KR20130115851A - Atimicrobial fabric treatment composition using phytoncide oil and atimicrobial fabric treating method - Google Patents

Abstract

PURPOSE: An antibacterial phytoncide fiber treatment agent and an antibacterial treatment method are provided to show superior antibacterial properties and emulsification stability without harming the human body and to prevent a color change when the treatment agent is treated on a fiber. CONSTITUTION: An antibacterial phytoncide fiber treatment agent with improved emulsification stability contains phytoncide essential oil, an emulsifier, and alcohols in water. The weight of the alcohols is 1-2 times greater than the essential oil. The alcohol is ethyl alcohol. An antibacterial treatment method comprises the steps of: mixing the treatment agent and acryl-based binders; dipping a fiber or a fabric into the mixture; and heating the fiber or the fabric.

Description

Atimicrobial fabric treatment composition using phytoncide oil and Atimicrobial fabric treating method

The present invention relates to a phytoncide fiber antimicrobial agent and antimicrobial processing method that is harmless to human body, has excellent antimicrobial properties, has excellent emulsification stability even when left for a long time, and does not change in dyed color when processed to a textile fabric.

Recently, with increasing interest in the environment and health, the final product using natural fiber as a material is also being advanced and highly functionalized, and antimicrobial processing using natural extracts has also attracted attention in the field of fiber antibacterial processing. Currently, antimicrobial agents used in antimicrobial processing generally use synthetic antimicrobial agents, which are almost all irritating compounds, which can be potentially harmful to the human body, and also cause problems of environmental pollution during manufacturing and processing. On the other hand, when the antimicrobial agent of natural products is used, there is less anxiety of human stability, such as formaldehyde detection, than the synthetic material.

Natural antibacterial substances include chitosan or natural antimicrobial substances contained in essential oils extracted from plants. Especially, essential oils extracted from plants are referred to as phytoncide, which is used to protect trees from pests and microorganisms. It refers to a directional antibiotic released in the air for self defense.

Various attempts have been made to obtain deodorant and antimicrobial properties by using phytoncite essential oils in fibers and the like. For example, Patent Publication No. 2011-0048635 (Method for producing phytoncide microcapsules impregnated with nanoparticles), Patent Publication No. 2011-0001421 (fabric fabric containing multifunctional composite capsules and uses thereof), Publication No. 2010 -0046301 (Atopy preventive fiber composition and coating method thereof), Patent Publication No. 2007-0006295 (composition of eco-friendly fiber antimicrobial agent), Patent Publication No. 2005-0037740 (Textiles treated with microencapsulated phytoncide and its manufacturing method) , Patent No. 0964027 (Fiber manufacturing method containing cypress leaf extract) and the like.

In the case of the invention using the phytoncide microcapsules of the proposed inventions there is a problem that the antimicrobial effect is expressed only when the capsules are expelled by the skin friction, the laundry durability is not good due to the destruction of the capsule due to friction during washing In addition, there may be problems of formaldehyde detection in melamine-based resin, which is a raw material of microcapsules supporting cypress oil, and consumers may feel dissatisfaction due to different preferences of cypress oil.

In the case of the invention using a mixture of cyanoyl oil composition and silver nano, the bacteriostatic reduction rate is 99.9%, but the antimicrobial durability after 20 times or more washing is not presented, there is a problem in the durability of the laundry.

The present invention for solving such a conventional problem is harmless to the human body, excellent antimicrobial properties, excellent emulsification stability even if left for a long time, there is no change in dyeing color when processed in textile fabric, odor of phytoncide is not strong The object of the present invention is to provide a phytoncide fiber antimicrobial agent and an antimicrobial processing method which are excellent in antimicrobial properties even after washing 20 times or more.

According to an aspect of the present invention,

It provides an phytoncide fiber antimicrobial processing agent with improved emulsion stability, characterized in that the phytoncide essential oil, emulsifier and alcohol is mixed with water.

