WO2011155807A2

WO2011155807A2 - Antibacterial synthetic fiber and method for producing same

Info

Publication number: WO2011155807A2
Application number: PCT/KR2011/004312
Authority: WO
Inventors: 석명호
Original assignee: Seok Myung-Ho
Priority date: 2010-06-11
Filing date: 2011-06-13
Publication date: 2011-12-15
Also published as: WO2011155807A3

Abstract

The present invention relates to an antibacterial synthetic fiber which is produced by selecting one or more antibacterial plant extracts, mixing the extracts and a polymeric material for producing fiber, and melt-spinning the mixture at the temperature of 150 to 300°C. The antibacterial synthetic fiber of the present invention exhibits significantly superior and continuous antibacterial property. In addition, the antibacterial synthetic fiber of the present invention has physical property more excellent than those of conventional antibacterial synthetic fibers, and therefore, is exactly appropriate for producing general clothing.

Description

[Correction 12.10.2011] by Rule 26 (26) Antibacterial synthetic fiber and its manufacturing method

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

Various attempts have been made to impart antimicrobial properties to synthetic fibers. Its main species was to include antimicrobial inorganic materials in synthetic fibers, and the inorganic materials used were elvan, jade, and silver nanoparticles. However, since these inorganic materials act as an obstacle in the manufacturing process of the fiber, they cannot be used in trace amounts, so they do not exhibit the desired level of antimicrobial properties. Especially in the case of silver nanoparticles known to have excellent antimicrobial effects, in addition to the above problems, silver nano used There is a fatal problem that the particles change color after dyeing the fibers.

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.

However, the melting temperature of the conventional synthetic fiber for the production of synthetic fibers from the polymer material is 220 ~ 300 ℃, the melting temperature of the polyacrylonitrile-based synthetic fibers vary depending on the manufacturing method, but usually at a temperature of 150 ~ 170 ℃ Since it is melt spinning, plant extracts or essential oils injected before melt spinning have a problem that volatilization, decomposition, deterioration, and the like are not sufficiently exerted.

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 to form pure nanofibers after the solvent contained in the jet stream reaches the incomplete region. 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.

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. 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.

One aspect of the method for producing antimicrobial synthetic fibers of the present invention is coated on the surface of the synthetic resin with at least one selected from antimicrobial plant extracts, oils or powders (hereinafter referred to as "antibacterial plant extracts"), and then dried and conventional It is spinning by melt spinning method. Another aspect of the production method of the present invention is to prepare a master batch chip by adding an antimicrobial plant extract and melt spinning it alone or mixed with a conventional synthetic resin chip. Another aspect of the production method of the present invention is to add the antimicrobial plant extracts before the polymerization of the synthetic resin, and then melt spinning by a conventional production method through a polymerization production process.

Another aspect of the production method of the present invention is to melt-spin the conventional antimicrobial plant extracts with a fiber-forming polymer material in a conventional manufacturing method.

Hereinafter, the present invention will be described in detail.

Antibacterial plants are very diverse.

The antimicrobial plants listed below are merely exemplary and include all antimicrobial plants, although not illustrated below.

Camphoraceae, cypressaceae, pineaceae, cedar, arboraceae, green tea, camellia, juniper, medicinal herbs, herb, oleaceae, ginkgo, sterling, cinnamon, flax, linaceae It is widely known that plant extracts from the leaves, stems, roots, and seeds of fruits, berries, and the like, Poaceae, Rheumaceae, Liliaceae, Lotus Leaf and Lamiaceae have excellent antimicrobial properties.

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.

Plant extract refers to a plant leaf, stem or root, fruit, seeds, etc. boiled with water or extracted with a solvent such as alcohol or hexane, concentrated or powdered, extracted with oil, or using a grinding device. Powder and the like obtained.

Appropriate methods may be adopted depending on the type of plant to be covered. For example, in case of Yeongyo, it is appropriate to extract by boiling with water. It is appropriate to extract the oil by pressurization.

