KR102403184B1 - Eco-friendly fiber yarn and manufacturing method thereof - Google Patents

Abstract

The present invention relates to an eco-friendly fiber yarn, a manufacturing method therefor, and a fabric and clothing product manufactured from the eco-friendly fiber yarn. More specifically, the eco-friendly fiber yarn, the fabric and the clothing product manufactured by the method have antibacterial and biodegradable properties, and at the same time have the effect of exhibiting excellent durability.

Description

Eco-friendly fiber yarn and manufacturing method thereof

The present invention relates to an eco-friendly fiber yarn and a manufacturing method thereof, and to fabrics and clothing products manufactured from the eco-friendly fiber yarn.

Modern people have become more interested in health and hygiene, etc. as their lives have become more prosperous, and the apparel industry has begun to focus on the development of fabrics with various functions such as hygiene.

Fabric is a raw material for all clothing. Most fabrics used for clothing are commercialized through simple processing and sewing processes that do not have any functionalities, thus forming favorable conditions for the growth of various harmful bacteria and fungi. There is a problem to do.

Propagation of harmful bacteria and fungi can cause discomfort to people around them due to bad odors, etc., reduce confidence and atrophy of people wearing clothes, and furthermore, bacteria or fungi multiply on the skin, which can cause diseases. can be a factor

In order to solve the above problem, a fabric with an antibacterial function has been developed, and as a conventional technique for exhibiting an antibacterial function, a material made of silver is representative. Silver is widely known to have sterilization and antibacterial effects in various fields, and is known to have low human toxicity and excellent antibacterial activity compared to general organic antibacterial agents.

Methods for treating such silver particles on fibers such as fabrics include direct deposition or adsorption on fabrics, a method of reacting silver ions with fibers using a solvent as a catalyst, a method of treating fabrics using a spray method, a coating method, etc. etc. are used in various ways.

However, the fibers treated with silver particles have problems in that it is difficult to control the fiber thickness due to the particle size, and the silver particles are lost in the fabric manufacturing process, so that the functionality due to silver is not sufficiently exhibited in the product or it is not exhibited for a long time. In addition, a method of treating a large amount of silver particles may be used to prevent loss in the manufacturing process, but the problem of causing discoloration of the processing agent itself and the object to be treated cannot be avoided.

In addition, a method of imparting antibacterial properties to clothes using a natural material extract having antibacterial activity has been devised, but it is difficult to maintain the functionality for a long time by spraying or coating the natural material extract on the fabric. The extracted natural ingredients are easily lost. In addition, when fabrics are manufactured using synthetic polymers to contain natural material extracts in the fibers themselves, functional substances exhibiting antibacterial properties are destroyed by the high heat used in the manufacturing process, so they are satisfied with the fact that they contain only natural antibacterial substances. In practice, there is a limit to sufficiently exhibiting its functionality.

On the other hand, fibers using currently commercialized plastic resins (for example, polyethylene, etc.) have very low degradability in their natural state, and have a fatal adverse effect on the environment when discarded. This has been discussed

Representative examples of such biodegradable plastic resins include poly lactic acid (PLA), poly butylenes succinate (PBS), and poly butylene adipate-co-terephthalate (PBAT). Despite their excellent environmental advantages due to their biodegradability, there is a problem in that they are not suitable as fibers for use in clothes in mechanical properties such as durability.

Republic of Korea Patent Publication No. 10-2300129 Republic of Korea Patent Publication No. 10-2263195 Republic of Korea Patent Publication No. 10-2021-0104551

The present inventors have recognized the problems of the prior art, and have completed the present invention by proving that the eco-friendly fiber yarn manufactured by a specific method can have excellent durability while having antibacterial and biodegradable properties.

The present invention relates to a method for manufacturing an eco-friendly fiber yarn comprising the following steps.

S1) PLA (Poly Lactic Acid) resin and PCL (Polycaprolactone) resin is put into an extruder, heated to a temperature of 200 to 230 ℃ to melt to prepare a base mixed resin;

S2) cooling the molten base mixed resin to 150 to 180 ℃;

S3) mixing the PLGA resin containing the natural complex extract with the cooled base mixed resin, and then stirring the mixture for 1 to 3 minutes;

S4) after extruding the stirred mixture, cooling to 55 to 65 ℃;

S5) cutting the cooled extrudate to prepare a master batch chip in the form of pellets; and

S6) manufacturing a yarn using the master batch chip.

The present invention relates to an eco-friendly textile fabric manufactured using the yarn manufactured by the manufacturing method of the present invention.

