WO2012105810A2 - Antibacterial synthetic fiber, and method for manufacturing same - Google Patents

Abstract

The present invention relates to an antibacterial synthetic fiber manufactured by selecting one or more antibacterial plant extracts, mixing the plant extracts and a polymeric material for forming fibers, and melt-spinning the mixture at a temperature of 200 to 300°C. The antibacterial synthetic fiber of the present invention may exhibit both very superior as well as continuous antibiotic action. In addition, the physical properties of the antibacterial synthetic fiber of the present invention are superior to those of conventional antibacterial synthetic fibers, and are thus very suitable for materials for general clothing.

Description

Antimicrobial Synthetic Fiber and Manufacturing Method Thereof

The present invention relates to an antimicrobial synthetic fiber, and more particularly, to an antimicrobial synthetic fiber containing a plant extract and a method for producing the same.

Various attempts have been made to impart antimicrobial properties to synthetic fibers. The main species were to include antimicrobial inorganic materials in synthetic fibers, and the inorganic materials used were elvan, jade, mica and silver nanoparticles. However, these inorganic materials do not give the desired level of antimicrobial properties because they act as a hinder in the manufacturing process of the fiber, and they can only be used in small amounts. Especially in the case of silver nanoparticles known to have excellent antimicrobial effects, Nanoparticles have a problem that the color changes by adversely affecting the light fastness of the fiber after the dyeing process of the fiber.

In addition, even if the use of a small amount of the conventional antimicrobial synthetic fiber due to the inorganic materials used has a problem that the physical properties are worse than the general synthetic fiber.

In order to solve this problem, there have been many attempts to use plant extracts or essential oils having antimicrobial properties.

Representative examples thereof include a method in which plant extracts having antimicrobial properties are directly applied to synthetic fibers and fixed, such as Korean Patent Registration No. 10-0726409 and Korean Patent Registration No. 10-0515808. However, the synthetic fiber produced in this way has a problem in that the applied plant extract does not continuously exert an effect because it is detached during washing.

In order to solve the above problems, methods of including plant extracts or essential oils in synthetic fibers have been steadily sought.

The present inventors also attempted to prepare a master batch chip by adsorbing the wood vinegar to porous mineral particles in order to obtain a deodorizing effect, such as Patent Publication No. 2000-0058680, but because most of the wood vinegar component is water and viscosity The production of master batch chips for a variety of reasons, such as agglomeration of mineral particles used when mixing the mineral particles with the particles, causes clogging of the filter of the master batching facility, decomposition by moisture, and lowering of the viscosity of the polymer. Was not possible.

When moisture is added to the mineral particles, aggregation of the mineral particles occurs, and it is impossible to prevent them. The aggregated mineral particles harden into agglomerates as they are dried. In this state, it cannot be used, and in order to reuse it, it is necessary to repeat the fine grinding with a pin mill or jet mill for a long time to make it to the desired level of granularity and to disintegrate the fine grinding to prevent reaggregation of particles.

* Although it is possible to reuse the aggregated mineral particles through such a complicated process, the production cost is greatly increased due to too much cost in the fine grinding and crushing process.

In addition, as already mentioned, minerals have a bad effect on the physical properties of the fiber, so even after such a complicated process, the physical properties of the obtained fiber is still poor.

Since the melting temperature of the conventional synthetic fiber for fiber is 200 ~ 300 ℃ the plant extract or essential oil added before the melt spinning has a problem that the volatilization, decomposition, deterioration, etc. is impossible to manufacture or the performance is not sufficiently exhibited.

As a method for solving the above problems there may be mentioned the electrospinning method disclosed in Korean Patent No. 10-0910241. This patent discloses one or more components selected from (a) vegetable natural extracts and vegetable natural essential oils, (b) one or more fiber-forming polymers, and (c) the (a) and (b) components to lower the spinning temperature. Disclosed is a method of electrospinning a spinning solution in which a solvent capable of dissolving is mixed.

