KR102619704B1 - Heavy metal free-antimicrobial polyester draw textured yarn and Manufacturing method thereof - Google Patents

Abstract

The present invention relates to an antibacterial polyester false twist yarn and a method of manufacturing the same, which contains little or no heavy metals harmful to the human body and has antibacterial properties, making it a fabric for clothing or products such as masks and underwear that come in direct contact with the body. It can be applied widely.

Description

Antibacterial polyester false twisted yarn and manufacturing method thereof {Heavy metal free-antimicrobial polyester draw textured yarn and manufacturing method thereof}

The present invention relates to a polyester-based false twist yarn and a method of manufacturing false twist yarn that minimizes or does not contain heavy metals harmful to the human body and has antibacterial properties.

In addition to improving living standards, demand for health and healthcare clothing is gradually increasing following the global COVID-19 outbreak. Accordingly, textile manufacturers are releasing polyester yarns and fabrics with various functional properties (antibacterial, deodorizing, far-infrared, sweat-absorbing and quick-drying) to meet the demands of the market, and are being used in various clothing products.

The purpose of manufacturing antibacterial fibers is to improve hygiene protection in everyday living environments and hospitals. Organic and inorganic antibacterial agents are usually added to fibers to provide antibacterial properties, or antibacterial properties are added to the fabric through post-processing. Grants.

However, most commercially produced polyesters are manufactured using antimony compounds as catalysts, so antimony is contained in the fibers. This is contrary to the purpose of antibacterial fibers and has a negative impact on safety, hygiene, and the environment. It is far from fiber.

In addition, the World Health Organization (WHO)'s International Agency for Research on Cancer (IARC) classifies antimony as a substance that is carcinogenic to humans, and environmental regulations limiting the use of antimony are currently accelerating, especially in Europe. There is an urgent need to develop antibacterial polyester.

Korean Patent Publication No. 10-2001-0056207 (publication date 2001.07.04)

The present invention was devised to solve the above-mentioned problem, and is made by melt-spinning master batch chips containing a polyester resin that does not contain heavy metals and an inorganic antibacterial agent at a certain ratio to create a polyester-based polyester that does not contain heavy metals and has antibacterial properties at the same time. The purpose is to provide false twist yarn and a method for manufacturing the same.

In order to solve the above problems, the present invention relates to an antibacterial polyester false twist yarn that does not contain heavy metals, and includes a chelate represented by the following formula (1) and an inorganic antibacterial agent represented by the following formula (2), and (1) ~ (2) Includes false twist yarn that satisfies the conditions.

(1) Total fineness: 50~300 de

(2) Number of strands: 12~144 ea

[Formula 1]

In Formula 1, R ¹ and R ² are each independently a straight-chain alkylene group having 1 to 5 carbon atoms or a branched alkylene group having 3 to 5 carbon atoms,

[Formula 2]

Ag _a Na _b H _c (H ₃ O) _d Zr _e Hf _f (PO ₄ ) ₃ · _n H ₂ O

In Formula 2, a, b, c, d, e and f are integers, and are numbers that satisfy 1.75<(e+f)<2.25 and a+b+c+d+4(e+f)=9 and n is 2 or less.

As a preferred embodiment of the present invention, the antibacterial polyester-based false-twisted yarn may contain 230 to 380 ppm of the chelate represented by Chemical Formula 1.

As a preferred embodiment of the present invention, the antibacterial polyester-based false twist yarn may contain 0.5 to 5.0% by weight of an inorganic antibacterial agent represented by Chemical Formula 2.

As a preferred embodiment of the present invention, the false twisted yarn of the present invention may contain 10 ppm or less of antimony (Sb) and cobalt (Co).

As a preferred embodiment of the present invention, the false twisted yarn of the present invention may further include 1,450 to 2,500 ppm of titanium element (Ti).

