JP2001329463A - Method for antimicrobial treatment of textile products - Google Patents

Abstract

PROBLEM TO BE SOLVED: To impart a durable antimicrobial effect harmless to human and livestock to cellulosic textile products. SOLUTION: This method comprises pretreating cellulosic textile products by contacting them with a treatment liquid containing a metal salt having coordinate bond-forming ability and then immobilizing extracts from tea leaves on the fiber by contacting the pretreated textyle products with a treatment liquid containing catechins of the extracts from tea leaves.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to a processing method for producing a fiber product having excellent physiological activity such as antibacterial, antiviral and antiallergic properties using catechin of tea leaf extract.

[0002]

2. Description of the Related Art In recent years, natural consciousness has been called out, and especially for natural fiber products, antibacterial products using various natural extracts have been developed. A fiber product using catechin as one of natural antibacterial fiber products has attracted attention. The tea leaf extract contains catechins having various functions such as antibacterial properties in addition to pigments. Fiber products treated with this catechin are recognized for their harsh color tone, antibacterial properties, deodorant properties, etc., and are expected to be used in a wide range of applications. The following prior art is mentioned as an antibacterial processing method of catechin obtained by treating a fiber product with a tea leaf extract.

(1) JP-A-8-296173 A method of impregnating and fixing fibers with a tea leaf extract containing a tea leaf tannin as a main component together with a binder such as glyoxal resin or polyamide resin to produce antibacterial fibers. (2) JP-A-9-316786 A method of dyeing a textile product by bringing a textile product into contact with a mordant containing a mordant after contacting the textile with a dying solution of a catechin, or dyeing a textile using both a catechin and a mordant. A dyeing method for textiles in which dyeing and mordant are simultaneously carried out by contacting a liquid and a mordant. (3) As a method of fixing catechin to a fiber product, a cationized substance reactive with cellulosic fiber is reacted with -OH group in the fiber in the presence of alkali to form cationized cellulose, and then a compound having an anionic group And salt formation.

[0004]

In the above prior art,
To fix the tea leaf extract, those using a synthetic resin of glyoxal resin or polyamide resin as a fixing agent can be applied to a wide range of fibers, but the texture becomes hard and the tear strength is also reduced. . In addition, there is a disadvantage that formalin is detected.

[0005] In the above-mentioned prior art, a post-mordanting method in which a fiber product is brought into contact with catechins and then brought into contact with a mordant is also performed. Catechins fall off in the next step such as washing with water, and the proportion of catechins remaining in textiles is small. Therefore, there is a drawback that the amount of catechin adhered is limited and the amount of the catechin greatly fluctuates. In addition, the method of immobilizing catechins by contacting textiles with a dye / mordanting liquid containing both catechins and mordants is a method of fixing catechins and mordants in a treatment liquid, so that the catechins and mordants are bonded to the textile. And the hue becomes unstable.

[0006] In the above-mentioned prior art, after treating a textile with a cationizing substance such as quaternary aminoepichlorohydrin and then immobilizing catechins on the fiber, the hue becomes dark reddish brown. , And become unstable,
It has the drawback of significantly impairing the color developability, and is also significantly discolored by sunlight.

[0007]

SUMMARY OF THE INVENTION According to the present invention, a textile product is contacted with a treatment solution containing a metal salt having coordination binding ability, pretreated, and then contacted with a treatment solution containing catechins of tea leaf extract. Then, by coordinating and binding, the tea leaf extract is immobilized on the fiber to impart antibacterial properties.

Hereinafter, the present invention will be described in detail. The fiber product referred to in the present invention is a cellulosic fiber, that is, cotton,
Regenerated cellulose fibers such as hemp, wet cellulose fibers (rayon, cupra, polynosic fiber, etc.) and dry cellulose fibers (tencel, lyocell, etc.), and blends and interwovens of these fibers with synthetic fibers such as polyester fibers and semi-synthetic fibers , Knitted fabrics, knitted fabrics, nonwoven fabrics and yarns.

In the present invention, the metal salt having coordination binding ability is a water-soluble salt of a polyvalent metal, that is, a copper compound (for example, copper sulfate), a tin compound (for example, stannous chloride), a zinc compound (for example, Zinc chloride), chromium compounds (eg, potassium dichromate), antimony compounds (eg, tartar), iron compounds (eg, ferrous sulfate), aluminum compounds (eg, aluminum sulfate, aluminum acetate, alum,
Aluminum chloride, a sulfuric acid band, etc.). The catechins of the tea leaf extract referred to in the present invention are a part of the water-soluble components of the tea leaf extract, and 10 to 18 of the water-soluble components.
%, And has useful properties such as antioxidant action, antibacterial action, deodorant action, and antiviral action.

