the agar medium with the cultured bacteria at 37 ° C for 24 hours, inoculating the test specimen, adding a certain amount of liquid to extract the bacteria from the test specimen, and then counting the number of bacteria remaining in the liquid containing the treated and untreated cells. It was determined by calculating the percentage reduction of bacteria due to the addition of inorganic particles, an antimicrobial agent.

If over 99%: Excellent

95 to 99%: Normal

Less than 95%: Bad

[Dispersibility Evaluation Method]

1) Dispersion: Add the inorganic particles of antimicrobial agent to liquid polyester by weight ratio, mix and disperse first at room temperature for 30 minutes, and then accurately measure the weight of chips with a certain amount of antimicrobial agent introduced into the melt extruder and then measure horizontally and vertically 18 The film was prepared by heat bonding on a hot plate of 280 ° C. to 300 ° C., placed between mm carbagrass, and counting 10 µm or more of agglomerated particles with a phase contrast microscope, and converting them into pieces / mg.

Level 1: 0-1.9

Level 2: 2 to 3.9

Level 3: 4 to 6.9

Level 4: More than 7.0

2) Pack pressure change: Add inorganic particles as antimicrobial agent to liquid polyester by weight ratio, mix and disperse first at room temperature for 30 minutes, and then dry chips with a certain amount of antimicrobial agent introduced into melt extruder, and then filter 1,000 mesh. The filter pressure (kg / cm <2>) after 2 hours on condition of 285 degreeC and discharge amount 7.05g / min was measured using the plasticoder apparatus. Here, when reaching 50 kg / cm <2> which is a limit measurement within 2 hours, the time until then was measured and compared.

The following examples and comparative examples further illustrate the present invention, but do not limit the scope of the present invention.

Example 1

5.0 g of adipic acid liquid polyester (ADK CIZER) with inorganic antimicrobial agent consisting of silica and alumina substituted with copper ions and silver ions in a stirrer (Korean Fine Ceramics, product name: CLEAN-P) (average particle diameter: 1.2μ) P-200, average molecular weight: 2,000) 5.0g of primary mixture is dispersed by using a stirrer and then mixed in a melt extruder using a screw feeder connected to the melt extruder for 995g of polyester, followed by spinning and stretching Was prepared to produce a stretched yarn of final 50d / 36f. The antimicrobial test and dispersibility evaluation are shown in Table 1.

Example 2

A phthalate liquid polyester (ADK CIZER PN-77, average molecular weight: 600) was used as a dispersant, and was carried out in the same manner as in Example 1, and the results are shown in Table 1.

Example 3

Except for using phthalate liquid polyester (ADK CIZER P-202, average molecular weight; 1,000) as a dispersant was carried out in the same manner as in Example 1 and the results are shown in Table 1.

Example 4

Adiphthalate liquid polyester (BAA-15, average molecular weight; 1,500) was used in the same manner as in Example 1 except that the dispersant was used in Table 1.

Example 5

Except that 20 g of adiphthalate liquid polyester (ADK CIZER P-200, average molecular weight; 2,000) was used as a dispersant, the same procedure as in Example 1 was carried out, and the results are shown in Table 1.

Comparative Example 1

Except that the addition amount of the dispersant was 1.0g, it was carried out in the same manner as in Example 1 and the results are shown in Table 1.

Comparative Example 2

Except having made the addition amount of a dispersing agent into 30g, it carried out similarly to Example 1, and shows the result in Table 1.

Comparative Example 3

Except that the addition amount of the dispersant was 1g, it was carried out in the same manner as in Example 4 and the results are shown in Table 1.

[Comparative Example 4]

Except that 5g of adipic acid liquid polyester (REOPLEX 430, average molecular weight: 6,000) as a dispersant was carried out in the same manner as in Example 1 and the results are shown in Table 1.

[Comparative Example 5]

Except not using a dispersing agent, it carried out similarly to Example 1, and shows the result in Table 1.

Comparative Example 6

Except that the amount of the antimicrobial agent was 1.0g, the amount of the dispersant was 1.0g, polyester 998g was carried out in the same manner as in Example 1 and the results are shown in Table 1.

TABLE 1

1) The amount of the dispersant added represents the weight ratio to the antimicrobial agent.

2) The amount of antimicrobial added indicates the amount of antimicrobial added to the final fiber.

3) Antibacterial: Excellent (○), Normal (▲), Poor (×)

Claims (5)

In the preparation of the antimicrobial polyester fiber, the liquid polyester type dispersant is mixed and dispersed 0.5 to 5 times in weight ratio with respect to the antimicrobial agent, and the mixture is added during spinning, but the anti-regulator adheres 0.3 to 5 wt% to the final fiber. Method for producing a polyester fiber excellent in particle dispersibility and antibacterial, characterized in that it is added. The method for producing a polyester fiber having excellent particle dispersibility and antimicrobial properties according to claim 1, wherein the liquid polyester type dispersant is a condensation product of an aliphatic or aromatic dicarboxylic acid and a dihydric alcohol, and has a molecular weight of 200 to 5,000. The method of claim 2, wherein the aliphatic or aromatic dicarboxylic acid is adipic acid, sebacic acid, azelaic acid, glutamic acid, terephthalic acid, isophthalic acid, phthalic acid, phthalic anhydride production of polyester fibers having excellent particle dispersibility and antibacterial properties Way. The method for producing a polyester fiber having excellent particle dispersibility and antimicrobial properties according to claim 2, wherein the dihydric alcohol is ethylene glycol, propylene glycol or butylene glycol. The method of claim 1, wherein the antimicrobial agent is porous inorganic particles composed of silica and alumina, and copper ions or silver ions are substituted on the surface thereof.