Another object of the present invention relates to a method of manufacturing the false-twisted yarn described above, wherein a master batch chip containing an inorganic antibacterial agent represented by Formula 2 and a polyester chip containing a chelate represented by Formula 1 are mixed and melted. Step 1: manufacturing molten resin; Step 2: manufacturing yarn by spinning the molten resin; and a third step of producing draw textured yarn by performing a false twisting process on the yarn.

As a preferred embodiment of the present invention, the yarn in the second stage may be an undrawn yarn (partially oriented yarn, POY), or a drawn yarn obtained by drawing the undrawn yarn (full draw yarn, FDY).

As a preferred embodiment of the present invention, the polyester chip may include a polyester resin prepared by polymerizing a composition containing 250 to 480 ppm of the chelate and 60 to 370 ppm of the heat stabilizer.

As a preferred embodiment of the present invention, the polyester chip may have an intrinsic viscosity (IV) of 0.65 to 0.85 dl/g.

As a preferred embodiment of the present invention, the ester reaction product may be prepared by esterifying the acid component and the diol component at a molar ratio of 1:1.0 to 2.0.

In a preferred embodiment of the present invention, the acid component may include at least one selected from among aromatic polyvalent carboxylic acids having 6 to 14 carbon atoms, aliphatic polyvalent carboxylic acids having 2 to 14 carbon atoms, and sulfonic acid metal salts.

As a preferred embodiment of the present invention, the diol component may include at least one selected from ethylene glycol and a diol represented by the following formula (3).

[Formula 3]

In Formula 3, R ¹ is a straight-chain alkylene group of C ₁ to C ₅ , and n is an integer of 1 to 20.

In a preferred embodiment of the present invention, the master batch chip contains 5 to 20% by weight of an inorganic antibacterial agent and a polyester resin as the remaining weight%, and the polyester resin is polyethylene terephthalate (PET), polybutylene terephthalate, etc. It may include one or more types selected from phthalate (PBT) and polytrimethylene terephthalate.

As a preferred embodiment of the present invention, the master batch chip containing an inorganic antibacterial agent may have an intrinsic viscosity (IV) of 0.45 to 0.55 dl/g.

As a preferred embodiment of the present invention, the molten resin may include the master batch chip and the polyester chip at a weight ratio of 1:9 to 19.

Another object of the present invention is to provide fabric for clothing, such as knitted fabric, using the antibacterial polyester false twist yarn.

The antibacterial polyester false-twisted yarn that does not contain heavy metals manufactured through the present invention does not contain heavy metals such as antimony and cobalt that are harmful to the human body, and at the same time has antibacterial properties, such as fabric for clothing or masks, underwear, etc. that come in direct contact with the body. It can be applied widely.

The present invention will be described in more detail through a method for manufacturing the polyester false twist yarn of the present invention.

The present invention includes the first step of producing molten resin by mixing and melting master batch chips and polyester chips at a certain ratio; Step 2: manufacturing yarn by spinning the molten resin; and a third step of manufacturing false twist yarn (DTY) by performing a false twist process on the yarn.

The first-stage master batch chip contains an inorganic antibacterial agent and a polyester resin represented by the following formula (2).

[Formula 2]

Ag _a Na _b H _c (H ₃ O) _d Zr _e Hf _f (PO ₄ ) ₃ · _n H ₂ O

In Formula 2, a, b, c, d, e and f are integers, and are numbers that satisfy 1.75<(e+f)<2.25 and a+b+c+d+4(e+f)=9 and preferably, a is 0.05 to 0.20, b is 0.02 to 0.15, c is 0.30 to 0.90, e is less than 0.90 to 2.05, f is 1.75<(e+f)<2.25 and a+b+c+d It is an integer that satisfies +4(e+f)=9. And, n in Formula 2 is 2 or less.

