KR930012185B1 - Method of preparation for a polyester fiber having an excellent antibiotic and deodorant activity - Google Patents

Abstract

adding the inorganic ceramice, e.g. multiporous silica alumina-based inorganic compound, in which metal ion is contained in the amount of 5-30 wt.%, and whose specific surface area is 100-800 m2/g, particle diameter is 0.1-5 μ, to the copolymerized polyester resin, whose melting point is 10-20 deg.C less than that of the regular polyester, to obtain conc. polyester pellet; mixing the pellet with the regular polyester resin; and spinning. The fiber made by the method has durable antibacterial, deodourizing properties because the finely-powdered multiporous ceramic is bonded physicochemically with the molecule of the odourous component.

Description

Manufacturing method of polyester fiber excellent in antibacterial and deodorant

This invention relates to the manufacturing method of the polyester fiber which makes porous inorganic microparticles | fine-particles exist in a fiber surface, and provides deodorization and antibacterial property. In the case of fibers, microorganisms multiply due to sweat and external pollution of the human body, so that a large amount of ammonia is generated, causing unpleasant odors and harmful problems to the human body. For that reason, many attempts have been made to impart this function to textile materials.

Organic silicone quaternary ammonium salts are widely used as a method of imparting antimicrobial properties to fibers. However, they show yellowing defects when using laundry durability and especially chlorine-based detergents. For this reason, Japanese Patent Application Laid-Open No. 54-38951 sometimes prepares ion-exchange copolymers and treats them with aqueous solutions of copper and silver salts to express metal ions on the fiber surface to impart antimicrobial properties. However, even in such a method, since the metal ions react with the polymer and the physical properties thereof are deteriorated, there is a problem that the process passability is poor in the post-production process and dyeing process.

The present inventors have solved this problem and not only impart antimicrobial activity to the fiber itself, but also to give a deodorizing performance, as a result of the presence of inert inorganic fine particles on the polyester fiber surface excellent washing durability and process permeability Excellent antimicrobial odor polyester fibers have been produced. Representative components of malodorous compounds include many kinds of malodorous components such as ammonia, hydrogen sulfide, trimethylamine, acetaldehyde, and methyl mercaptan. It can be divided into chemical adsorption methods.

In the present invention, in order to remove odor, fine powder porous ceramics are used to physically and chemically combine with malodorous constituent molecules to provide deodorant performance, and are stable to temperature and humidity conditions, and have excellent antibacterial and deodorant properties. Polyester fibers can be produced. Metals chemically bonded to malodorous components generally include iron, copper, silver, mercury, alcohol, lead, and the like. In view of economic reasons and toxicity, in the present invention, copper, silver, iron, etc. Some metal oxides were chemically adsorbed with molecules of malodorous constituents to show deodorizing effect and were stable in temperature and humidity.

The present invention focuses on the fact that metal ions destroy the metabolism of microorganisms and exhibit antimicrobial properties and remove odorous components by the large surface area of porous and metal oxides. A polyester fiber having a property was prepared. In the case of the porous inorganic fine particles used in the present invention, it was used as a binder of metal ions, and the composition of the composition is silica alumina-based inorganic material and has a specific surface area of 100-800 m ² / g. In order to apply to the fiber, the particle size was adjusted to a size of 0.1 to 5 microns, and porous ceramics were dried at 200 to 600 ° C prior to use because of excellent moisture adsorption.

Hereinafter, the present invention will be described in detail.

In the present invention, the addition amount of the porous inorganic ceramic containing metal ions is preferably 0.1 to 10% with respect to the polyester resin, and most preferably 0.5 to 5% by weight. If it is less than 0.1% by weight, the effect is insufficient among the final source. If it is more than 10% by weight, it is not only difficult to pass through the process but also economically lost.

In the case of the metal ion-containing inorganic ceramics used in the present invention, the effect of the antibacterial and deodorant performance is largely dependent on the amount of metal ions present on the surface of the porous ceramic, and moreover, the color of the final stretched yarn depends greatly on this amount.

In order to effectively exhibit the antibacterial and deodorant performance of the present invention, the amount of the metal contained in the porous inorganic ceramics was 1-50% by weight of the total weight of the porous inorganic ceramics, and preferably 5-30% by weight. If it is less than 1% by weight, the antimicrobial deodorizing effect is insufficient for the final fiber, if more than 50% by weight changes the color of the final stretched yarn added with inorganic ceramics occurs a problem that the dyeing of the desired color after weaving becomes impossible. Therefore, in order to contain the appropriate amount of metal ions in the porous inorganic ceramics, the water-soluble metal salt solution was treated before adding it to the polymer, and the excess metal ions remaining on the ceramic surface were washed with water, and then dried under vacuum and not treated. The difference with the weight fraction of the porous inorganic ceramic was calculated to adjust the content of the appropriate metal ion.

In the present invention, the method of adding the inorganic ceramic containing metal ions to the fiber is added to the polymerization process. The metal component on the surface of the ceramic catalyzes during the polymerization reaction so that side reactions occur during the polymerization reaction or the metal ions Formation of a complex compound causes a problem of changing the color of the resin. Therefore, in the present invention, a master batch chip was melt-mixed in a compounder and mixed with a general polyester resin at a ratio of about 1 to 5 times to use a method of dispersing in an extruder during a spinning process. In this case, in order to make the master batch chip, the master batch chip is manufactured by using a thermoplastic polymer having a lower melting point than that of the general polyester in order to uniformly distribute the inorganic ceramic containing metal ions on the surface of dispersibility and the final stretched yarn. It was mixed with an ester resin to prepare a yarn.

