KR20040014957A - Anti-bacterial fiber and anti-bacterial processing method - Google Patents

Abstract

Antimicrobial activity is provided by processing bamboo vinegar liquor into fibers without accompanying yellowing, hardening of the touch, and exploitation.

Description

Anti-bacterial fiber and anti-bacterial processing method

Wood vinegar (木 酢 液) extracted from various trees is known to have an excellent antibacterial action. In particular, bamboo vinegar extracted from bamboo material contains substances having antibacterial action such as fatty acids such as acetic acid, phenols, and lower alcohols.

Cloth products using the antibacterial action of bamboo vinegar include:

Japanese Unexamined Patent Application, First Publication No. Hei 9-176965 discloses a cloth product or a paper product characterized by impregnating a liquid collected when making activated carbon from bamboo material.

Japanese Patent Laid-Open No. 10-131057 discloses a textile product characterized by adhering a sustained release carrier of fine particles impregnated with bamboo vinegar with a binder.

However, bamboo vinegar produced by the prior art is a by-product produced when making activated carbon and is a liquid collected as a drain of steam, and is usually treated at a carbonization temperature of 400 ° C to 600 ° C. For this reason, some of the active ingredient is decomposed, and the bamboo vinegar itself has a yellowish color.

Moreover, since processing at high temperature, a part of components polymerize and a tar phase component is produced, and there exists a problem that the touch after processing becomes hard.

Furthermore, there was a problem that the carbon odor at the time of carbonization of bamboo vinegar does not disappear after processing.

On the other hand, in order to solve the above problems, there is a method of purifying bamboo vinegar by distillation, etc., but it is not a practical method because it takes a lot of time and money.

The present invention relates to a fiber and an antimicrobial processing method that gives antimicrobial activity using bamboo vinegar (竹 酢 液).

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a diagram for explaining how to collect bamboo vinegar.

2 is a diagram illustrating another method of collecting bamboo shoot liquor.

3 is a diagram illustrating another method of collecting bamboo liquor.

An object of this invention is to provide antimicrobial property by processing bamboo vinegar liquid into a fiber, without accommodating yellowing, hardening of a touch, and exploitation which were a problem in the prior art.

The present invention imparts antibacterial properties by processing bamboo vinegar liquor into fibers. Bamboo vinegar liquid used in the present invention is put bamboo bamboo in an external heating furnace that cuts off the air supply, 95 ℃ to 300 ℃, preferably 95 ℃ to 280 ℃, more preferably It is obtained by heating at a relatively low temperature of 95 ° C to 110 ° C to condense the smoke (gas) discharged from the furnace. For the collection of such bamboo vinegar liquor, for example, an external heat furnace disclosed in Japanese Patent Application No. 2000-328709 (filed October 27, 2000) can be used. Here, the external heat furnace refers to a furnace of a type in which a filler (in this case, bamboo ash) in a furnace does not naturally heat by heating from the outside. The heating source is not limited. In addition, by blocking the supply of air, bamboo ash does not spontaneously cause thermal decomposition. By maintaining at said relatively low temperature, generation | occurrence | production of a tar component is prevented and thermal decomposition of the component which exhibits antibacterial effect is suppressed.

Bamboo liquor made by the prior art is a by-product of making activated carbon and is a liquid collected as a drain of steam, and is usually treated at a carbonization temperature of 400 ° C to 600 ° C. As a result, the bamboo vinegar itself has a yellowish color, and also smells of bamboo. In addition, it contains a tar-like component, and when processed into fibers, antimicrobial properties are imparted, but there are many other problems.

On the other hand, the external heat type is intended to collect bamboo vinegar solution, and since bamboo is treated at relatively low temperature to collect bamboo vinegar solution, there is no yellowing and no carbonization or polymerization of the active ingredient occurs. Also, there is little smell of bamboo burned.

The fiber processed with this bamboo vinegar solution is an antibacterial material that does not have a smell that occurs during yellowing or carbonization of bamboo and maintains the original feel of the material.

According to the present invention, it was confirmed that there was no yellowing of the cloth and no exploitation of the cloth by processing the fiber with bamboo vinegar, and an antibacterial material in which the original feel of the material was maintained was obtained.

Examples of the state of the textile product which can be used in the present invention include, but are not limited to, a cotton block, a sliver shape, a filament, a woven fabric, a knit fabric, a nonwoven fabric, a filter, a sewing product, and the like.

