KR910003655B1 - Preparation of polyester fibers having excellent antibacterial and decorizing properties - Google Patents

Abstract

A antibacterial major compd., which is mainly 4th grade ammonium salt using organic silicone as a carrier, is formulated 0.05-5 wt.% as applicable amount per treated fiber. A durability-improving agent is composed of modified silicone compd., fatty acid salt surfactant, and is formulated 20-60 wt.% or 10-40 wt.% respectively per major compd. A cross linking agent is amino silane compd., and used 3-20 wt.% per major compd. The mixed solution of antibacterial compd and two assisting agents are diluted with water. Then the polyester fiber is impregnated or sprayed by the diluted solution and heated at 90-170 deg.C for 10-30 min. This process enables polyester fiber to be crosslinked or ion-bonded with antibacterial compd.

Description

Manufacturing method of polyester fiber excellent in antibacterial deodorization

The present invention provides a polyester which prevents embrittlement, staining and foul odor of fiber materials due to the propagation of microorganisms by giving antimicrobial deodorization property to the polyester fiber, in particular, among the most closely related synthetic fibers in our daily lives. It relates to a method for producing a fiber.

In general, polyester fibers are used for bedding (quilting, mattresses, cushions, etc.), interior products (wallpaper, carpets, curtains, etc.), clothing, household goods (socks, sportswear, cloths, etc.) as well as industrial materials (filtration filters, And various nonwoven fabrics).

On the other hand, there are various kinds of bacteria and fungi in our living environment, and they are attached to and inhabited in textile materials. Among them, they do not directly affect the human body, but they cause deterioration, embrittlement, staining and odor of textile materials. Some are pathogenic, which can directly harm the human body. Therefore, in order to solve the problems caused by such molds, antimicrobial and deodorizing processing have been the subject of much interest in the past, but unlike other processing, the processing results are invisible, so the value as a product cannot be greatly evaluated. As consumers' living standards improve and their desire to pursue a more pleasant life increases, the social environment changes, which emphasize the importance of public health, is now becoming a necessary processing tool rather than a temporary boom.

That is, the methods that have been examined when providing antimicrobial properties to polyester fibers so far include: 1) a method of imparting an antimicrobial compound at the time of polyester fiber polymerization, and 2) a method of imparting an antimicrobial compound at the time of spinning after polyester fiber polymerization, followed by mixed spinning. 3) The method of imparting an antimicrobial compound by post-processing after polyester fiber production, and the method of 1), 2) is difficult to manufacture because the antimicrobial compound is treated at the time of polymerization or spinning, color fading after production It is pointed out the disadvantages such as causing problems, and the method of 3) is generally easy to manufacture because it is easy to manufacture, but the durability of the antibacterial effect is poor due to the lack of durability of the laundry compared to the method of 1), 2). there was.

Antimicrobial compounds that have been used in the post-processing of textile materials so far include organic mercury compounds and organotin compounds, but recently, quaternary ammonium salts, which have been avoided due to toxic problems and high in human safety, have been attracting attention.

As an example, Japanese Patent Laid-Open No. 59-130371 proposes a method for producing a textile product using an organosilicon quaternary ammonium salt. The organosilicon quaternary ammonium salt is a cationic antimicrobial agent that combines ionic bonds with the surface of the minus-charged fiber, and especially in the case of cellulose fibers, the reactive silicone is the OH group of the fiber. It is well known that the antimicrobial effect is almost semi-permanent by covalently bonding with (base), but when organic silicon is difficult to bind, such as synthetic fibers, only a temporary antimicrobial effect is obtained.

The present invention ion-bonds the cationic antimicrobial agent to the surface of the negatively charged fibers via organic silicon to compensate for this drawback in the conventional manufacturing method and product properties, and at the same time crosslinking the modified silicone compound and fatty acid surfactant It is added to the antimicrobial agent is strongly combined with polyester fiber to provide a polyester fiber with significantly improved laundry durability, and the present invention for achieving the above object is an antimicrobial compound through the organic silicone as a medium A quaternary ammonium salt was used to adjust the adhesion amount to 0.05-5% by weight with respect to the fiber to be treated, and the modified silicone compound and the fatty acid surfactant represented by the following formula (I) were added to the antimicrobial compound adhesion amount as the durability improving aid. 20-60% by weight and 10-40% by weight based on the crosslinking agent The antimicrobial compound was prepared by using the amino silane compound represented by 3-20% by weight of the antimicrobial compound adhesion amount, and then diluting it with water to impregnate or spray the polyester fiber and then heat-treat the antimicrobial compound by ion bonding and It is characterized by crosslinking.

Where R ₁ , R _{2 and} R ₃ are CnH _{2n + 1} , n is an integer of 0-10 and x, y is an integer of 1-15.

Wherein R ₁ , R _2, R ₃ are CnH _{2n + 1} , and n is an integer of 0-10.

As the quaternary ammonium salt compound, alkyldimethyl ammonium chloride and alkylbenzyl ammonium chloride are used. Hexyl dimethyl ammonium chloride, octyl dimethyl ammonium chloride, decyl dimethyl ammonium chloride are used as the alkyl dimethyl ammonium chloride compound, and as the alkyl benzyl ammonium chloride compound, 2-chloro benzyl ammonium chloride, 4-chloro benzyl ammonium chloride, 2-4 -Dichloro benzyl ammonium chloride, 3,4-dichloro benzyl ammonium chloride, 4-nitro benzyl ammonium chloride is used, most preferably octadecyl dimethyl (3-trimethoxyl) propyl ammonium chloride.

The adhesion amount of the antimicrobial agent is 0.05 to 5% by weight with respect to the fiber to be treated. The antimicrobial property is poor at 0.05% or less and the antimicrobial property is not improved at 5% or more. Cause problems.