When the powdery extract is used, it is difficult to obtain fine powder due to the characteristics of the plant, and the powdery extract used is not only susceptible to deterioration due to heat, but also in the manufacturing process, it is easy to cause abnormalities such as trimming. Is inadequate and can only be applied to the production of coarse fibers such as duvets or industrial yarns.

In addition, when extracting by boiling water with an antimicrobial plant or extracting using a solvent, most of the extracts are water or volatile components such as alcohol or hexane, and thus are removed from additional heating and other drying processes. Ingredient. Impurities, such as solids, are filtered out and extracted by pressurization, depending on the plant used.

Based on plant extracts, the appropriate content is 0.01 to 10.0% by weight, more preferably 0.05 to 6.0% by weight, even more preferably 0.1 to 5.0% 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.

One aspect of the manufacturing method of the present invention is 0.01 to 10% by weight of the antimicrobial plant extract, preferably 0.05 to 6.0% by weight, more preferably 0.1 to 5.0% by weight to the synthetic resin chip and coated and then dried sufficiently after the usual It is composed of melt spinning by the method.

However, this method is poorer in physical properties than the fibers obtained in comparison with the masterbatch method described later, and thus can be applied in the case of relatively thick fine fibers such as quilting fibers, but is unsuitable for the production of fine fine fibers like clothing fibers.

Another aspect of the production method of the present invention is to obtain a master batch chip containing a high concentration of plant extract and then mixed with the master batch chip alone or a general synthetic resin chip content of the plant extract is 0.01 ~ 10% by weight, preferably 0.05 ~ 6.0 weight%, More preferably, it mixes so that it may become 0.1 to 5.0 weight%, and melt-spins by a conventional method. The physical properties of the fibers obtained by this method are superior to those by the coating method described above, and thus can be suitably used for the production of fine fine yarns for textiles.

In another method, the plant extract is added in an amount of 0.01 to 10% by weight, preferably 0.05 to 6.0% by weight, more preferably 0.1 to 5.0% by weight, prior to polymerization of the fiber-forming polymer, and the polymerization is completed by a conventional method. Then, this polymer is melt-spun in a conventional manner. In this case, the added plant extract may be a liquid or powder.

Another aspect is to melt-spin by conventional manufacturing methods by mixing 0.01 to 10% by weight of plant extracts, preferably 0.05 to 6% by weight, more preferably 0.1 to 5% by weight with a fiber-forming polymer material. This method is suitable for spinning of polyacrylonitrile-based fibers.

Synthetic fiber containing a plant extract more than the above range is improved water absorption to 30mm or more based on the ks k 0815.6.27.1:2008B method for 10 minutes, and if the water absorption is improved, the antimicrobial activity is further improved. There are various methods of increasing the absorbency, and a known method for producing absorbent fibers may be adopted.

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 a continuous 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

2kg each of duct bridge crushed powder was placed in a PP nonwoven fabric bag, 8Kg was placed in a pressure bath, 20Kg water, boiled at 130 ° C for 3 hours, pressurized in a hydraulic press to obtain 16Kg of extract, and passed through a 5 micron filter twice and concentrated to 4Kg. Filtered concentrate was prepared.

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

(Production Examples 2 to 3)

* Preparation of Gold Coin and Ginkgo Biloba Concentrate

Gold silver coins and ginkgo biloba were prepared in the same manner as in Preparation Example 65 to prepare a filtered concentrate 65Kg.

(Production Example 4)

* Preparation of Flaxseed Oil Extract

Flaxseed 480 Kg was extracted from the milking machine with 152 Kg of oil, and then passed through a 5 micron filter twice to obtain 140 kg of filtered oil.

(Production Example 5)

* Preparation of Cinnamon Bark Fine Powder

A sufficiently dried cinnamon bark was first pulverized and then finely pulverized in a bead mill to prepare 400 Kg of fine powder having an average particle diameter of 50% or less and 1% or less and 99% or less.