The present invention relates to a clothing product manufactured using the eco-friendly textile fabric.

Hereinafter, this will be described in detail. All combinations of the various elements disclosed herein are within the scope of the present invention. In addition, it cannot be considered that the scope of the present invention is limited by the following specific description.

The present invention provides a method for producing an eco-friendly fiber yarn comprising the following steps:

S1) PLA (Poly Lactic Acid) resin and PCL (Polycaprolactone) resin is put into an extruder, heated to a temperature of 200 to 230 ℃ to melt to prepare a base mixed resin;

S2) cooling the molten base mixed resin to a temperature of 150 to 180 ℃;

S3) mixing the PLGA resin containing the natural complex extract with the cooled PLA resin, and then stirring the mixture for 1 to 3 minutes;

S4) after extruding the stirred mixture, cooling to 55 to 65 ℃;

S5) cutting the cooled extrudate to prepare a master batch chip in the form of pellets; and

S6) manufacturing a yarn using the master batch chip.

Hereinafter, a method for manufacturing an eco-friendly fiber yarn will be described in detail.

Step S1) in the manufacturing method of the present invention is a step of preparing a base mixed resin by putting a PLA (Poly Lactic Acid) resin and a PCL (Polycaprolactone) resin into an extruder, and heating it to a temperature of 200 to 230°C to melt it.

In the present invention, "PLA (Poly Lactic Acid)" refers to a biodegradable resin mainly made from plants such as corn and sugar cane, and is produced the most among eco-friendly (biodegradable) polymer compounds worldwide. Cargill-Dow Polymer, Chronopol, and Mitsui Chemicals in the US are producing this material, and more than 1.5 million tons are being supplied worldwide. Polylactic acid (PLA) resin is being studied a lot in material engineering by adding substances that are not harmful to the human body or by itself, and is medically used as a scaffold in tissue engineering (Biomaterials. 2004 May;25(10):1901-9., Avd Exp Med Biol, 2003;534: 191-9., Ann N Y Acad Sci. 2002 Oct;974:556-64) It is a biodegradable resin that possesses several characteristics even from a commercial point of view for general use, not for special fields.

In the present invention, PLA resin may be directly manufactured or pre-manufactured and sold, and may be used regardless of the production company (Cargill Dow Polymers, Mitsui Chemical, Chronopol or Dhimadzu, etc.).

In addition, according to the experimental examples of the present invention, PLA may have a molecular weight of 5,000 to 500,000 Da, preferably about 80,000 to 90,000 Da, but is not limited thereto.

In the present invention, "PCL (Polycaprolactone)" means a semi-crystalline biodegradable thermoplastic polyester having a melting point of about 60 ° C. It is used in tapes, tissue engineering, orthopedics, and dental implants.

The PCL induces a transesterification reaction by alcohol decomposition during melt blending for the production of PLA and base mixed resin to form a copolymer, thereby reducing the disadvantages related to the physical properties of PLA, for example, low thermal stability, mechanical properties, etc. can play a role in improving it.

In the present invention, the PCL resin may be directly manufactured or pre-manufactured and sold. In addition, according to the experimental examples of the present invention, PCL may have a molecular weight of about 1,500 to 3,000 Da, but is not limited thereto.

In the present invention, "base mixed resin" means a mixed resin of PLA and PCL that is pre-mixed before mixing the PLGA resin containing the natural complex extract during the manufacturing process of the master medium chip.

In the present invention, the temperature for preparing the base mixed resin may be 200 to 250° C., preferably 200 to 230° C., but is not limited thereto.

If it is less than the above range, the degree of improvement of the physical properties of PLA may be low because the transesterification reaction of PLA and PCL is not sufficient, and if it exceeds the above range, the quality of the molded article may be deteriorated due to oxidation by heat.

PLA and PCL included in the base mixed resin in the present invention may be included in a weight ratio of 1:0.8 to 1:1.8, preferably 1:1 to 1:1.6.

In the present invention, when PCL to PLA is included in less than the above weight ratio, excellent durability of the yarn and fabric manufactured therefrom may not be secured, and when PCL to PLA is included in more than the above weight ratio, yarn and manufactured therefrom The hardness of the fabric increases, so it may not be suitable for use in clothes.

According to embodiments of the present invention, PLA and PCL included in the base mixed resin may be included in a weight ratio of 1:1.3, but is not limited thereto.