The principle of electrospinning is that the solution discharged through the nozzle is converted into a jet stream by the electric force formed between the collector and the nozzle, and the solvent is volatilized after the solvent contained in the jet stream reaches the incomplete region to form pure nanofibers. By this technology, problems with all the prior arts have been mostly solved. However, the fiber obtained by this method has a problem of low mechanical properties because it is difficult to obtain strength improvement through molecular orientation of the polymer itself. For this reason, the fiber obtained by the electrospinning method can not be used as a material for clothing, it is limited to only industrial special use.

In addition, the electrospinning method has a disadvantage in that a drop or bead frequently occurs during spinning, so that the process is not stable, and the production cost is very high while the production amount is very small.

One solution to the above problem is the method published in US 2010/0221969 A1. It discloses a method in which a vegetable essential oil is added to a microcapsule and then mixed with a polymer material and spun before spinning for the purpose of imparting the aroma function of the fiber. However, in this method, the microcapsule itself lowers the physical properties of the fiber. Especially during melt spinning of the synthetic resin, the material inside the microcapsule may be eluted in a high temperature and high pressure environment where the polymer material is melted and spun up to the point where it is spun. In this case, there is a big problem that can adversely affect the physical properties of the polymer material to cause abnormalities in the manufacturing process.

It is an object of the present invention to provide an antimicrobial synthetic fiber containing an antimicrobial plant extract. Another object of the present invention is to provide a synthetic fiber having a continuous antimicrobial. Still another object of the present invention is to provide a synthetic fiber having excellent antimicrobial reproducibility. Still another object of the present invention is to provide an antimicrobial synthetic fiber that can be used as a material for clothing.

The method for producing antimicrobial synthetic fibers of the present invention is characterized in that the antimicrobial plant extracts are contained in a fiber-forming polymer material, followed by melt spinning in a conventional manner.

The method of incorporating the extract of the antimicrobial plant into the fiber-forming polymer material includes (i) a method of melt spinning the chip obtained by coating and drying the antimicrobial plant extract on a synthetic chip, and (ii) adding a plant extract. After the production of the master batch chip and mixing with the master batch chip alone or synthetic resin chip, melt spinning method, (iii) method of adding the antimicrobial plant extract during the polymerization step and the like.

Hereinafter, the present invention will be described in detail.

Antibacterial plants are very diverse, and most plants have antibacterial properties with varying degrees.

The antimicrobial plants listed below are examples and in the present invention, all plants having antimicrobial properties may be used even if not illustrated below.

Camphoraceae, cypressaceae, pineaceae, cedar, arboraceae, green tea, Camellia, juniper, medicinal herbs, Herbaceae, Oleaceae, Ginkgo, Honeysuckle, Camphoraceae, Linaceae, Poaceae, Plant extracts extracted from leaves, stems, flowers, roots, fruits, or seeds, such as Rhododendron, Liliaceae, Lotus Leaf, Lamiaceae, Asteraceae, Oak and Sumac, and sap and sap from trees are widely antibacterial. Known.

As mentioned above, various methods such as electrospinning have been attempted to prevent the active ingredient of the plant extract from being pyrolyzed or degraded.

However, the inventors have confirmed that the active ingredient of the plant extract does not completely decompose or deteriorate even through ordinary melt spinning. Even if the active ingredient of the plant extract is partially pyrolyzed or degraded, if some remain and exert antimicrobial properties, it is very useful industrially and this fact has been clarified by the present inventors.

Part of the active ingredient remaining means that part of the active ingredient remains intact and that some components of the active ingredient remain. For example, when the product is dried for a long time at high temperature and subjected to high temperature melt spinning and dyeing process, the unique flavor of plant extract is lost, but the antibacterial property is maintained as it is.

In the present invention, the plant extract refers to a plant leaf, flower, stem, root, sap, sap, fruit, seeds or the like boiled with water to extract the active ingredient or extracts obtained by cooling and condensing the smoke generated when burning the plant, etc. Means.