It is preferable that the alcohol is mixed 1 to 2 times with respect to the weight of the essential oil, and in particular, it is preferable to use ethyl alcohol as the alcohol.

The emulsifier is preferably mixed 1.5 times with respect to the weight of the essential oil, the emulsifier is HLB (Hydrophilic Lipophlic Balance) is preferably 14.7 or more.

In addition, the present invention provides an antimicrobial processing method characterized in that the fiber or fiber fabric is immersed in a mixture mixture of the phytoncide fiber antimicrobial processing agent and the acrylic binder is heated.

At this time, the acrylic binder is preferably used 5 to 10% by weight based on the weight of the fiber.

The phytoncide fiber antimicrobial processing agent of the present invention is harmless to the human body, has excellent antibacterial properties, has excellent emulsification stability even when left for a long time, there is no change in dyeing color when processed to the textile fabric, and the odor of the phytoncide is not strong, and consumers' rejection of the aroma is not. There is no, even after washing 20 times or more has an excellent antibacterial effect.

1 is a photograph taken after leaving the fiber antimicrobial agent of Examples 1-1 to 1-7 for 24 hours or more,
Figure 2 is a photograph taken after leaving the fiber antimicrobial agent of Examples 2-1 to 2-7 for 24 hours or more,
3 is a photograph taken after leaving the fiber antimicrobial agents of Examples 3-1 to 3-7 for 24 hours or more.
Figure 4 is an antimicrobial test report for the fabric treated with the phytoncide fiber antimicrobial processing agent of Examples 4-1 to 4-4.
5 is a fabric treated with phytoncide fiber antimicrobial agents at concentrations of 0% (a), 1% (b), 3% (c), 5% (d), 7% (e), and 10% (f) Shows the result of analysis by FT-IR.

Hereinafter, the phytoncide fiber antimicrobial processing agent having improved emulsion stability will be described in detail.

The phytoncide fiber antimicrobial processing agent having improved emulsion stability is made by mixing phytoncide, essential oil, emulsifier and alcohol in water.

The phytoncide essential oil is a phytoncide essential oil of the cypress of the cypress family known to have a high content of phytoncide, which is a natural antibacterial substance in the plant.

And the emulsifier is to improve the emulsion stability, such as to prevent the separation of the oil phase and the water phase even after a long time, and other ionic surfactants such as nonionic surfactants can be used, but the preparation of the preparation by the ionic reaction during post-processing It is recommended to use nonionic surfactants to minimize troubles due to aggregation.

Since the emulsifier is not high in viscosity of the processing agent, it is preferable to mix 1.5 times with respect to the weight of the phytoncide essential oil in order to easily stir and improve the emulsion stability.

In particular, the HLB (Hydrophilic Lipophlic Balance) of the emulsifier is preferably 14.7 or more. When the HLB of the emulsifier is 14.7 or more, the experimental results showed the optimum emulsification stability for phytoncide essential oil.

In addition, the alcohol is used to help micelle formation in the emulsification process of the phytoncide essential oil and to enhance the stability of the micelles produced. A primary or secondary alcohol such as ethylene glycol, propylene glycol, methyl arool, ethyl alcohol, etc. may be used. Can be.

The alcohol is preferably used 1 to 2 times the weight of the phytoncide essential oil in order to lower the viscosity and effectively improve the micelle formation and the stability of the micelle during the emulsification process to prevent foaming.

After the fiber fabric is immersed in the blended mixture of the phytoncide fiber antimicrobial processing agent and the binder having improved emulsion stability of the present invention, the fiber fabric can be subjected to antimicrobial post-processing.

At this time, the type of the binder is not particularly limited, but an acrylic binder may be used. In particular, the binder is preferably used 5 to 10% by weight based on the weight of the fiber in order to maintain high washing durability and antibacterial properties. If the binder is mixed at less than 5% by weight, there is a fear that the laundry durability is lowered, and if the binder is mixed at more than 10% by weight, the fabric may be stiff.