The content of the inorganic antibacterial agent in the master batch chip is 5 to 20% by weight, preferably 7.5 to 15.0% by weight. If the inorganic antibacterial agent content is less than 5% by weight, the melting ratio with the polyester chip increases, thereby increasing the inorganic content in the false twisted yarn produced. If the antibacterial agent content is too low, the antibacterial effect of the false-twisted yarn may be minimal, and if the content of the inorganic antibacterial agent in the master batch chip exceeds 20% by weight, the polyester chip-to-melt ratio is lowered, resulting in a decrease in the dispersibility of the antibacterial agent within the false-twisted yarn. Since the content of the inorganic antibacterial agent is too high at 5.0% by weight, there may be a problem of deterioration of the mechanical properties and processability of the false twisted yarn, so it is recommended to include it in the master batch chip within the above range.

And, the polyester chip used to manufacture the master batch chip has an intrinsic viscosity (IV) of 0.65 to 0.85 dl/g, preferably an intrinsic viscosity (IV) of 0.75 to 0.85 dl/g, more preferably an intrinsic viscosity (IV) of 0.75 to 0.85 dl/g. It is preferable to use 0.80 to 0.85 dl/g in terms of miscibility with inorganic antibacterial agents, solubility, etc.

The polyester chip may include one or more selected from polyethylene terephthalate (PET), polybutylene terephthalate (PBT), and polytrimethylene terephthalate, and may preferably include PET.

And, the content of the polyester resin used to manufacture the master batch chip is the remaining weight percent of the remaining 100 weight percent excluding the inorganic antibacterial agent described above.

In addition, the master batch chip may have an intrinsic viscosity (IV) of 0.45 to 0.55 dl/g, preferably an intrinsic viscosity (IV) of 0.50 to 0.55 dl/g.

Next, the polyester chip of step 1 may be made of a polyester resin prepared by polymerizing a composition containing an ester reaction product of an acid component and a diol component, a chelate represented by the following formula (1), and a heat stabilizer. .

[Formula 1]

In Formula 1, R ¹ and R ² are each independently a straight-chain alkylene group having 1 to 5 carbon atoms or a branched alkylene group having 3 to 5 carbon atoms. Preferably, R ¹ and R ² are each independently having 1 carbon atom. It is a straight-chain alkylene group with ~ 3 carbon atoms or a branched alkylene group with 3-4 carbon atoms, and more preferably, R ¹ and R ² are each independently a straight-chain alkylene group with 1-3 carbon atoms.

Among the compositions used to produce polyester chips, the ester reaction product is obtained by esterifying the acid component and the diol component at a molar ratio of 1:1.0 to 1:5.0, preferably 1:1.0 to 1:2.0. It may be an ester reactant. At this time, if the diol component is contained in a molar ratio of less than 1.0 to the acid, the acidity may become excessively high and a problem of promoting side reactions may occur, and if it is contained in a molar ratio exceeding 5.0, a problem may occur in which the degree of polymerization does not increase.

The acid component may include at least one selected from aromatic polyvalent carboxylic acids having 6 to 14 carbon atoms, aliphatic polyvalent carboxylic acids having 2 to 14 carbon atoms, and sulfonic acid metal salts, and preferably aromatic polyvalent carboxylic acids having 6 to 12 carbon atoms. It may contain one or more types selected from carboxylic acids, aliphatic polyhydric carboxylic acids having 3 to 14 carbon atoms, and sulfonic acid metal salts, and more preferably, terephthalic acid, which does not reduce the heat resistance of polyester, can be used as the acid component. .

Additionally, the diol component may include one or more types selected from ethylene glycol and diol represented by the following formula (3).

[Formula 3]

In Formula 3, R ¹ is a straight-chain alkylene group of C ₁ to C ₅ , preferably a straight-chain alkylene group of C ₂ to C ₄ , more preferably a straight-chain alkylene group of C ₂ to C ₃ It is an alkylene group. Additionally, n in Formula 3 is an integer of 1 to 20, and is preferably an integer of 1 to 10.

In addition, the acid components in the composition used for manufacturing polyester chips include oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, suberic acid, citric acid, pimeric acid, azelaic acid, sebacic acid, and nonanoic acid. , it may further include one or more selected from decanoic acid, dodecanoic acid and hexanodecanoic acid.