[0010] Tea catechins each contain four types of catechins having different structures.
Usually about 18% epigallocatechin, about 6% epicatechin,
About 54% of epigallocatechin galade and about 13% of epicatechin galade in total, about 90% in total. The catechin used in the present invention is a commercially available catechin preparation, which preferably contains 5% or more of epigallocatechin galade, and each of these catechins has 4 to 7 hydroxyl groups. Forms complex compounds with metal salts.

In the method of the present invention, first, a metal salt having a coordination binding ability, for example, an aqueous solution of aluminum sulfate (0.5 to 5.
0% by weight), and the cellulosic fiber product is immersed in this liquid. Next, a small amount of an alkaline compound, for example, sodium carbonate, is added thereto, and the mixture is left for a while. The metal salt gradually changes to hydroxide and is adsorbed in the fiber.

Next, when this fiber product is treated with a 0.1 to 5.0% by weight aqueous solution of catechins extracted from tea leaves, the metal hydroxide in the fiber and the catechins are distributed between the hydroxyl group of catechin and the metal ions. To form a water-insoluble complex compound.

[0013] A dyeing method for fixing a plastid extracted from a plant or the like on a fiber, which is conventionally called plant dyeing, is known. In this dyeing method, the plastid is attached to the fiber and then the dye is applied with a mordant. Means for immobilization are taken. However, in this method, it is difficult to sufficiently fix the catechins on the fibers, and desired antibacterial properties cannot be obtained. In addition, there is a method in which a plastid extracted from plants is treated with a mordant and the same bath to fix it on fibers. In this method, the catechins and the mordant react in the treatment bath and cannot be sufficiently immobilized on the fibers, so that desired antibacterial properties cannot be obtained. By taking the method of the present invention, the antibacterial property is improved for the first time, and dyeing can be suppressed.

The metal salt having coordination ability used in the treatment of the present invention is desirably used at a concentration of 0.5 to 5.0% by weight. If it is less than 0.5% by weight, it is difficult to immobilize catechins sufficiently by chelate bond, and it is difficult to make it 5.0% by weight.
It is difficult to increase the immobilization of catechins to a predetermined level or more, even if the above is used. On the other hand, the amount of catechins used in the tea leaf extract to be used is preferably 0.1 to 5.0% by weight. 0.1
If the amount is less than 5% by weight, the antibacterial property cannot be sufficiently exhibited, and if the amount is 5.0% by weight or more, the effect of the antibacterial property does not change, so that the production cost increases.

The pretreatment conditions for the compound having coordination binding ability are preferably at 40 ° C. to 60 ° C. for about 20 minutes to 40 minutes.
When the temperature is lower than 40 ° C., the compound having the coordination binding ability is not sufficiently adsorbed on the fiber. When the temperature is 60 ° C. or higher, the compound having the coordination binding ability is apt to become a hydroxide before binding to the fiber, so that it hardly penetrates into the fiber, and the chelate bond with catechins is weakened.

The treatment conditions for immobilizing the catechins of the tea leaf extract on the fibers are preferably at 30 ° C. to 60 ° C. for about 20 minutes to 40 minutes. When the temperature is 30 ° C. or lower, the reaction between the compound having coordination binding ability and the catechins is insufficient, so that antibacterial properties with washing resistance cannot be obtained. If the temperature is higher than 60 ° C., the chelate binding ability is weakened, and it is difficult to sufficiently immobilize catechins on the fibers. In addition, when the reaction time is not more than 20 minutes, the reaction between the compound having the coordination binding ability and the catechins is insufficient, so that antibacterial properties having washing resistance cannot be obtained. Also, 40
Prolonging the time for more than a minute should be avoided because it hardly contributes to the immobilization of the catechins on the fibers, or rather, some of the chelated bonds fall off the fibers.