In the fibrous material which can be used in the present invention, the cellulose fibers include natural cellulose fibers such as cotton and hemp, regenerated cellulose fibers such as viscose rayon, East Ammonia method rayon and polynostic, and refined cellulose fibers such as tencel. Semisynthetic fibers such as acetate, diacetate, and the like, but are not limited thereto. Animal fibers include wool fibers such as wool and cashmere, silk, and the like, but are not limited to these. Synthetic fibers include polyester, polyamide, acrylic, polyvinyl chloride, polyvinylidene chloride, polyethylene, polypropylene, polyurethane, polyvinyl alcohol, fluorine, and the like. no. The regenerated fiber includes chitin chitosan fiber, collagen fiber and the like, but is not limited thereto.

The filamentous fibrous material that can be used in the present invention includes, but is not limited to, spun yarn of single fiber or blended yarn of multiple fibers, multi-layered yarn, and the like. In the case of regenerated cellulose fibers, semisynthetic fibers, synthetic fibers, and regenerated fibers, long fibers (filaments) may be used, spun yarns may be used, and plural fibers may be mixed.

As a processing method in the present invention, an aqueous solution containing bamboo vinegar is prepared and the fiber is impregnated with it. Impregnation can use any method, such as a conventionally known immersion method, a pad method, a spray method, and a coating method. Moreover, you may use binders, such as a suitable crosslinking agent and resin, for the purpose of improving washing durability. The bamboo vinegar solution may be encapsulated in a microcapsule made of a substrate such as polyurethane or cyclodextrin, and then fixed to the fiber with a binder. In addition, bamboo vinegar may be added to regenerated cellulose fibers, semisynthetic fibers, synthetic fibers, and regenerated fibers.

The bamboo vinegar liquid used in the present invention can express excellent antibacterial property by providing 0.1% by weight to 10.0% by weight, preferably 0.3% by weight to 5.0% by weight, based on the weight of the fiber to be processed. At 0.1 wt% or less, there is an initial effect but low washing durability, and more than 10.0 wt% is not preferable in terms of cost.

Hereinafter, the present invention will be described in more detail with reference to examples, which are not intended to limit the scope of the invention set forth in the claims.

a. Collection of Bamboo Vinegar

Example 1 (FIG. 1)

Bamboo liquor was extracted using an external heat-cut furnace that cuts off the air supply. As bamboo shoots, 8 kg of undehydrated and undried Mengjongjuk was used to obtain 2470 bamboo shoots in 9 hours after the furnace was lit. The fuel of the furnace was a gas, and the temperature in the furnace was maintained at around 250 ° C on average. The change of the yield accompanying the passage of time at that time is shown in FIG. The numbers on the line represent the yield per hour. The smoke from the furnace is cooled to extract bamboo liquor, and water vapor from the first bamboo ash begins to emerge. About 1 hour after the fire, bamboo vinegar began to be extracted. Bamboo shoot liquor was extracted at about 350 kPa per hour for 3 to 6 hours after ignition. Yields began to decrease after 6 hours of ignition and decreased to 200 kPa after 9 hours of ignition, so extraction was stopped at this point. The extracted bamboo vinegar solution was colorless and transparent, and almost no tar component was confirmed.

Example 2 (FIG. 2)

Bamboo liquor was extracted using an external heat-cut furnace that cuts off the air supply. As a bamboo ash, using 175.5 kg of undehydrated blind bamboo (= bamboo shoots), 19580 ml of bamboo vinegar was obtained 24 hours after the furnace was lit. If you use a ring burner consisting of four concentric burners as the heat source, if you call it Burner 1, Burner 2, Burner 3 and Burner 4 from the center outwards, first burn all burners and After the passage of time, the burner was turned off once at about 95 ° C and the furnace was kept at about 105 ° C. After 11 hours, all other burners were turned off. The change in temperature and yield over time is shown in FIG. 2. In Fig. 2, the mark indicates temperature and the mark indicates yield. The broken line portion of the temperature line is speculative. As shown in Fig. 2, droplets start to fall off from 2 hours after burner ignition. From the beginning it was possible to obtain a transparent and burnt smell. After 3 hours, it became a drop image, and it flowed out continuously after that. After about 7 hours, the yield increased rapidly and 500 ml was extracted in 10 minutes. After 10 hours, yields began to decline to 460 ml in 10 minutes. At the time of turning off all the burners, the amount reached 16055 ml, and the extraction continued after turning off, and after 24 hours, the total extraction amount was 19580 ml. The extracted bamboo vinegar was colorless and transparent, and no tar component was found. On the other hand, about 2 liters remained at the bottom of the furnace.