In addition, the esterification reaction between the acid component and the diol component can be performed under esterification reaction conditions commonly used in the industry, and a preferred example is performed at a speed of 40 to 80 rpm at 200 to 260°C for 150 to 240 minutes. It can be performed, and more preferably, it can be performed at 210 to 250°C for 180 to 210 minutes at a speed of 50 to 70 rpm.

In addition, the chelate in the composition used to manufacture polyester chips serves as a polymerization catalyst. Since the chelate is stable even in the presence of water molecules, it is not deactivated even when added before the ester reaction in which a large amount of water is produced as a by-product. As a result, the polycondensation reaction can be performed in a shorter time than before, and coloring can be suppressed. In addition, polymerization reactivity is excellent even at low polymerization temperatures, and the relatively high degree of polymerization reduces the generation of carboxyl groups (COOH) at the ends of the produced polyester resin, thereby reducing contamination of the nozzle surface by oligomers and monomers during the spinning process. The number of times the nozzle surface is cleaned can be reduced, thereby improving production yield and reducing defective rates. Additionally, this makes it possible to manufacture human-friendly polymers with reduced acetaldehyde content.

In addition, the chelate content in the composition may be 250 to 480 ppm, more preferably 250 to 400 ppm, and even more preferably 250 to 380 ppm, based on the total weight of the composition. At this time, if the chelate content is less than 250 ppm, the content is too small and the polymerization reaction does not occur well, which may cause problems with polymerization fairness. If the chelate content exceeds 480 ppm, residual chelate in the false-twisted yarn may cause damage to the false-twisted yarn due to excessive use. Since there may be a problem that the color tone b value increases excessively, it is better to produce a polyester resin by performing a polymerization reaction using the above range in the composition.

In addition, the heat stabilizer includes triphenylphosphate (TPP), triethylphosphate (TEP), Phosphoric Acid (H ₃ PO ₄ ), Trimethylphosphate (TMP), tributylphosphate, and tributyl phosphate. One selected from Tributoxyethyl phosphate, Tricresyl phosphate, Triarylphosphate isopropylated and Hydroquinone bis-(diphenyl phosphate) It may include the above, and preferably may include one or more selected from TPP, TEP, H ₃ PO ₄ and TMP, and the content of the heat stabilizer in the composition is 60 to 370 ppm, preferably 62. It may be ~ 250 ppm, more preferably 70 ~ 220 ppm. At this time, if the heat stabilizer content in the composition is less than 60 ppm, the content is so small that the heat stabilization effect due to its use may be insufficient, and if the amount used exceeds 370 ppm. If used, the heat stabilizer content in the false-twisted yarn may exceed 250 ppm, which may significantly reduce the elongation of the false-twisted yarn. Therefore, it is recommended to use within the above range.

In addition, when manufacturing the polyester chip in the first step, the composition may further include a complementary colorant and/or a matting agent in addition to the ester reaction product, chelate, and heat stabilizer.

The complementary color agent is used to adjust the color tone to make the color of the dye dyed in the dyeing process stronger and better when dyeing the manufactured false-twisted yarn, and those known in the textile field can be added. This is a non-limiting example. There are dyes for dyeing, pigments, vat dyes, disperse dyes, and organic pigments. However, it is preferable to use a mixture of blue and red dyes. This is because cobalt compounds, which are commonly used as complementary colorants, are undesirable because they are highly harmful to the human body, whereas complementary colorants mixed with blue and red dyes are desirable because they are harmless to the human body.

Additionally, when a mixture of blue and red dyes is used, there is an advantage in that the color tone can be finely controlled. For example, the blue dye may include solvent blue 104, solvent blue 122, and solvent blue 45, and the red dye may include solvent red 111, solvent red 179, and solvent red 195. In addition, the blue dye and red dye can be mixed at a weight ratio of 1: 1.0 to 3.0, which is advantageous for producing a significant effect in the desired fine color tone control.