In the present invention, the base mixed resin may further contain a biodegradable polymer material to supplement physical properties, for example, aliphatic polyester (AP), cellulose acetate (CA) and cellulose di acetate (CDA), polybutylene succinate (PBS). ), Polyester urethane (PEU) and Ployglycolic acid (PGA), polyhydroxyalkanoic acid (PHA), poly(3-hydroxybutyrate) (PHB), poly(3-hydroxyvalerate) (PHV) and pullulan (Pullulan) It may be one or more selected from the group consisting of, but is not limited thereto.

Step S2) in the manufacturing method of the present invention is a step of cooling the molten base mixed resin to 150 to 180 ℃.

In the eco-friendly fiber yarn manufacturing method of the present invention, before mixing the PLGA resin containing the natural complex extract, the step of cooling to 150 to 180 ℃ should be performed.

When the PLGA resin containing the natural complex extract is mixed at a temperature exceeding the above range, the functional substances contained in the natural complex extract are destroyed, and the desired effect may be insignificant due to the substances, and the When mixing the PLGA resin containing the natural complex extract at temperature, the fluidity of the base mixed resin of PLA and PCL is lowered, so it may not be well mixed with the PLGA resin.

Step S3) in the manufacturing method of the present invention is a step of mixing the PLGA resin containing the natural complex extract with the cooled base mixed resin, and then stirring the mixture for 1 to 3 minutes.

In the present invention, "extract" means the result of extraction using an appropriate extraction solvent, and the extract is an extract obtained by extraction, a diluted or concentrated solution of the extract, a dried product obtained by drying the extract, a prepared or purified product thereof, or fractions.

In the present invention, "natural complex extract" refers to an extract extracted through a manufacturing process in a mixture state in which the natural raw materials of each extract are mixed at the same time.

In the present invention, the natural complex extract may include extracts from Hwangchil tree, Duchung tree, and Hobak tree extract.

In the present invention, "Hwangchil tree (Dendropanax morbifera)" is an evergreen tree belonging to the Araliaceae family, and it can be seen in some island areas of the southern coast of our country. .

In the present invention, "Eucommia ulmoides oliver" is a deciduous tree belonging to the Eucommia ulmoides oliver family. The leaves are alternately oval, and when the fruit is cut into a flat long circle, a rubbery viscous thread comes out, and the dried bark is used as herbal medicine. . The bark of the duchung tree is called duchung, and the young leaves are called cotton.

In the present invention, "Magnolia officinalis Rehd et Wils." is a deciduous tree that is native to China and is known to grow at an altitude of 700 m or less in the southern island region in Korea. It has been reported that the effect of nutmeg tree is effective in gastric ulcer and duodenal spasm, and also has a blood pressure lowering action and a relatively strong antibacterial action. In addition, there are clinical reports that it is effective against acute gastroenteritis or bacterial dysentery. The main components of green pepper are honokiol, magnolol, eudesmagnolol, magnoloside A, B, C, and magnocurarine.

In the present invention, "crushing" may mean crushing an object of a certain size, but is not limited thereto, and may mean any act of reducing the size of an object.

According to the embodiments of the present invention, the extracts of hwangchil tree, cypress tree and champignon tree extract for preparing the natural complex extract are pulverized and evenly mixed in a dried form, and are extracted through an extraction method under certain conditions.

According to embodiments of the present invention, the method for preparing a natural complex extract in the present invention includes the following steps:

a) pulverizing hwangchil wood, duchung wood, and spruce wood;

b) mixing the pulverized hwangchil wood, duchung wood, and spruce wood;

c) adding 80% (v/v) ethanol to the mixture and extracting at 60 to 80° C. for 8 hours;

d) filtering the obtained extract to separate a filtrate and a residue;

e) adding purified water to the residue separated in step d) and sonicating while continuously stirring at 60 to 80° C. for 8 hours using an ultrasonic extractor;

f) filtering the obtained extract to separate a filtrate and a residue; and

g) mixing the filtrate separated in steps d) and f).

In the step b) of the present invention, the hwangchil tree, the duchung tree and the rhododendron tree may be mixed in a weight ratio of 1:1:1. In order to obtain a functional effect due to the natural complex extract in the present invention, it is preferable to mix in the above weight ratio.

Ethanol as the extraction solvent in step c) of the present invention may preferably have a concentration of 70 to 90% (v/v) in order to maximize the extraction of the active ingredients contained in Hwangchil tree, Duchung tree, and Hobak tree. not limited According to embodiments of the present invention, ethanol as the extraction solvent preferably has a concentration of 80% (v/v), but is not limited thereto.