And when the antimicrobial post-processing treatment may be used in combination with a fiber antimicrobial agent, a binder. As the softener, Anion softener, Cation softener, Nonion softener and the like can be used. When mixing the softening agent, it is good to determine and use it well so that trouble does not occur according to the type of binder. For example, when an acrylic binder, which is an anionic binder, and a Cation softener are used together, an ionic reaction occurs, and a trouble occurs between the acrylic binder and the Cation softener.

Hereinafter, the phytoncide fiber antimicrobial processing agent with improved emulsification stability of the present invention will be described in detail with reference to Examples. The scope of the present invention is not limited to the following Examples.

Example 1

The emulsion stability test according to the change of the HLB of the emulsifier was mixed with oil, emulsifier and water as shown in Table 1 to prepare a fiber antimicrobial processing agent.

At this time, the oil was phytoncide essential oil (ECOMIST CO., LTD), the emulsifier was used a non-ionic surfactant (PROTEXKOREA CO., LTD).

A phytoncide essential oil, an emulsifier, water and ethanol were added in the ratios shown in Table 1 below, followed by agitation at 50 or more, followed by stirring at 10,000 RPM for 10 minutes using a Homogenizer to prepare a fiber antimicrobial agent.

Example
1-1 Example
1-2 Example
1-3 Example
1-4 Example
1-5 Example
1-6 Example
1-7 oil weight% 10 10 10 10 10 10 10 Emulsifier
weight% 10 10 10 10 10 10 10 HLB 10 12.6 13.7 14.7 15 16 17 water weight% 80 80 80 80 80 80 80 Gross weight% 100 100 100 100 100 100 100

In order to confirm the emulsion stability according to the change in the HLB of the emulsifier, the prepared fiber antimicrobial agent was left at room temperature for at least 24 hours to check the stability.

After leaving for 24 hours or more, photographs taken of the fiber antimicrobial agents of Examples 1-1 to 1-7 are as shown in FIG. 1. As a result of standing for 24 hours as shown in Figure 1 the layer separation occurred under all conditions. In addition, a lot of agitation problems and bubbles due to the viscosity rise during the test process.

[Example 2]

And unlike Example 1, a fiber antimicrobial agent was prepared by mixing oil, emulsifier, water and alcohol as shown in Table 2. Alcohol was used as Ethyl Alcohol (99.9%) (SAMCHUN PURE CHEMICAL CO., LTD).

Example
2-1 Example
2-2 Example
2-3 Example
2-4 Example
2-5 Example
2-6 Example
2-7 oil weight% 10 10 10 10 10 10 10 Emulsifier
weight% 10 10 10 10 10 10 10 HLB 10 12.6 13.7 14.7 15 16 17 water weight% 60 60 60 60 60 60 60 Alcohol weight% 20 20 20 20 20 20 20 Gross weight% 100 100 100 100 100 100 100

In order to confirm the emulsion stability according to the use of alcohol and the change in the HLB of the emulsifier, the prepared fiber antimicrobial agent was left at room temperature for at least 24 hours, and then the stability was confirmed.

After leaving for at least 24 hours, the photograph of the state of the fiber antibacterial agent of Examples 2-1 to 2-7 is shown in FIG. 2. As a result of standing for 24 hours as shown in FIG. 2, the layer separation occurred under all conditions, but the problem due to the viscosity increase during stirring was eliminated and no bubbles were generated.

[Example 3]

Unlike Example 2, the amount of the emulsifier was increased to 15% by weight to prepare a fiber antimicrobial agent by mixing oil, emulsifier, water and alcohol as shown in Table 3.

Example
3-1 Example
3-2 Example
3-3 Example
3-4 Example
3-5 Example
3-6 Example
3-7 oil weight% 10 10 10 10 10 10 10 Emulsifier
weight% 15 15 15 15 15 15 15 HLB 10 12.6 13.7 14.7 15 16 17 water weight% 55 55 55 55 55 55 55 Alcohol weight% 20 20 20 20 20 20 20 Gross weight% 100 100 100 100 100 100 100

In order to confirm the emulsion stability of the fiber antimicrobial agent of Example 3, the prepared fiber antimicrobial agent was left at room temperature for at least 24 hours, and then the stability was confirmed.