Example 3 (FIG. 3)

Bamboo liquor was extracted using an external heat-cut furnace that cuts off the air supply. About 23 liters of bamboo vinegar solution was obtained 24 hours after the furnace was turned on using 172.355 kg of dead bamboo shoots (= bamboo shoots) which were not cut and dried as bamboo ash. Using a concentric ring burner of four burners as a heat source, if you call it Burner 1, Burner 2, Burner 3 and Burner 4 from the center outwards, the first one will ignite and burn about 4.5 The burner was turned off at about 95 ° C after the passage of time, the burner 1 was re-ignited after 7 hours, and the furnace was kept at about 100 ° C by adjusting the burner of burner 4 after 10 hours. did. At 11.5 hours, all other burners were turned off. 3 shows changes in temperature and yield over time. In Fig. 3,? Indicates temperature, and? Indicates yield. The dashed portion of the yield curve is speculative. As shown in FIG. 3, droplets began to fall from about 1.5 hours after burner ignition. After 3 hours, it became a drop image, and it flowed continuously continuously after that. At about 4.5 hours, 500 ml of extraction was carried out in 20 minutes. About 20 liters were reached when all burners were turned off, and the extraction continued after turning off, and the total extraction amount was about 23 liters after 24 hours. The extracted bamboo vinegar was colorless and transparent, and no tar component appeared. In addition, about 4 liters remained at the bottom of the furnace.

b. Example

Example 1

Immerse the following formulations in a cotton broadcloth (thread thickness: 50 warp yarn single yarn, 50 weft yarn single yarn, fabric density: 144 warp yarn / inch, 78 warp yarn / inch) And tightened with mangle to 60% tightening rate. Then, after drying for 2 minutes at 130 degreeC, curing was performed for 1 minute at 160 degreeC. There was no yellowing of the cloth after processing, and no exploitation. In addition, the texture of the fabric was almost unchanged from before processing.

Drug combination composition

Bamboo vinegar solution (collected by the method described in a. Above): 1% by weight

Glyoxal Resin [Brand Name "Benkamin DC-W"

(Japan Nippon Ink Industry Co., Ltd.)]: 10% by weight

Resin Catalyst [Brand Name "Sumitex Accelerator X-80"

(Sumitomo Chemical Co., Ltd.): 2% by weight

Water: 83 wt%

c. Comparative example

A drug was blended and processed under the same conditions as in Example, except that 1% by weight of a commercially available bamboo vinegar solution (manufacturer's sales agency: Nippon Oriental Medicine Research Institute) was used. This commercially available bamboo vinegar solution is dark yellow as the conventional bamboo vinegar liquid generally, and the smell of acetic acid and tar was confirmed. After processing, yellowing and exploitation of the fabric were observed. In addition, the touch of the cloth became hard.

d. Antibacterial test

The antimicrobial property was evaluated about the cloth processed by the Example and the comparative example. The results are shown in Table 1.

TABLE 1

Bactericidal activity Staphylococcus aureus Pneumonia MRSA Micro Tak 10 times of washing Micro Tak 10 times of washing Micro Tak 10 times of washing Example 1.97 1.97 1.86 1.86 2.03 2.03 Comparative example 1.97 -1.21 0.97 -0.96 0.34 -1.76

The antimicrobial test was carried out in accordance with JIS L 1902 (antimicrobial test method for textile products), and the bactericidal activity value was calculated by measuring the number of bacteria after washing and washing ten times.

Test bacteria were Staphylococcus aureus ATCC 6538P, pneumococcal bacillus ( Klebsiella pneumoniae ATCC4352), and methicillin resistant Staphylococcus aureus (MRSA). The washing method used JIS L 0217 103 method, and the detergent used JAFET standard detergent (designated detergent of the New Product Evaluation Council for Textiles).

If the bactericidal activity value is 0, it indicates that the number of bacteria after 18 hours of incubation is the same number as the initial number of bacteria. In addition, when it exceeds 0, it shows the number of bacteria reduced, and when it is less than 0, it shows that the number of bacteria increased. Therefore, the greater the bactericidal activity, the higher the antimicrobial effect.

The Examples had a high antibacterial effect in both unwashed and washed 10 times, whereas the Comparative Example had a lower antimicrobial effect than the Staphylococcus aureus at the stage of micro-washing, and the antibacterial effect was obtained by washing. Disappear.

Example 2

(a) Preparation of microcapsules

① According to Japanese Patent No. 1813429 (Method for producing hollow inorganic particulate), a. A porous hollow inorganic spherical fine particles having a mean particle size of 0.5 µm containing 50% by weight of bamboo shoot liquid collected by the method described in Example 1 (trade name: "Godball: 鈴木 油脂 工業 (製)") were prepared.