The silicone compound used as the durability improving aid is generally contained in an antimicrobial agent. For stronger bonding with polyester fiber, a modified active silicone compound and a fatty acid surfactant should be used in combination. In this case, the amount of the modified silicone compound is suitable for 20 to 60% by weight of the amount of antimicrobial agent in consideration of activity and reactivity, and less than 20% of the reactivity is not good to improve the durability, and the antimicrobial processing solution is stable at 60% or more. Inhibits. In addition, in the case of fatty acid surfactant, 10 to 40% by weight of the antimicrobial agent adhesion amount is suitable, if outside this range does not help to improve the durability. The crosslinking agent is an amino-based silane compound that promotes crosslinking of the silicone compound, and 3 to 20% by weight of the antimicrobial agent adhesion amount is suitable, and less than 3% does not help to improve the durability, and at least 20% inhibits the stability of the antimicrobial processing liquid. And a touch hardening after manufacture.

By preparing a mixed antimicrobial processing liquid of the above kind, by impregnating or spraying the treated fiber and heat treatment at 90 ℃ to 170 ℃ for 10 to 30 minutes it was possible to obtain a polyester fiber excellent in antibacterial deodorization and laundry durability.

Hereinafter, the present invention will be described in detail with reference to Examples. The antimicrobial properties shown in the Examples were in accordance with the Shake Flask Method and JIS Z 2911 Mold Resistance Test Method. ) And chathamium clobosome (Chaetomium Globosum, American Type Culture Collection No. 6265). And the washing method conforms to JISL-0844 (using a household washing machine).

Example 1

4 g of octadecyl dimethyl (3-trimethoxyl) propyl ammonium chloride (42% active ingredient) via organic silicon as an antibacterial compound, 2 g of modified silicone compound (30% active ingredient) to improve the reaction between the antimicrobial compound and the fiber , 0.7g fatty acid surfactant (active ingredient 50%), 0.26g amino silane compound (active ingredient 30%) to improve crosslinking ability with fiber, and then diluted with water to prepare 100cc of antimicrobial process liquid. After spraying the polyester fiber, and heat-treated at 170 ℃ for 10 minutes. (The adhesion amount of the mixed antimicrobial agent is 7.00% by weight based on the fibers to be treated.)

Property evaluation results at this time are as Table 1, 2, 3.

Comparative Example 1

As an antimicrobial compound, 0.015 g of octadecyl dimethyl (3-trimethoxyl) propylammonium chloride via organic silicon was used in the same manner as in Example 1, and the physical property evaluation results are shown in Tables 1,2 and 3 below.

Comparative Example 2

As an antimicrobial compound, 8 g of octadecyl dimethyl (3-trimethoxyl) propyl ammonium chloride was used as an organic silicone, and the same procedure as in Example 1 was carried out. .

Comparative Example 3

Except for using 0.75g of the modified silicone compound was carried out in the same manner as in Example 1, the physical properties evaluation results are shown in Tables 1,2,3.

[Comparative Example 4]

3.5g of the modified silicone compound was used in the same manner as in Example 1, and the results of the physical property evaluation are shown in Tables 1,2 and 3 below.

[Comparative Example 5]

Except for using 0.3g fatty acid surfactant was carried out in the same manner as in Example 1 and the physical properties evaluation results are shown in Table 1,2,3.

Comparative Example 6

Except for using 1.7g fatty acid surfactant was carried out in the same manner as in Example 1, the physical properties evaluation results are shown in Table 1,2,3.

Comparative Example 7

Except that 0.1g of the amino-based silane compound was carried out in the same manner as in Example 1 and the physical properties evaluation results are shown in Tables 1,2,3.

Comparative Example 8

The procedure of Example 1 was repeated except that 1.3 g of an amino silane compound was used.

Comparative Example 9

Except that the heat treatment conditions were performed for 10 minutes at 80 ℃ was carried out in the same manner as in Example 1 and the results of physical properties evaluation are shown in Table 1,2,3.

Comparative Example 10

The heat treatment conditions were carried out in the same manner as in Example 1 except that for 40 minutes at 180 ℃ and the physical properties evaluation results are shown in Table 1,2,3.

Table 1 Antimicrobial activity against shake flask method

[Table 2] Antimicrobial activity by mold resistance test method

* Mold resistance evaluation result (fungus multiplied on the sample)

◎: No growth at all ○: Only growth marks remain

△: small amount multiplied ×: large amount multiplied

[Table 3] Yellowing phenomenon

○: Yellowing Occurrence ×: Yellowing Occurrence

Claims (2)

The modified silicone compound and fat represented by the following formula (I) are used as an antimicrobial compound by adjusting the amount of the quaternary ammonium salt through the organic silicon to 0.05 to 5% by weight based on the fibers to be treated, and to improve the durability. An acidic surfactant is used in an amount of 20 to 60% by weight and 10 to 40% by weight based on the amount of the antimicrobial compound attached, and an amino silane compound represented by the following formula (II) is used in the amount of 3 to 20% by weight of the amount of the antimicrobial compound attached as the crosslinking agent. To prepare an antimicrobial process solution, and then dilute the antimicrobial process solution with water to impregnate or spray the polyester fiber, and then heat-process the antimicrobial compound to produce the polyester fiber.

Provided that R ₁ , R _{2, and} R ₃ are CnH _{2n + 1} , n is an integer of 0-10, and x, y is an integer of 1-15.

R ₁ and R ₂ are CnH _{2n + 1} and n is an integer of 0-30. The method of claim 1, wherein the heat treatment conditions are carried out over a period of 10 to 30 minutes at a temperature of 90 ℃ to 170 ℃.