In addition, conventionally, a complementary colorant containing cobalt was used as the complementary colorant, but since cobalt is a type of heavy metal, it is preferable to use a non-cobalt-based complementary colorant.

Additionally, the content of the complementary colorant in the composition may be 0.1 to 10 ppm, preferably 1 to 5 ppm, based on the total weight of the composition. At this time, if the complementary colorant content is less than 0.1 ppm, the amount used is too small and the color tone of the false-twisted yarn may not be adjusted to the desired level. If it exceeds 10 ppm, it is uneconomical due to an increase in cost, so it is better to use it within the above range.

In addition, the matting agent serves to suppress the gloss of the false twist yarn, and it is recommended to use TiO ₂ as the matting agent. When using a matting agent, it is recommended that the amount of TiO ₂ used is such that the Ti element content in the produced false-twisted yarn is about 1,450 to 2,500 ppm, and preferably about 1,600 to 2,300 ppm. At this time, if the matting agent content in the composition is less than 1,450 ppm, the amount used is too small and the gloss suppression effect may be insignificant, and if the matting agent in the composition is used so that the Ti element content in the false twist yarn exceeds 2,500 ppm, the gloss suppression effect is increased. It is better to use it within the above range because it can deteriorate fairness and physical properties of false twist yarn without it being present anymore.

Next, in the false twist yarn manufacturing method of the present invention, the second step is a process of manufacturing yarn by spinning the molten resin obtained by melting the master batch chip and the polyester chip of the first step. At this time, the spinning is performed using a spinneret ( Spinning can be performed through a nozzle) at 270 to 310°C and at a spinning speed of 2,200 to 3,500 mpm (meters per minute), preferably at a spinning speed of 2,500 to 3,200 mpm. At this time, if the spinning speed is less than 2,200 mpm, productivity may decrease and the cost may increase, and if the spinning speed exceeds 3,500 mpm, spinning operability may rapidly decrease, so spinning must be performed under the above conditions. It is good to practice.

In addition, the yarn in the second stage may be an undrawn yarn (partially oriented yarn, POY) that has not been drawn, or it may be a full draw yarn (FDY yarn) manufactured by stretching the undrawn yarn. At this time, the stretching method can be performed through a general method used in the art.

Next, step 3 is a process of producing draw textured yarn by performing a false twisting process on the yarn (POY yarn or FDY yarn) manufactured in step 2. The false twisting process is done through a general method used in the industry. It can be manufactured.

The polyester-based false-twisted yarn of the present invention manufactured by this method may contain 230 to 380 ppm, preferably 250 to 350 ppm, of the chelate represented by Chemical Formula 1. At this time, if the chelate content in the false-twisted yarn exceeds 380 ppm, a problem may occur in which the color tone b value of the false-twisted yarn excessively increases.

In addition, the polyester-based false-twisted yarn of the present invention manufactured by the above method may contain 0.5 to 5.0% by weight, preferably 0.8 to 2.0% by weight, of the inorganic antibacterial agent represented by Chemical Formula 2.

In addition, the polyester-based false-twisted yarn of the present invention manufactured by the above method may contain a heat stabilizer at 50 to 250 ppm, preferably at 70 to 220 ppm. In this case, if the heat stabilizer content is less than 50 ppm, the thermal stability is low. It may be insufficient, and if it exceeds 250 ppm, there is a problem of increased cost, and the physical properties of the false twisted yarn may deteriorate due to an increase in the phosphorus (P) content in the false twisted yarn, so it is recommended to use it within the above range.

In addition, when a matting agent is used during production of the polyester-based false-twisted yarn produced by the above method, the polyester-based false-twisted yarn of the present invention may contain 1,450 to 2,500 ppm of titanium (Ti) element.

Additionally, the polyester-based false twist yarn of the present invention can satisfy the following conditions (1) to (2).

Conditions (1) Total fineness: 50 to 300 de, preferably 55 to 200 de, more preferably 60 to 150 de.