In step e) of the present invention, ultrasonic extraction using an ultrasonic extractor is applied. Ultrasonic extraction can improve the permeability of the solvent by air bubbles and lower the extraction temperature, thereby increasing the extraction yield while preventing the destruction of heat-labile substances in the raw materials of natural extracts.

Steps c) and e) in the present invention may be carried out at a temperature of 60 to 80 ℃, preferably it may be carried out at a temperature of 65 to 75 ℃.

When heat is applied to a temperature exceeding the above range, the extraction yield may be increased or the extraction process time may be shortened. In addition, when heat is applied to a temperature less than the above range, it may be undesirable in terms of extraction efficiency. Therefore, performing steps c) and e) at a temperature within the above range is very advantageous in terms of integrity and extraction yield of the extracted active ingredient.

According to embodiments of the present invention, steps c) and e) may be performed at a temperature of 70° C., but is not limited thereto.

In addition, in the present invention, steps c) and e) may be performed for 6 hours to 10 hours, preferably for 7 hours to 9 hours, and more preferably for 7 hours 30 minutes to 8 hours 30 minutes. it could be According to embodiments of the present invention, it may be about 8 hours, but is not limited thereto.

When it is performed less than the above range, the extraction of the active ingredient of the extract may not be sufficient to show the effect, and when it is performed beyond the above range, the extraction efficiency of the active ingredient may be lowered compared to the input time and energy.

Between steps c) and d) in the present invention; And between steps e) and f) may further include the step of cooling and aging the sonicated mixture solution to 4 ℃.

The aging step increases the extraction rate and efficacy of the active ingredient in the natural raw material, and if the aging step is not included, the content and antibacterial properties of the active ingredient may not reach the level intended in the present invention.

In the present invention, in the manufacturing method listed in alphabetical order of a) to g), each step is sequentially performed in alphabetical order. If the order of each step is changed, the functional ingredients included in the finally obtained natural complex extract may not be extracted to the level intended by the present invention.

In the present invention, the PLGA resin containing the natural complex extract is prepared through the following preparation method:

x) dissolving the natural complex extract and PLGA in an organic solvent;

y) adding the prepared solution to 1% PVA aqueous solution, followed by stirring; and

z) Magnetic stirrer A step of evaporating the organic solvent with a magnetic stirrer to solidify PLGA to obtain PLGA containing a natural complex extract.

In the present invention, "PLGA (polylactide-co-glycolide)" is a random copolymer of lactide (LA) and glycolide (GA). It refers to a bioplastic with characteristics such as biodegradability, biocompatibility, structural stability, and low toxicity. , are mainly used as medical polymers such as drug delivery systems and implants.

In the present invention, PLGA can form an outer wall for the natural complex extract, and can serve to minimize the denaturation of the natural complex extract during the time that PLGA is melted in the production of master batch chips.

In the present invention, the PLGA may have a molecular weight of 4,000 Da to 75,000 Da, preferably 50,000 to 75,000 Da, but is not limited thereto.

In the present invention, the PLGA may have a monomer molar ratio of lactide and glycolide of 90:10 to 50:50, preferably 85:15, but is not limited thereto.

In the present invention, in the PLGA, an end group may be an ester (neutral charge) or a carboxylic acid (negative charge).

In the present invention, PLGA can be directly manufactured or purchased commercially sold products can be used. Examples of commercially available products include 10P001 (50:50) from the Expansorb ^® family of products from PCAS; 10P002 (75:25); 10P003 (75:25); 10P007 (90:10); 10P008 (85:15); 10P009 (85:15E); 10P010(65:35E); 10P016(50:50E); 10P017(50:50); 10P019(50:50E); 10P020 (85:15); 10P022(50:50); 10P023(90:10); 10P024(50:50); 10P025 (90:10), RG 502 (50:50) from the Resomer ^® range from Aldrich ^® Evonik Rohm Pharma GmbH; RG 502H (50:50); RG503 (50:50); RG 503H (50:50); RG 504 (50:50); RG 504H (50:50); RG 505 (50:50); RG653H (65:35); RG 752H (75:25); There is the RG 756S (75:25). Also PDLG 7502 (75:25) from Purac Biomaterials' Purasorb ^® family; PDLG 7502A (75:25); PDLG7507 (75:25); PDLG 5002 (50:50); PDLG 5002A (50:50); PDLG 5004 (50:50); PDLG5004A (50:50); PDLG 5010 (50:50), PLGA-7505 (75:25) from Wako Pure Chemical Industries; PLGA-7510 (75:25); PLGA-7515 (75:25); PLGA-7520 (75:25); PLGA-5005 (50:50); PLGA-5010 (50:50); PLGA-5015 (50:50).