After leaving for 24 hours or more, the photographs of the fiber antimicrobial agents of Examples 3-1 to 3-7 are taken as shown in FIG. 3. In the case of HLB 14.7 or more as shown in Figure 3 it can be confirmed that the emulsification was made stably without separation.

In the above experiments, the stability of emulsification according to the change of HLB was determined to be the optimum emulsification stability of phytoncide oil, emulsifier, and alcohol in the ratio of 1: 1.5: 2 under HLB 14.7.

Example 4 Post-processing of Cotton Fiber Fabric

In order to evaluate the antimicrobial activity of the phytoncide fiber antimicrobial agent of Example 3-4, a test was carried out on a standard white cotton cloth. 3%, 5%, 7% and 10% solutions were prepared and treated to the fabric. In addition, acrylic binders (SNOTEX AR 4260, DAE YOUNG CHEMICAL CO., LTD) are used in the same way as the concentration of the processing agent to act as a binder between the fiber and the processing agent to increase the durability when processing the textile antimicrobial processing agent on the cotton fabric. owf 3%, 5%, 7%, 10% were added. Standard white cotton cloth was immersed in the solution prepared under the above conditions, and padding was performed at 100% pick-up rate, and then treated with a Mini-tenter for 60 sec at a temperature of 160 ° C.

In order to examine the antimicrobial properties of the fabrics treated with each concentration by treating the fiber antimicrobial agent on the cotton fabric, the durability test was also conducted by testing the antimicrobial properties after the presentation and washing 20 times based on KS 0693. Staphylococcus aureus and Klebsiella pneumoniae (pneumococcus) were used in this study.

In order to increase the durability of the fiber antimicrobial processing agent obtained through the emulsification stability test of the cypress essential oil, the antibacterial test and the durability test of the antibacterial test and the laundry durability test were carried out by treating the standard white cotton cloth with the acrylic binder in each of the above conditions. As shown, the antimicrobial activity was higher than 99.9% at the concentration of 5% or more of owf, and the durability was 99.9% or higher at the concentration of 5% or more of owf. On the other hand, the antimicrobial test report for the fabric treated with the phytoncide fiber antimicrobial processing agent of Examples 4-1 to 4-4 is as shown in FIG.

fiber
Antimicrobial Processing Agent Acrylic
bookbinder Fungus Before washing 20 times after washing
Example 4-1

3%

3%
Staphylococcus
aureus 99.7 99.8 Klebsiella
pneumoniae 99.9 99.9
Example 4-2

5%

5%
Staphylococcus
aureus 99.9 99.9 Klebsiella
pneumoniae 99.9 99.9
Example 4-3
7%

7%
Staphylococcus
aureus 99.9 99.9 Klebsiella
pneumoniae 99.9 99.9
Example 4-4

10%

10%
Staphylococcus
aureus 99.9 99.9 Klebsiella
pneumoniae 99.9 99.9

[FT-IR Analysis]

FT-IR was measured to observe whether the fabrics treated with the phytoncide fiber antimicrobial treatment agents of Examples 4-1 to 4-4 were used, and the Avatar 370 equipment of Thermo nicolet was used.

5 is a fabric treated with phytoncide fiber antimicrobial agents at concentrations of 0% (a), 1% (b), 3% (c), 5% (d), 7% (e), and 10% (f) Shows the result of analysis by FT-IR.

In comparison with the untreated standard white cotton (a), after the phytoncide essential oil treatment, the absorption peak by carbonyl group, which was not seen in the untreated white cotton cloth, was found around 1720 cm-1 (frequency). It can be judged that the antimicrobial agent is bound to cotton fabric by physical and chemical reactions.

[Evaluation of Color Change after Treatment of Dyestuffs]

In order to find out the color change when dyed cotton fabric was treated with cypress essential oil processing agent, the color difference before and after treatment was measured by treating the extract after the reaction dyeing under the following conditions.