Condition (2) Number of filaments: 12 to 144 ea, preferably 24 to 116 ea, more preferably 48 to 100 ea

Additionally, the polyester-based false-twisted yarn of the present invention may contain 10 ppm or less of antimony (Sb) and/or cobalt (Co), and preferably may not contain antimony and/or cobalt at all. Antimony and/or cobalt are inevitably introduced during the false-twisted yarn manufacturing process or due to antimony and/or cobalt components contained in materials used in the production of master batch chips and polyester chips.

In addition, the polyester-based false twist yarn of the present invention has excellent antibacterial properties and can be applied to a wide range of textile products such as fabric for clothing or masks and underwear in direct contact with the body.

Hereinafter, the present invention will be described in more detail through examples. However, the following examples are intended to aid understanding of the present invention, and should not be construed as limiting the scope of the present invention by the following examples.

[Example]

Example 1

(1) Manufacturing of masterbatch chips and polyester chips

A first resin was prepared by mixing 8% by weight of an inorganic antibacterial agent represented by the following formula 2-1 and 92% by weight of a polyethylene terephthalate resin with an intrinsic viscosity (IV) of 0.80 dl/g, and then chipped to produce a master batch chip (inherent). Viscosity (IV) = 0.53 dl/g) was prepared.

[Formula 2-1]

Ag _a Na _b H _c (H ₃ O) _d Zr _e Hf _f (PO ₄ ) ₃ · _n H ₂ O

In Formula 2-1, a = 0.35, b = 0.15, c = 0.25, d = 0.25, e = 1.98, and f = 0.02, and n = 0.27.

Separately, polyester chips were manufactured and prepared as follows.

Terephthalic acid (acid component) and ethylene glycol (diol component) were esterified at a molar ratio of 1:1.2 to obtain an ester reaction product. Next, as a polymerization catalyst, 300 ppm of chelate represented by the following formula 1-1, 150 ppm of H ₃ PO ₄ (heat stabilizer), and a complementary color mixed with blue and red dyes (solvent blue 122:solvent red 195 = 1:1.8~ A composition was prepared by mixing 3.2 ppm (2.0 weight ratio), 2,300 ppm of TiO ₂ (matting agent), and the remaining amount of the ester reaction product.

Next, the composition was subjected to a polymerization reaction at 290°C to prepare a polyester resin, which was then chipped to produce a polyester chip (intrinsic viscosity (IV) = 0.82 dl/g).

[Formula 1-1]

In Formula 1-1, R ¹ and R ² are methylene groups.

(2) Manufacturing of antibacterial polyester false twist yarn

The master batch chip and the polyester chip were added and mixed at a weight ratio of 1:13.5 in a melt extruder at 295°C to prepare a molten resin.

The molten resin was supplied to the spinneret and spun at a spinning temperature of 290°C and a spinning speed of 3,200 mpm to produce POY (partially oriented yarn).

The manufactured POY yarn had a total fineness of 122 de and a filament count of 72 ea.

Next, the POY yarn was subjected to a false twisting process at a false twist speed of 500 mpm, a draw ratio of 1.65 times, a heat setting temperature of 170°C, and a false twist belt angle of 105° to produce an antibacterial polyester false twist yarn (DTY) with a total fineness of 75de and a filament count of 72 ea. was manufactured.

Examples 2 to 3 and Comparative Examples 1 to 3

False-twisted yarn was manufactured in the same manner as in Example 1, but the content of the inorganic antibacterial agent in the master batch chip or the mixing ratio of the master batch chip and the polyester chip was varied as shown in Table 1 below, and then the false-twisted yarn was manufactured using this. Thus, Examples 2 to 3 and Comparative Examples 1 to 3 were carried out, respectively.

Example 4 and Comparative Examples 4 to 6

False twist yarn was manufactured in the same manner as in Example 1, but when manufacturing the master batch chip as shown in Table 1 below, the master batch chip was manufactured by varying the content of the inorganic antibacterial agent represented by Chemical Formula 2-1, and then false twisted using the same. Each yarn was manufactured, and Example 4 and Comparative Examples 4 to 6 were performed.