In step x) of the present invention, the organic solvent is not particularly limited as long as it can dissolve the biodegradable polymer. For example, dichloromethane, chloroform, acetonitrile, dimethyl sulfoxide (DMSO), dimethylformamide (Dimethylformaldehyde), ethyl acetate (Ethylacetate), butyl acetate (Butyl acetate), Ethyl formate (Ethyl formate), isopropyl acetate (Isopropylacetate), isopropyl formate (Isopropyl formate), diethyl ether (Diethyl ether) and glycofurol (Glycofurol) may be at least one selected from the group consisting of, It is not limited thereto.

According to embodiments of the present invention, the organic solvent may be DCM (dichloromethane), but is not limited thereto.

In step x) of the present invention, the natural complex extract may be mixed in an amount of 0.1 to 40% by weight, and PLGA may be mixed in an amount of 60 to 99.9% by weight.

In addition, in step x) of the present invention, the natural complex extract and PLGA may be mixed in a weight ratio of 0.1:99.9 to 4:6, and according to embodiments, it may be 3:7 (natural complex extract: PLGA). , but not limited thereto.

In the present invention, in the step z), it is preferable to strongly stir with a magnetic stirrer so that the fine droplets do not agglomerate with each other.

In addition, step z) may be performed for 3 to 5 hours, and when less than 3 hours, PLGA, a biodegradable polymer, is less cured and agglomeration occurs between particles, so it may be difficult to mix evenly in the base mixed resin, 5 hours If it exceeds, it is not suitable for manufacturing efficiency.

In the present invention, the method for producing PLGA including the natural complex extract may further include a step q) of vacuum drying (30 to 40° C.) of the solidified PLGA prepared in step z).

In the present invention, step S3) is a step of mixing the PLGA resin containing the natural complex extract with the base mixed resin cooled to 150 to 180° C. and then stirring, and the stirring time of the mixture is preferably 1 to 3 minutes.

If the stirring is less than the above range, it is difficult for the PLGA resin to be evenly mixed with the base mixed resin. If the stirring exceeds the above range, the PLGA is completely melted and the natural complex extract is exposed to heat, so that the functional components of the natural complex extract are altered. degree may increase.

In the present invention, step S4) is a step of cooling the stirred mixture to 55 to 65 ° C. .

In the present invention, the master batch chip may contain 30 parts by weight of the PLGA resin including the natural complex extract relative to 100 parts by weight of the base mixed resin.

In the present invention, step S6) is a step of manufacturing a yarn using the master batch chip.

In the present invention, the production of the yarn may be prepared through a conventional method in the industry. For example, the master batch chip may be put into an extruder equipped with a yarn manufacturing mold, and the yarn may be manufactured through the processes of melting, spinning and cooling.

Another aspect of the present invention provides an eco-friendly textile fabric manufactured using the yarn manufactured by the above manufacturing method.

The eco-friendly textile fabric may have antibacterial properties and biodegradability, and may also have excellent durability.

In the present invention, "antibacterial" means a property that resists bacteria.

In the present invention, "biodegradability" refers to the property of being completely decomposed into water, carbon dioxide, methane, etc. by microorganisms such as fungi and bacteria.

In the present invention, "durability" means that the tensile strength and tear strength of the fabric made of the fiber yarn is more than the recommended standard that a fabric that can be used for clothes, etc. should have.

Another aspect of the present invention provides a clothing product manufactured using an eco-friendly textile fabric.

In the present invention, "clothes" is a generic term for things that protect or decorate the body and appearance, and includes not only clothes necessary for daily life such as T-shirts and underwear, but also military clothes and winter clothes used in special situations.

In the present invention, the details of the eco-friendly textile fabric and clothing are the same as those described in the eco-friendly fiber yarn manufacturing method unless otherwise stated, and are omitted to avoid excessive repetition of the specification.

Since the eco-friendly fiber yarn manufacturing method of the present invention is advantageous in securing the integrity of the functional components of the natural complex extract, the yarn prepared therefrom can exhibit excellent antibacterial properties, and useful effects of functional ingredients other than the antibacterial properties of the natural complex extract can be fully obtained.

In addition, since the eco-friendly fiber yarn manufacturing method of the present invention uses a biodegradable polymer in the manufacturing process, it is eco-friendly and harmless to the human body.