In the extract extracted by boiling water in the antimicrobial plant, water is removed in a drying process or a master batch manufacturing process, and an active ingredient having a pharmacological action is present in the fiber. Impurities such as solids and the like are filtered out. The extract should be sufficiently concentrated and preferably concentrated by heating until the weight is reduced to 25 to 60% or less, more preferably 30 to 50%, of the material (antibacterial plant) and water added. If the degree of concentration is less than this, a lot of flammable volatiles remain in the extract liquid, making the continuous process difficult, and the physical properties of the obtained fiber are also very poor. If the degree of concentration is higher than this, the viscosity becomes too high and workability is inferior, and deterioration of the material occurs due to excessive concentration. Preferable extraction temperature is 110-150 degreeC, More preferably, it is 120-130 degreeC. If it is below this range, the extraction efficiency is insufficient, and if it exceeds this range, there is no further increase in extraction efficiency, and the risk of the process increases due to the high pressure generated during extraction.

The ratio of the weight of the material (antibacterial plant) and the water used for the first time is a ratio of 1: 2 to 5 as in the case of conventional herbs.

Powders obtained by extracting the active ingredient of the plant with a solvent, then drying and pulverizing, or powders obtained by drying and pulverizing the plant itself cannot be used in the present invention. Not only is it difficult to obtain the desired level of fine powder, but it is also severely degraded or burned during drying or melt spinning before spinning. When the added plant powder burns down, the viscosity of the synthetic resin decreases drastically, and spinning itself becomes impossible.

Based on the plant extract, the appropriate content is 0.01 to 10.0% by weight, more preferably 0.05 to 6.0% by weight, more preferably 0.1 to 3.0% by weight. If it is less than this range, the effect of the input is insufficient, even if it exceeds this range there is no further effect improvement and adversely affect the physical properties of the fiber.

The production method of the present invention is to melt-spun in a conventional manner by containing 0.01 to 10% by weight, preferably 0.05 to 6.0% by weight, more preferably 0.1 to 3.0% by weight of the extract of the antimicrobial plant in the fiber-forming polymer material It is composed.

As described above, a coating method, a master batch method, a polymerization method, or the like may be used as a method of containing the extract of the antimicrobial plant in the fiber-forming polymer material.

In the coating method, in order to prevent deterioration of the plant extract, it is preferable to dry using low temperature drying or rotary hot air drying equipment.

Synthetic fiber of the present invention prepared by the above manufacturing method contains 0.01 ~ 3.0% by weight of the active ingredient of the antimicrobial plant extract or wood vinegar, has an excellent antimicrobial activity of more than 90% bacterial antibacterial rate over 18 hours.

The antimicrobial synthetic fiber of the present invention exhibits very good antimicrobial properties and at the same time continuously exerts antimicrobial properties. In addition, it is excellent in physical properties than the conventional antimicrobial synthetic fiber is very suitable as a general medical material, non-woven fabric or industrial material, and also can be effectively used as a diaper for infants or patients because the antimicrobial properties persist even after repeated washing and excellent skin diseases and anti-allergic effects. On the other hand, even when used as bristles will exhibit excellent antibacterial effect.

1 is a comparative photograph of the control and test pieces 18 hours after inoculation.

(Production Example 1)

* Preparation of duct bridge concentrate

Put 2Kg of pulverized crushed powder into PP non-woven bag and put 8Kg in the pressure bath, add 20Kg of water, boil at 130 ℃ for 3 hours, pressurize in hydraulic press to obtain 15Kg of extract, and pass it through 5 micron filter twice and concentrate it to 5Kg. Filtered concentrate was prepared.

This step was repeated to prepare 65 Kg of filtered concentrate.

(Production Examples 2-4)

* Preparation of Gold Coin, Ginkgo Leaf and Cinnamon Concentrate

Filtration, ginkgo biloba leaves, cinnamon peel was prepared in the same manner as in Preparation Example 1 to obtain a filtered concentrate.