Experimental Example 1: Physical property measurement

The contents of heavy metals (Sb, Co) in the false-twisted yarns, antibacterial properties, workability, and operability of each of the false-twisted yarns manufactured in the above Examples and Comparative Examples were measured and evaluated, and the results are shown in Table 1 below.

(1) Measurement of antibacterial activity

It was evaluated as bacteriostatic reduction rate (%) according to KS K 0693-2006. Specifically, the reduction rate was calculated using Staphylococcus aureus and Klebsiella pneumoniae using the initial bacterial count and the bacterial count after 18 hours of incubation.

(2) Evaluation of workability and operability

Workability and operability were evaluated by measuring the number of thread breaks during the 24-hour brazing process (◎ - 0 times, ○ - 1 time, △ - 2 times, × - 3 or more times).

division Example 1 Example 2 Example 3 Example 4 Comparative Example 1 Inorganic antibacterial agent content in master batch chip 8% by weight 11.8% by weight 8% by weight 18.0% by weight 8% by weight Masterbatch chips and polyester chips
weight ratio 1:13.5 1:19 1:10.3 1:13.5 1:5.0 Inorganic antibacterial agent content in false-twisted yarn (% by weight) 0.55 0.52 0.70 1.24 1.33 Chelate content in false twist yarn (ppm) 279 285 273 276 250 Ti element content in false twisted yarn (ppm) 1454 1468 1449 1453 1432 Total fineness (de) / number of filaments (ea) 75/72 75/72 75/72 75/72 75/72 Contains heavy metals Nothing Nothing Nothing Nothing Nothing antibacterial 99% 98% 99% 99% 99% Workability and operability ◎ ◎ ○ ○ ×

division Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6 Content of inorganic antibacterial agent in master batch chip 8% by weight 8% by weight - 4.5% by weight 20.5% by weight Masterbatch chips and polyester chips
weight ratio 1:20 1:8.0 1:13.5 1:13.5 1:13.5 Inorganic antibacterial agent content in false-twisted yarn (% by weight) 0.38 0.88 - 0.31 1.41 Chelate content in false twist yarn (ppm) 285 266 278 279 278 Ti element content in false twisted yarn (ppm) 1471 1445 1451 1458 1449 Fineness (de) / Number of filaments (ea) 75/72 75/72 75/72 75/72 75/72 Contains heavy metals Nothing Nothing Nothing Nothing Nothing antibacterial 46% 99% 0% 24% 99% Workability and operability ◎ △ ◎ ◎ ×

Looking at the physical property measurement results in Tables 1 and 2, the false-twisted yarns of Examples 1 to 4 showed high antibacterial properties and excellent workability and operability during the manufacturing process.

On the other hand, in the case of Comparative Example 2, in which polyester chips were used in a weight ratio exceeding 19 compared to the master batch chips, workability and operability were excellent, but there was a problem of insufficient antibacterial properties, and the polyester chips were used in a weight ratio less than 9 compared to the master batch chips. In the case of Comparative Examples 1 and 3 used, the results showed poor workability and operability compared to Example 3.

In the case of Comparative Example 4, which did not use a master batch chip, and Comparative Example 5, where the content of inorganic antibacterial agent in the master batch chip was less than 5% by weight, it was confirmed that there was a problem of very insufficient antibacterial activity, and the content of inorganic antibacterial agent in the master batch chip was 20% by weight. In the case of Comparative Example 6 where the weight % was exceeded, antibacterial properties were excellent, but workability and operability were very poor.

Through the above examples and experimental examples, it was confirmed that the antibacterial polyester false-twisted yarn of the present invention had excellent operability and workability during the manufacturing process, as well as excellent antibacterial properties. It was confirmed that the antibacterial polyester false-twisted yarn of the present invention is suitable for use as a functional clothing fabric, mask material, etc., while having antibacterial properties and having no adverse effects on the human body due to heavy metals.