Reactive dyes used for cotton fabric dyeing were Sunfix® supra Red S3B, Sunfix® supra Yellow S3R 150% and Sunfix® supra Blue SBR from OHYOUNG IND, CO, .LTD (KOREA). Was used as is

5g standard white cloth was dyed at 60 ° C. for 60 minutes under a bath ratio of 10: 1 using a reactive dye 1.0% owf, followed by soaping and washing with water. At this time, Na ₂ CO ₃ 10g / L, Na ₂ SO ₄ 30g / L was used.

Processed acrylic binder (SNOTEX AR 4260, DAE YOUNG CHEMICAL CO., LTD) to act as a binder between fiber and processing agent to increase durability when processing textile antimicrobial processing agent on cotton fabrics reacted with each color. 3%, 5%, 7%, and 10% of owf standards were added in the same manner as the concentrations of. Standard white cotton cloth was immersed in the solution prepared under the above conditions, and padding was performed at 100% pick-up rate, and then treated with a Mini-tenter for 60 sec at a temperature of 160 ° C.

Table 5 shows the results of measuring the color change before and after treatment by treating the fiber antimicrobial treatment agent to the concentration of cotton fibers dyed with a reactive dye.

Dye Conc of
finishing
agent (%)

Color value Color difference
(ΔE) L a b
sunfix ^? supra
Red s3b
untreated 54.22 55.49 -6.03 - One 54.39 55.41 -6.20 0.26 3 54.33 55.80 -6.53 0.61 5 53.83 56.30 -5.96 0.90 7 54.09 55.97 -6.61 0.77 10 53.67 56.44 -6.42 1.17
sunfix ^? supra
Yellow s3r
150% untreated 78.71 19.08 67.36 - One 78.32 18.87 66.95 0.60 3 78.34 18.81 67.90 0.71 5 78.45 18.71 66.73 0.77 7 78.71 18.52 68.02 0.87 10 78.63 18.31 67.98 1.00
sunfix ^? supra
Blue SBR untreated 54.31 -3.74 -27.30 - One 54.49 -3.49 -27.21 0.32 3 54.16 -3.46 -27.74 0.55 5 53.57 -3.58 -27.27 0.77 7 53.28 -3.53 -27.85 1.19 10 53.33 -3.50 -27.88 1.17

As shown in Table 5, even when the textile fabrics treated with reactive dyes were treated with fiber antimicrobial agents at concentrations of 1, 3, 5, 7, and 10%, they showed little or no color difference ΔE or less than 1.20. It is hard to feel the change of color. It is believed that this is practically possible for cotton fabrics dyed with common reactive dyes.

Claims (7)

Phytoncide fiber antimicrobial processing agent with improved emulsion stability, characterized in that the phytoncide essential oil, emulsifier and alcohol is mixed with water.
The method of claim 1,
The alcohol is phytoncide fiber antimicrobial processing agent with improved emulsion stability, characterized in that 1 to 2 times mixed with the weight of the essential oil.
3. The method of claim 2,
The alcohol is phytoncide fiber antibacterial processing agent with improved emulsion stability, characterized in that ethyl alcohol.
3. The method of claim 2,
The emulsifier is phytoncide fiber antimicrobial processing agent with improved emulsion stability, characterized in that 1.5 times with respect to the weight of the essential oil.
3. The method of claim 2,
The emulsifier is phytoncide fiber antimicrobial processing agent with improved emulsion stability, characterized in that the HLB (Hydrophilic Lipophlic Balance) is 14.7 or more.
The antimicrobial processing method characterized by heating after immersing a fiber or a fabric material in the compound liquid which mixed the phytoncide fiber antimicrobial processing agent of any one of Claims 1-5, and an acrylic binder.
The method of claim 1,
The acrylic binder is an antimicrobial processing method, characterized in that 5 to 10% by weight based on the weight of the fiber.

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