(Production Examples 5-8)

2 wt% of each extract obtained in Preparation Examples 1 to 4 was mixed with a polypropylene chip, and dried at 60 ° C. for 2 hours using a rotary hot air dryer to prepare a coated chip.

2Kg of the coating chip was used to spin a conventional spinning method at a spinning temperature of 225 ° C. with a pilot spinning machine to produce 150 denier 28 filament yarns.

(Production Example 9)

3 wt% of the extract obtained in Preparation Example 1 was mixed with nylon chips and dried at 60 ° C. for 3 hours using a rotary hot air dryer to prepare 50 Kg of coated chips. The obtained coating chip was mixed with a general nylon chip in a ratio of 1: 1, and dried in a conventional manner, and then spun at a spinning temperature of 235 ° C. in a pilot spinning machine to prepare nylon filament yarn of 150 denier 28 filaments.

(Production Example 10)

2 wt% of the filtered oak vinegar solution was mixed with a polypropylene chip and dried at 60 ° C. for 3 hours using a rotary hot air dryer to prepare 50 kg of coated chips. The coated chip was spun using a conventional manufacturing method at a spinning temperature of 225 ° C. using 2 Kg alone to produce 150 denier 28 filament yarns.

(Production Example 11)

65Kg of duct bridge extract concentrate prepared in Preparation Example 1 and 700Kg of polyester crushed chips were mixed and pre-dried to melt-extrude at a melting temperature of 285 ° C in a master batch equipment (Twinscrew Germany W & P) to prepare 620Kg of masterbatch chips. . This master batch chip and a conventional polyester chip with an average intrinsic viscosity of 0.64 were mixed and spun at a weight ratio of 1: 7 to produce 4,080Kg of 1.4D and 38mm staple fibers.

Spun the fibers to produce 40S / 1 yarn (spun yarn), knit S / J knitting, refine it in a high-pressure dyeing machine, dye it, shop, process absorbent softeners, and then go through the tenta process to produce a conventional yarn. Obtained a specimen.

(Examples 1-8)

The filament yarns prepared according to Production Examples 5 to 10 were prepared in the form of a sock. As a result of performing antimicrobial experiments on the knitted fabric and the specimen obtained according to Production Example 11, the total antimicrobial activity was passed for 18 hours as shown in Table 1 below. This was very good at over 90%. The test method was as follows.

Test Method: Compliant with KS K 0693-2006

About the specimen obtained by Preparation Example 11 was further tested for antimicrobial activity against MRSA bacteria, which are super bacteria, the test results are shown in Table 2 below, and the test conditions are as follows. The comparative photograph of the control piece and the test piece 18 hours after the inoculation is shown in FIG. 1.

Test species: Staphy lococcus aureus (MRSA) ATCC 33591

* Concentration of inoculum fluid: 1.2 × 10 ⁵ CFU / mL CFU

* Contrast: Standard cotton cloth

* Nonionic surfactant: Tween80, 0.05% added to inoculum

Table 1

division	Test species	Antibacterial rate
Preparation Example 5 (Compass)	Staphylococcus aureus ATCC 6538 (Staphylococcus aureus)	99.9% or more
	Klebsiella pneumonia ATCC 4352	99.9% or more
Preparation Example 6 (Gold and Silver Coins)	Staphylococcus aureus ATCC 6538 (Staphylococcus aureus)	99.7%
	Klebsiella pneumonia ATCC 4352	99.1%
Preparation Example 7 (Ginkgo biloba leaves)	Staphylococcus aureus ATCC 6538 (Staphylococcus aureus)	98.3%
	Klebsiella pneumonia ATCC 4352	92.1%
Preparation Example 8 (Cinnamon)	Staphylococcus aureus ATCC 6538 (Staphylococcus aureus)	99.9% or more
	Klebsiella pneumonia ATCC 4352	99.9% or more
Preparation Example 9 (Compass)	Staphylococcus aureus ATCC 6538 (Staphylococcus aureus)	99.4%
	Klebsiella pneumonia ATCC 4352	99.9% or more
Preparation Example 10	Staphylococcus aureus ATCC 6538 (Staphylococcus aureus)	99.9% or more
	Klebsiella pneumonia ATCC 4352	99.9% or more
Preparation Example 11 (Compass)	Staphylococcus aureus ATCC 6538 (Staphylococcus aureus)	99.9% or more
	Klebsiella pneumonia ATCC 4352	99.9% or more
	Staphylococcus aureus (MRSA) ATCC 33591	99.9% or more