In addition, the yarn manufactured by the eco-friendly fiber yarn manufacturing method of the present invention has excellent durability, so that it can be usefully used for clothing products.

In addition, since the clothing product containing the yarn manufactured by the method for producing an eco-friendly fiber yarn of the present invention has excellent softness, breathability, comfort and drape properties, it is possible to provide emotional fibers to our daily life.

Hereinafter, the present invention will be described in more detail by way of Examples. However, these examples are for illustrative purposes only, and the scope of the present invention is not limited by these examples. In addition, it will be understood that terms not specifically defined herein have meanings commonly used in the technical field to which the present invention pertains.

Example

(1) Preparation of natural complex extract

After washing the hwangchil tree (stem), the cypress tree (bark), and the rhododendron tree (bark) cleanly, drying it, and grinding it to 1 to 3 cm through a grinder, it is mixed in a weight ratio of 1:1:1. mixed evenly. 10 L of 80% (v/v) ethanol was added to 1 kg of the mixture, and the mixture was extracted at 60 to 80° C. for 8 hours. Thereafter, the obtained extract was filtered, the filtrate and the transcript were separated, and the filtrate (the first filtrate) was separately stored. Then, purified water is added to the separated residue, and ultrasonic treatment is performed while continuously stirring at 60 to 80° C. for 8 hours using an ultrasonic extractor, and the sonicated extract is filtered to obtain a filtrate (second filtrate) and It was isolated as a residue. Then, the first filtrate and the second filtrate were mixed, concentrated under reduced pressure, and then freeze-dried to prepare a natural complex extract.

(2) Preparation of PLGA resin containing natural complex extract

After mixing the prepared natural complex extract and PLGA (Manufacturer: Purac Biomaterials, PLA:PGA=85:15, molecular weight: 50,000 to 75,000 Da) in a weight ratio of 3:7, it was dissolved in DCM (dichloromethane), and the obtained solution was added to 1% PVA aqueous solution, followed by stirring. Thereafter, DCM was evaporated with a magnetic stirrer and PLGA was solidified to prepare PLGA containing a natural complex extract.

(3) Preparation of master medium chips

PLA resin (manufacturer: Shimadzu, molecular weight: 80,000-90,000 Da) and PCL resin (manufacturer: Union Carbide, molecular weight: 1,500 to 3,000 Da) in a weight ratio of 1:1.3 (PLA:PCL) into the extruder, 200 to 230 It was melted by heating to a temperature of °C. After that, the molten PLA and PCL mixed resin (herein, referred to as "base mixed resin") is cooled to a temperature of 150 to 180 ° C. through a cooler, and the PLGA resin containing the prepared natural extract is mixed with the base. 30 parts by weight of PLGA resin containing a natural complex extract was mixed with respect to 100 parts by weight of the resin, and stirred for about 2 minutes. After that, the stirred mixture was extruded, cooled to 55 to 65° C. through a cooler, and the cooled extrudate was cut to prepare master batch chips in the form of pellets.

(4) Manufacture of eco-friendly fiber yarn

The prepared master batch chip was put into an extruder equipped with a yarn manufacturing mold, and a yarn was prepared through a conventional method in the industry (eg, through a process of melting, spinning and cooling).

Comparative Example 1

In the manufacturing method of the example, after preparing the yarn through the same method as in the example except that only the hwangchil tree (stem) was used during the preparation of the natural complex extract, the fabric was prepared according to a conventional method.

Comparative Example 2

In the manufacturing method of the example, after preparing the yarn through the same method as in the example except that only the cypress tree (bark) was used in the preparation of the natural complex extract, the fabric was prepared according to a conventional method.

Comparative Example 3

In the manufacturing method of the example, after manufacturing the yarn through the same method as in the example except that only the spruce tree (bark) was used during the preparation of the natural complex extract, the fabric was prepared according to a conventional method.

Comparative Example 4

In the preparation method of Example, when preparing PLGA resin containing natural complex extract, PLGA having different LA:GA ratio and molecular weight (Manufacturer: Purac Biomaterials, LA:GA=50:50, molecular weight: 7000-17000 Da) was used After the yarn production in substantially the same manner as in Examples, except for, the fabric was prepared according to a conventional method.

Comparative Example 5

PLA resin (manufacturer: Shimadzu, molecular weight: 80,000-90,000 Da), PCL resin (manufacturer: Union Carbide, molecular weight: 1,500 to 3,000 Da), natural complex extract, and PLGA resin mixture are put into the extruder, and the temperature of 200 to 230 ℃ was heated to melt. Then, after extruding the stirred mixture, it was cooled to 55 to 65° C. through a cooler, and the cooled extrudate was cut to prepare a pellet-type master batch chip, and using the master batch chip, the examples and The yarn and fabric were prepared in substantially the same way.