(Production Examples 6-9)

* Manufacture of coated chips

12Kg of each extract obtained in Preparation Examples 1 to 4 was mixed while spraying onto 300Kg of polyester chips, and dried at a temperature of 150 ° C. for 3 hours to prepare chips coated with plant extracts.

(Production Examples 10-13)

* Preparation of polyester filament yarn

The coated chip prepared in Preparation Examples 6-9 and the general polyester chip were mixed at a ratio of 1: 4, dried at a temperature of 185 ° C. in a Pyrod drier for 3 hours, and then spun in a Pyrod spinner to 150 denier. Filament yarn of 28 filaments was prepared.

(Production Example 14)

* Preparation of staple fiber for quilting cotton

400Kg of cinnamon powder obtained in Preparation Example 5 was mixed with 3,600Kg of polyester crushed chip having an intrinsic viscosity of 0.80, mixed and melt-extruded to prepare a master batch chip, which was a ratio of 1: 4 with a polyester chip having an intrinsic viscosity of 0.64. After mixing for 2 hours at 185 to melt spinning and then through the stretching and post-processing to prepare a staple fiber for 7 denier 51mm duvet cotton.

(Examples 1-5)

The filament yarns obtained in Production Examples 10 to 13 were woven into socks, and the results of the antimicrobial tests on the knitted fabric and the staple fibers obtained according to Production Example 14 were as follows. The antibacterial rate was over 90% and the antimicrobial activity was very good. Test methods were as follows.

* Sample name: 1 point for each knit fabric and staple fiber

* Test Method: Compliant with KS K 0693-2006

Table 1

(Example 6)

65Kg of duct bridge extract concentrate prepared in Preparation Example 1 and 650Kg of polyester shredding chip were added in a rotary mixer and mixed for 50 minutes, and then melted at 285 ° C in a twin screw master batch facility (W & P, Germany) using a 300 mesh filter. The master batch chip was extruded to obtain 619 Kg, and the master batch chip and the conventional polyester chip having an intrinsic viscosity of 0.64 were mixed and spun at a ratio of 1: 7 in weight ratio to prepare 4,080 Kg of staple fiber having 1.4 D and 38 mm. .

Spun the fibers to produce 40s / 1 yarn, knit S / J knitting, refine it in high pressure dyeing machine, dye it, and soap it, process the absorbent softener, and then go through the tenter process to prepare the specimen by the usual manufacturing method. Got it.

After washing 5 times with the obtained specimens, the antimicrobial test results were obtained as in Example 1 (antibacterial rate of 99.9% or more), and the results of the test for antimicrobial activity against the MRSA bacteria, super bacteria, as shown in Table 2 below. 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

[Revision 12.10.2011 under Rule 26]
TABLE 2

The results of testing the absorption rate with the same sample are shown in Table 3 below.

[Revision 12.10.2011 under Rule 26]
TABLE 3

(Comparative Example)

The single jersey knitting fabric knitted with polyester 40s / 1 spun yarn was refined and dyed in a high pressure dyeing machine and then dehydrated and dried to immerse in a solution mixed with 95% by weight of water and 5% by weight of ductile extract obtained in Preparation Example 1 with a softener. After passing through the mangle and processing through a tenter step to obtain a sample.

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

(Example 7)

* Manufacture of nylon filament yarn

300 kg of a master batch chip was prepared by precisely mixing 4% by weight of filtered flaxseed oil and 96% by weight of nylon chips.

The antimicrobial master batch chip: general nylon chip was mixed so that the ratio of 1: 1 and dried at 90 for 4 hours to obtain a filament yarn of 150 denier 28 filament at a melting temperature of 230 ℃ by a conventional manufacturing method.

The filament yarn obtained was woven in the shape of a sock, and the antimicrobial test results were the same as in Example 5.

(Example 8)

* Manufacture of polypropylene filament yarn

In the same manner as in Example 7, polypropylene chips were mixed instead of nylon chips and spun at a melting temperature of 225 without undergoing drying to obtain 150 denier filament yarns of 28 filaments. The filament yarn obtained was woven in the shape of a sock, and the antimicrobial test results were the same as in Example 5.