(2) A porous hollow inorganic spherical fine particle (trade name "Godball: 鈴木 油脂 工業") was prepared in the same manner except that the average particle size was about 0.3 µm.

(3) Porous non-porous inorganic material having an average particle diameter of about 0.5 µm in which 50% by weight of bamboo vinegar solution collected by the above method was carried out according to Japanese Patent No. 1882225 (Method for producing porous silica microspheres). Spherical fine particles (brand name "Godball: 鈴木 油脂 工業 (株) 製)" were created.

(b) cloth processing

The following compound is immersed in cotton broad cloth (thickness of yarn: single yarn with 50 warp yarns, single yarn with 50 weft yarns, and fabric density: 144 yarns / inch warp, 78 yarns / inch weft) . Then, after drying at 130 degreeC for 2 minutes, it cured at 155 degreeC for 2 minutes. After processing, there was no yellowing of the fabric and no exploitation. In addition, the touch of the cloth was almost unchanged from before processing.

Drug formulation composition

(1) Inorganic spherical fine particles (trade name "Godball", 鈴木 油脂 工業 (:)): 1% by weight

Binder (Brand Name: "NK Binder KM", Shin-Gion Chemical Co., Ltd.): 12% by weight

Water: 87 wt%

(2) Inorganic spherical fine particles (trade name "Godball", 鈴木 油脂 工業 (:)): 2% by weight

Binder (Brand Name: "NK Binder KM", Shin-Gion Chemical Co., Ltd.): 12% by weight

Water: 86 wt%

(3) Mineral spherical fine particles (trade name "Godball", 鈴木 油脂 工業 (:)): 3% by weight

Binder (Brand Name: "NK Binder KM", Shin-Gion Chemical Co., Ltd.): 12% by weight

Water: 85 wt%

(c) antibacterial test

Antimicrobial activity was evaluated about the processed cloth. The results are shown in Table 2.

TABLE 2

Mineral globular fine particles Particulate amount (% by weight) Bactericidal activity Micro Tak 10 times of washing ① One 0.15 0.06 2 0.44 0.28 3 1.21 1.10 ② One 0.73 0.41 2 0.99 0.46 3 1.35 1.21 ③ One 0.08 0.04 2 0.37 0.11 3 0.88 0.31

The antimicrobial test was carried out in accordance with JIS L 1902 (antimicrobial test method for textile products), and the microbial count and the number of bacteria after 10 washes were measured, and bactericidal activity values were calculated.

Test bacteria were used Staphylococcus aureus ATCC 6538P. The washing method used JIS L 0217 103 method, and the detergent used JAFET standard detergent (designated detergent of the New Product Evaluation Council for Textiles).

When the bactericidal activity value is 0, it indicates that the number of bacteria after 18 hours of cultivation is the same as the number of initial bacteria. In addition, when it exceeds 0, it shows the number of bacteria decreased, and when it is less than 0, it shows that the number of bacteria increased. Therefore, the larger the bactericidal activity value, the higher the antimicrobial effect.

In the embodiment according to the present invention, after 10 times of washing and washing, all had a high antibacterial effect.

Claims (8)

An antimicrobial fiber formed by adhering bamboo ash to an external heat furnace that cuts off air and heating it to 95 ° C. to 300 ° C., and attaching the fiber to the fiber using bamboo vinegar obtained by condensing the gas discharged from the furnace. The antimicrobial fiber according to claim 1, wherein the heating temperature of the furnace is in the range of 200 ° C to 280 ° C. The antimicrobial fiber according to claim 1, wherein the heating temperature of the furnace is maintained for a predetermined time within a range of 95 ° C to 110 ° C. The antibacterial fiber of any one of Claims 1-3 which provided 0.1 weight%-10.0 weight% of bamboo vinegar solution with respect to the weight of the fiber to process. An antimicrobial processing method characterized by adhering bamboo shoots obtained by adding bamboo ash to an external heating furnace that cuts off air and heating them at 95 ° C to 300 ° C, and condensing the gas discharged from the furnace. The antimicrobial processing method according to claim 5, wherein the heating temperature of the furnace is in the range of 200 ° C to 280 ° C. The antimicrobial processing method according to claim 5, wherein the heating temperature of the furnace is maintained for a predetermined time within a range of 95 ° C to 110 ° C. The antibacterial processing method according to any one of claims 5 to 7, wherein 0.1 wt% to 10.0 wt% of bamboo vinegar is added to the weight of the fiber to be processed.