In the present invention, the polymer used to make the master batch chip has a melting point of 10 to 20 ° C. lower than that of general polyester, and among the components, dicarboxylic acid is terephthalic acid, dimethyl terephthalate, isophthalic acid, 1,2 As aromatic dicarboxylic acid and glycol, such as -bis (4-carbophenoxy) ethane and 2, 6- naphthalenedicarboxylic acid, ethylene glycol, propylene glycol, butylene glycol, neopentyl glycol, polypropylene glycol polyethylene glycol, polytetramethylene Glycols and the like can be used. When the polymer having a low melting point of 10 to 20 ° C. is mixed with a general polyester and spun, the polymer has a lower viscosity than that of a polyester, so it is spun and formed into a fiber, and the porous inorganic ceramic is distributed in the outer region of the fiber cross section. The deodorizing performance can be sufficiently represented. In addition, by the technology of the composite spinning can be made of the structure of the sea-core and side-by-side and the inorganic ceramic containing the metal in the seed portion is controlled to be distributed.

The composite ratio is preferably such that the portion of the porous inorganic ceramic containing the metal ion is added in the range of 30 to 50% by weight in the total cross-sectional area, and includes the portion containing the inorganic ceramic containing the metal ion for effective performance. It is desirable to be in the outer portion of the fiber cross section rather than the portion that is not.

The antimicrobial test method, deodorant test method and laundry durability test method used in the present invention are as follows.

Antibacterial test method

Test standard The antibacterial effect was tested against Staphylococcus aureus by the AATCC-100 test method. After inoculating the agar medium with the culture group and inoculating the specimen with the incubator for 24 hours at 37 ° C, a certain amount of liquid is added to extract bacteria from the specimen. The percentage of bacteria remaining due to the addition of porous inorganic ceramics containing metal ions was then calculated by measuring the number of bacteria remaining in the treated and untreated fabrics. Usually, 95% or less was determined as bad.

The anti-fog test was carried out using the Aspergillus niger ATTCC 6275 test specimen by the wet method of JISZ-2911. After inoculating the specimens placed in water for one day, inoculated with the specimens (spore suspension) incubated at 20 to 28 ° C for 10 to 20 days, and incubating for 4 weeks, the degree of mycelial growth around the specimens was determined by the following criteria. It was.

Deodorization test method

Place a glass evaporation tube containing odorous gas such as ammonia or hydrogen sulfide under the desiccator, place the specimen on the plate of the passage connected to it, seal the desiccator, leave it at 25 ° C for 2 hours, and then place the glass evaporation tube. The odor concentration was measured in the detector tube and the odor concentration reduction rate was calculated by the following equation, and the percentage was 99% or more and excellent, 95% to 99%, and 95% or less.

Laundry durability test method

100 g of the test cloth was placed in 20 L of water and a washing bath of 35 g of detergent and treated for 12 minutes at a temperature of 40 DEG C, and then repeated 20 times. After washing, the antibacterial and deodorant properties were evaluated by the above method.

The drawn yarn obtained in the present invention can be used in combination with various additives such as known additives, pigments, stabilizers, lubricants, and the like for the purpose of, for example, dyeing and antistatic in a later step.

Hereinafter, the embodiments will be described.

[Examples 1-3]

Containing 4 mole% of isophthalic acid, the melting point is 20 ℃ lower than that of general polyester, and 30% by weight of metal ions vacuum-dried at 150 to 300 ℃ and 1mmHg or less on 90% by weight of copolymerized polyester having a melting point of 0.54 dl / g. 10% by weight of the porous inorganic ceramic contained therein is melt-mixed in a twin screw compounder to prepare pellets. At this time, the temperature of the heating zone is such that one zone is 230 to 245 캜, two zones are 250 to 280 캜, three zones are 260 to 280 캜, four zones are 260 to 280 캜, and five zones are 260 to 285 캜. The pellets were dried at 140 ° C for 8 hours, and then mixed with a polyester resin having an intrinsic viscosity of 0.65 dl / g to 0.5, 2.5% by weight of total polyester in a V-type mixer, followed by a room temperature of 285 ° C and a flux of 2,500m. Spin at / min to get a semi-extended yarn. This semi-stretched yarn was drawn in a conventional manner to form 50 denier / 36 filaments, squeezed and refined in a circular knit machine, and the results were shown in Table 1 above.

[Examples 4 to 6]

Except for adjusting the amount of metal in the porous inorganic ceramics vacuum dried at 150 ~ 300 ℃, 1mmHg or less 5, 20, 30% by weight was the same as in Example 1 and the results are shown in Table 1.

Comparative Example 1

The results are shown in Table 1 in the same manner as in Example 1 except that a polyester resin having an intrinsic viscosity of 0.65 dl / g was used and melted and mixed in a compounder.

Comparative Example 2-4

Except that the amount of addition of the porous inorganic ceramic containing metal ions was the same as in Example 1 and the results are shown in Table 1.

[Comparative Examples 5-7]

Except that the amount of the metal contained in the total weight of the porous inorganic ceramics was changed to the same as in Example 1 and the results are shown in Table 1.

TABLE 1

Claims (1)

When inorganic ceramics are added to copolymerized polyester resins having a melting point of 10 to 20 ° C. lower than that of general polyesters to form high-density polyester pellets, the polyester fibers are mixed and spun to prepare polyester fibers. As inorganic ceramics, metal ions contain 5 to 30% by weight with respect to the total weight of inorganic ceramics, and porous silica alumina-based inorganic materials having specific surface areas of 100 to 800 m ² / g and particle sizes of 0.1 to 5 microns are used. Method of producing a polyester fiber with excellent antibacterial and deodorant performance.