(Example 9)

* Manufacture of Acrylic Fiber Staple Fiber

2% by weight of flaxseed oil was added and melt spun by a conventional polyacrylonitrile manufacturing method, followed by a post-cutting process to prepare a 3 denier staple fiber. The obtained staple fibers were spun with theta yarn and dyed to prepare a knitted fabric, which was then tested for antimicrobial activity as in Example 5.

(Example 10)

* Addition of plant extracts during polymerization

1% by weight of flaxseed oil was added to the initial stage of the ester reaction during the polyester polymerization, and then polymerized by a conventional method at a polymerization temperature of 290 ° C. to prepare a polyester chip, followed by a drying process. 2,000 kg of 100d / 48f FY yarn were spun.

The obtained FY yarn was knitted with a single jersey and dyed, and then the antimicrobial test was performed.

(Example 11)

* Extraction of plant extracts using solvents and yarn production

1 kg by weight of dried cinnamon powder and 10 parts by weight of hexane were mixed and stirred, and the container was sealed. After 24 hours, the solvent was removed, and then 50 kg of water was added to 15 kg of the extract obtained by stirring, and the extract was filtered through a 5 micron filter. 750 Kg of a polyester crushed chip having a viscosity of 0.80 was mixed with a screw mixing mixer, followed by preliminary drying at 100 ° C. for 1 hour to remove water, and then melt extrusion to prepare a master batch chip. The obtained masterbatch chip and polyester chip having an intrinsic viscosity of 0.64 were mixed at a ratio of 1: 4, dried at 185 for 3 hours, and melt-spun in a pilot spinning machine to prepare 150 denier 28 filament yarns.

The antimicrobial test results of the filament yarn obtained were the same as in Example 5.

Claims

A method for producing an antimicrobial synthetic fiber, characterized in that the coating is mixed with 0.01 to 10% by weight of at least one selected from plant extracts, oil or fine powder with antimicrobial and mixed with a fiber-forming polymer material.
One or more substances selected from antimicrobial plant extracts, oils or fine powders are mixed with fiber-forming polymeric materials to produce a master batch chip, and then mixed with this chip alone or common synthetic resin chips in plant extracts, oils or fine powders. Method for producing an antimicrobial synthetic fiber, characterized in that the melt spinning so that the content of at least one selected from 0.01 to 10% by weight.
0.01 to 10% by weight of at least one selected from plant extracts, oils or fine powders having antimicrobial properties are added to the initial stage of the polymerization of the fiber-forming polymer material, and then prepared by a conventional polymerization method to melt spinning. Manufacturing method.
Preparation of antimicrobial synthetic fibers characterized in that the melt spinning by conventional polyacrylonitrile production method by mixing 0.01 ~ 10% by weight of at least one selected from plant extracts, oil or fine powder with antimicrobial with a fiber-forming polymer material Way.
The antimicrobial synthetic fiber according to any one of claims 1 to 4, wherein the fiber-forming polymer material comprises polyester, polyamide, polypropylene, polyacrylonitrile and polybutylene. Manufacturing method.
The method for producing an antimicrobial synthetic fiber according to claim 2 or 3, wherein the product is melt-spun and molded for nonwoven fabric.
The plant according to any one of claims 1 to 3, wherein the plant having an antimicrobial activity includes camphor family, cypressaceae, pine family, cedar family, arboraceae, green tea family, camellia family, juniper family, equipment family, herb family, Oleaceae, ginkgo. Method for producing antimicrobial synthetic fibers, characterized in that it comprises a tree, gold, cinnamon, linseed, Linaceae, Poaceae, Poaceae, Liliaceae, lotus leaf, Lamiaceae .
An antimicrobial synthetic fiber prepared by the method of any one of claims 1 to 4, containing 0.01 to 10% by weight of one or more substances selected from plant extracts, oils or fine powders having antimicrobial properties.
The antimicrobial synthetic fiber of claim 8, wherein the absorbency (ks k 0815.6.27.1:2008B method) is 30 mm or more for 10 minutes.