[Revision under Rule 91 03.07.2012]
TABLE 2

 (Comparative Example 1)

The single jersey knitting fabric knitted with polyester 40s / 1 spun yarn was dehydrated and dried after refining dye shopping in a high pressure dyeing machine. Subsequently, 5% by weight of the soft-leaved extract obtained in Preparation Example 1 was mixed with water (95% by weight) to which a softening agent was added, the fabric was immersed therein, passed through a mangle, and a sample was obtained through a tenter process.

The sample before washing showed 99.9% antimicrobial activity, but after 5 washes, the antimicrobial activity was significantly reduced to 34% or less.

(Comparative Example 2)

5 Kg of porous mineral particles were mixed with 20 L of wood vinegar, and aggregation of the mineral particles occurred. For melt spinning, 2% by weight of mineral powder adsorbed with wood vinegar was mixed with polyester chip and dried for 6 hours at a temperature of 130 ~ 160 ° C. After drying, the aggregated mineral particles became agglomerated in a hardened state. No further process could proceed.

Claims (9)

1. A method for producing antimicrobial synthetic fibers by melt spinning in a conventional manner by containing 0.01 to 10% by weight of at least one selected from the water extraction solution or wood vinegar of the antimicrobial plant in the fiber-forming polymer material.
2. The method of claim 1, wherein the method of containing at least one material selected from the water extract or wood vinegar of the antimicrobial plant in the fiber forming polymer material comprises adding the at least one material selected from the extract or wood vinegar of the antimicrobial plant to the fiber forming polymer material before melt spinning. Method for producing an antimicrobial synthetic fiber, characterized in that the coating method.
3. The method of claim 1, wherein the method of containing the fiber-forming polymer material with at least one material selected from the water extract or wood vinegar of the antimicrobial plant comprises mixing the at least one material selected from the water extract or wood vinegar of the antimicrobial plant with the fiber-forming polymer material. Method for producing an antimicrobial synthetic fiber, characterized in that the method for producing a master batch chip.
4. The method of claim 1, wherein the method for containing the fiber-forming polymer material with at least one material selected from water extracts or wood vinegar of the antimicrobial plant comprises polymerizing the fiber-forming polymer material with at least one material selected from the water extract or wood vinegar solution of the antimicrobial plant. Method for producing an antimicrobial synthetic fiber, characterized in that the method of adding.
5. The method for producing the antimicrobial synthetic fiber according to any one of claims 1 to 4, wherein the fiber-forming polymer material is a polymer material capable of melt spinning.
6. The method for producing an antimicrobial synthetic fiber according to any one of claims 1 to 4, wherein the product is melt-spun and molded for nonwoven fabric.
7. The plant according to any one of claims 1 to 4, wherein the plant having an antimicrobial activity includes camphor family, cypressaceae, pine family, cedar family, arboraceae, green tea family, camellia family, juniper family, plant family, herb family, Oleaceae, ginkgo. Method for producing antimicrobial synthetic fibers, characterized in that it comprises trees, honeysuckle, camphor, Linaceae, Poaceae, Unhyang, Liliaceae, Lotus Leaf, Lamiaceae, Chrysanthemum, Oak, Sumac .
8. An antimicrobial synthetic fiber prepared by the method of any one of claims 1 to 4, containing 0.01 to 3.0% by weight of an active ingredient of at least one selected from water extracts or wood vinegar solutions of the antimicrobial plant.
9. The antimicrobial synthetic fiber according to claim 8, wherein the microbial antimicrobial rate is at least 90% after 18 hours.

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