Here, compared to 100 parts by weight of the resin mixed with PLA and PCL, the natural complex extract and the PLGA resin mixture were mixed in an amount of 30 parts by weight. The weight ratio of PLA:PCL is 1:1.3, and the weight ratio of the natural complex extract and PLGA resin mixture is 3:7.

Comparative Example 6

In the manufacturing method of the embodiment, when the master batch chip is manufactured, the base mixed resin is cooled to a temperature of 150 to 180° C. through a cooler, and the PLGA resin containing the prepared natural extract is mixed, followed by stirring for 30 minutes except that Then, yarns and fabrics were prepared in substantially the same manner as in Examples.

Experimental Example 1. Antibacterial test

Whether the eco-friendly fiber yarn of the present invention has antibacterial properties was measured using the KS K 0693 test method, which is an antibacterial activity test of fibers.

Specifically, the fabrics of Examples and Comparative Examples were sterilized with a high-temperature autoclave, 1 x 10 ⁷ pieces of Staphylococcus aureus were inoculated, and after culturing for 18 hours, bacteriostatic bacteria compared to standard comedones The reduction rate of % was measured and shown in Table 1. Here, the Staphylococcus aureus is one of the representative bacteria that intensify the symptoms of atopic dermatitis and is known to easily multiply in textiles such as clothes, shoes, and bedding.

Antibacterial (%) Example 99.9 1 in comparison 90 Comparative Example 2 92 Comparative Example 3 87 Comparative Example 4 96 Comparative Example 5 35 Comparative Example 6 60

As can be seen from the above table, the fabric of Examples prepared by the manufacturing method of the present invention exhibited excellent antibacterial properties of 99.9%.

In contrast, in Comparative Examples 1 to 3 using a natural extract alone, and Comparative Example 4 using PLGA having a PLA:PGA ratio and molecular weight different from those of Examples in the preparation of PLGA including a natural complex extract, antibacterial properties were exhibited, The antibacterial activity of the examples did not reach.

On the other hand, in the case of Comparative Examples 5 and 6, in which some changes were made in the method for producing an eco-friendly fiber yarn of the present invention, it was confirmed that the antibacterial activity was significantly reduced compared to the Example.

In addition, the fabric of Example was washed 20 times, sterilized with a high-temperature and high-pressure sterilizer, 1 x 10 ⁷ pieces of Staphylococcus aureus were inoculated, and then cultured for 18 hours, compared with standard cotton cloth. The reduction rate of bacteria was measured in % and shown in Table 2.

Antibacterial (%) Example 99.7

As can be seen in the table above, the fabric of the embodiment exhibits high antibacterial activity even after washing 20 times, so it can continuously provide antibacterial activity to clothes compared to the conventional method of imparting antibacterial activity by a method such as a coating that lowers the antibacterial activity after washing. confirmed that there is.

Experimental Example 2. Tensile strength and tearing strength

Tensile strength refers to the value obtained by dividing the maximum tensile load until fracture of the specimen by the cross-sectional area of the specimen before the test in a tensile test of a material. The larger the value, the higher the strength of the material. It is the ratio of the initial length to the break length.

Tear strength refers to the numerical quantification of the durability against tearing of sheet-like materials such as fabric or film. It is a testing machine that calculates the force required to The higher the tear strength measurement value, the less likely the fabric will be torn.

Methods for measuring physical properties and experimental results for fabrics manufactured using the yarns of Examples are shown in Table 3 below.

Experimental method Result (unit: N) before washing The tensile strength KS K 0520 140 tear strength KS K 0536 18 after washing
(20 episodes) The tensile strength KS K 0520 138 tear strength KS K 0536 14

As can be seen from the above table, the fabrics of Examples exhibited good tensile strength and tearing strength above the recommended standards (tensile strength: 110 N, tear strength: 7 N) that fabrics that can be used for clothing and the like should have.

In addition, even after washing 20 times, the fabrics of Examples exhibited good tensile strength and tear strength, which is higher than the recommended standards that fabrics that can be used for clothes and the like should have.

This can be seen as a significant solution to the durability problem of existing biodegradable clothing.