Claims (9)

Contains 230 to 380 ppm of chelate represented by Formula 1 below and 0.5 to 5.0% by weight of an inorganic antibacterial agent represented by Formula 2 below,
An antibacterial polyester false-twisted yarn that satisfies the following conditions (1) to (2) and further contains 1,450 to 2,500 ppm of titanium element (Ti).
(1) Total fineness: 50~300 de
(2) Number of filaments: 12 ~ 144 ea
[Formula 1]

In Formula 1, R ¹ and R ² are each independently a straight-chain alkylene group having 1 to 5 carbon atoms or a branched alkylene group having 3 to 5 carbon atoms,
[Formula 2]
Ag _a Na _b H _c (H ₃ O) _d Zr _e Hf _f (PO ₄ ) ₃ · _n H ₂ O
In Formula 2, a, b, c, d, e and f are integers, and are numbers that satisfy 1.75<(e+f)<2.25 and a+b+c+d+4(e+f)=9 and n is 2 or less.
The antibacterial polyester false-twisted yarn according to claim 1, characterized in that it contains 10 ppm or less of antimony (Sb) and cobalt (Co).
delete A first step of preparing a molten resin by mixing and melting a master batch chip containing an inorganic antibacterial agent represented by Formula 2 below and a polyester chip containing a chelate represented by Formula 1 below;
Step 2 of manufacturing yarn by spinning the molten resin to produce partially oriented yarn (POY) as yarn, or by drawing the undrawn yarn to manufacture full draw yarn (FDY); and
Step 3 of producing draw textured yarn containing 1,450 to 2,500 ppm of titanium element (Ti) by performing a draw twisting process on the yarn;
It is manufactured by performing a process including,
The polyester chip of the first stage is an antibacterial polyester-based fuse, characterized in that it contains a polyester resin prepared by polymerizing a composition containing an ester reaction product, a chelate represented by the following formula (1), a heat stabilizer, and a matting agent. Yarn manufacturing method.
[Formula 1]

In Formula 1, R ¹ and R ² are each independently a straight-chain alkylene group having 1 to 5 carbon atoms or a branched alkylene group having 3 to 5 carbon atoms,
[Formula 2]
Ag _a Na _b H _c (H ₃ O) _d Zr _e Hf _f (PO ₄ ) ₃ · _n H ₂ O
In Formula 2, a, b, c, d, e and f are integers, and are numbers that satisfy 1.75<(e+f)<2.25 and a+b+c+d+4(e+f)=9 and n is 2 or less.
The method of claim 4, wherein the polyester chip is
A method for producing an antibacterial polyester false-twisted yarn, comprising a polyester resin prepared by polymerizing a composition containing 250 to 480 ppm of the chelate and 60 to 370 ppm of the heat stabilizer.
The method of claim 4, wherein the ester reaction product is prepared by esterifying the acid component and the diol component at a molar ratio of 1:1.0 to 2.0,
The acid component includes at least one selected from aromatic polyhydric carboxylic acids having 6 to 14 carbon atoms, aliphatic polyhydric carboxylic acids having 2 to 14 carbon atoms, and sulfonic acid metal salts,
A method for producing an antibacterial polyester-based false twist yarn, wherein the diol component includes at least one selected from ethylene glycol and a diol represented by the following formula (3);
[Formula 3]

In Formula 3, R ¹ is a straight-chain alkylene group of C ₁ to C ₅ , and n is an integer of 1 to 20.
The method of claim 4, wherein the master batch chip contains 5 to 20% by weight of an inorganic antibacterial agent and polyester resin as the remaining weight%,
A method for producing an antibacterial polyester-based false twist yarn, wherein the polyester resin includes at least one selected from polyethylene terephthalate (PET), polybutylene terephthalate (PBT), and polytrimethylene terephthalate.
The method of claim 4, wherein the molten resin includes the master batch chips and the polyester chips in a weight ratio of 1:9 to 19.
A knitted fabric comprising the antibacterial polyester false twist yarn of claim 1 or 2.