Experimental Example 3. Sensory Test

After preparing a cotton (20 count) blend fabric containing the yarn prepared in the above example in a weight ratio of 15%, sensory evaluation was performed on clothes manufactured using the fabric, and as a control, the yarn was not included. Clothes made of cotton (20 counts) were used.

In consideration of age and gender, a total of 20 men and women in their teens to 40s were selected, 5 for each age group.

The sensory evaluation items are softness, breathability, comfort, and drape (flexibility), and the result is calculated using a 5-point scoring method (5 points: very good, 4 points: good, 3 points: average, 2 points: bad, 1 point: very bad) was used, and the results are shown in Table 4 below as an average value.

Soft breathable comfort drape Example 4.75 4.65 4.5 4.3 control 3.4 3.85 3.85 3.4

As shown in the table above, in the case of clothing manufactured using the cotton blend fabric including the yarns of Examples, excellent evaluations of 4 or more in softness, breathability, comfort and drape were obtained, which were manufactured using only cotton fabrics. In the case of clothing, it is in contrast to the evaluation of 4 points or less in all of softness, breathability, comfort and drape.

This means that the fabric using the eco-friendly fiber yarn manufactured by the manufacturing method of the present invention can be usefully used as a clothing product.

Claims (14)

An eco-friendly fiber yarn manufacturing method comprising the steps of:
S1) PLA (Poly Lactic Acid) resin and PCL (Polycaprolactone) resin is put in an extruder, heated to a temperature of 200 to 230 ℃ to melt to prepare a base mixed resin;
S2) cooling the molten base mixed resin to 150 to 180 ℃;
S3) mixing the cooled base mixed resin with a polylactide-co-glycolide (PLGA) resin containing a natural complex extract, and then stirring the mixture for 1 to 3 minutes;
S4) after extruding the stirred mixture, cooling to 55 to 65 ℃;
S5) cutting the cooled extrudate to prepare a master batch chip in the form of pellets; and
S6) manufacturing a yarn using the master batch chip. According to claim 1,
PLA and PCL of the step S1 is an eco-friendly fiber yarn manufacturing method that is included in a weight ratio of 1:0.8 to 1:1.8. The method of claim 1,
The natural complex extract is an eco-friendly fiber yarn manufacturing method comprising extracts of Hwangchil tree, Duchung tree, and Hobak tree. 4. The method of claim 3,
The natural complex extract is an eco-friendly fiber yarn manufacturing method prepared by a manufacturing method comprising the following steps:
a) pulverizing hwangchil wood, duchung wood, and spruce wood;
b) mixing the pulverized hwangchil wood, duchung wood, and spruce wood;
c) adding 80% (v/v) ethanol to the mixture and extracting at 60 to 80° C. for 8 hours;
d) filtering the obtained extract to separate a filtrate and a residue;
e) adding purified water to the residue separated in step d) and sonicating while continuously stirring at 60 to 80° C. for 8 hours using an ultrasonic extractor;
f) filtering the obtained extract to separate a filtrate and a residue; and
g) mixing the filtrate separated in steps d) and f). 5. The method of claim 4,
In the step b), hwangchil wood, duchung wood, and squash wood are mixed in a weight ratio of 1:1:1, an eco-friendly fiber yarn manufacturing method. delete According to claim 1,
The PLGA resin containing the natural complex extract is an eco-friendly fiber yarn manufacturing method that is manufactured through the following manufacturing method:
x) dissolving the natural complex extract and PLGA in an organic solvent;
y) adding the prepared solution to 1% PVA aqueous solution, followed by stirring; and
z) evaporating the organic solvent with a magnetic stirrer to solidify PLGA to obtain PLGA containing a natural complex extract. The method of claim 1,
The PLGA is an eco-friendly fiber yarn manufacturing method having a molecular weight of 50000 to 75000 Da. delete 8. The method of claim 7,
In step x), the natural complex extract is 0.1 to 40% by weight, and the PLGA 60 to 99.9% by weight is mixed in an eco-friendly fiber yarn manufacturing method. The method of claim 1,
The master batch chip is an eco-friendly fiber yarn manufacturing method comprising 30 parts by weight of PLGA resin containing a natural complex extract compared to 100 parts by weight of the base mixed resin. Claims 1 to 5, claim 7, claim 8, claim 10 or claim 11, eco-friendly textile fabric manufactured using the yarn manufactured by any one of the manufacturing method. 13. The method of claim 12,
The eco-friendly fiber fabric is an eco-friendly fiber fabric having antibacterial properties and biodegradability. A clothing product manufactured using the eco-friendly textile fabric of claim 12.