Hereinafter, the method of the present invention will be described more specifically with reference to examples. Example 1 A 40-thread cotton single yarn was knitted to a basis weight of 220 g / m with a smooth structure using a 22 gauge double circular knitting machine. Above cotton 1
One piece (about 10 kg) of a knitted fabric of 00% was put into a jet dyeing machine, scoured and bleached at a temperature of 90 ° C. by a usual method, and washed with water to prepare an object to be treated. In a solution of a dyeing machine in which the weight ratio between the object to be treated and the treatment solution was 1:15, 3.0% by weight of aluminum alum dissolved in water and 0.5% by weight of sodium carbonate were added, and the temperature was increased. 3 at a temperature of 50 ° C
After the treatment for 0 minutes, the water was drained and sufficiently washed with water.
Then, catechin (trade name: Polyphenone, manufactured by Mitsui Norin) 3.0 dissolved in hot water of up to 60 ° C. in the solution of the dyeing machine was used.
Wt% and 10.0 wt% of sodium sulfate, and the temperature was raised.
After treating at a temperature of 30 ° C. for 30 minutes, drainage was performed, and washing was performed.

Example 2 A mixed knitted fabric of 55% cotton and 45% polyester (about 1
0Kg) into a jet dyeing machine, scouring and bleaching at a temperature of 90 ° C. by a usual method, dyeing cotton by a usual method, washing with water, and treating the object to be treated. Got ready. Thereafter, in the same manner as in Example 1, pretreatment with aluminum alum was performed. Thereafter, treatment with catechin was performed in the same manner as in Example 1.

Comparative Example 1 (Method of JP-A-8-296173) One piece (about 10 kg) of a 100% cotton knitted fabric was put into a jet dyeing machine, and scoured at a temperature of 90 ° C. by a usual method. After bleaching and washing with water, an object to be treated was prepared. 0.5% by weight of catechin (trade name: polyphenone, manufactured by Mitsui Norin) obtained by dissolving the object in hot water at 60 ° C., and a glyoxal resin (trade name: Beckamine LF-K, manufactured by Dainippon Ink) as a binder ) Padding is performed at a squeezing rate of 80% with a treatment liquid containing 4.0% by weight and 1.3% by weight of a catalyst (trade name: Catalyst G, manufactured by Dainippon Ink) and dried at a temperature of 100 ° C. After that, a heat treatment was performed at a temperature of 140 ° C. for 1 minute.

Comparative Example 2 (Method of JP-A-9-316786) One piece (about 10 kg) of a knitted fabric made of 100% cotton was put into a jet dyeing machine, and scoured at a temperature of 90 ° C. by a usual method. After bleaching and washing with water, an object to be treated was prepared. After adding 3.0% by weight of catechin (trade name: polyphenone, manufactured by Mitsui Norin Co., Ltd.) dissolved in hot water at 60 ° C. into the solution of the dyeing machine, the temperature was raised, and the mixture was treated at 80 ° C. for 30 minutes. Drained and washed thoroughly with water. Subsequently, 4.0% by weight of sodium stannate dissolved in water was added to the solution of the dyeing machine, the temperature was raised, the treatment was carried out at a temperature of 90 ° C. for 30 minutes, and then drained and washed with water.

Comparative Example 3 One piece (about 10 kg) of a knitted fabric made of 100% cotton was charged into a jet dyeing machine, scoured and bleached at a temperature of 90 ° C., and washed with water to prepare an object to be treated. Into the solution of the dyeing machine, 10.0% by weight of a cationized substance dissolved in water (trade name: Cationone UK, manufactured by Yasuo Yushi) and 1.5% by weight of NaOH were added, and the temperature was raised. After the treatment for 30 minutes, the water was drained and sufficiently washed with water. Then 6 in the solution of the dyeing machine
Catechin (trade name: polyphenone, manufactured by Mitsui Norin) dissolved in hot water at 0 ° C. was added by 3.0% by weight, and the temperature was increased.
After a treatment at a temperature of 0 ° C. for 30 minutes, the water was drained and washed with water.

The antibacterial test in each of Examples and Comparative Examples was performed as follows. (Antibacterial test) The treated cloths obtained in Examples 1 and 2 and Comparative Examples 1, 2, and 3 were tested for Staphylococcus aureus (Staphy).
lococcus aureus): IFO 1273
The antibacterial activity against No. 2 was examined and is shown in the table below. Add a bouillon suspension of the test bacterium to the sterilized test cloth and place in a closed container 37
The number of viable cells after culturing at 18 ° C. for 18 hours was measured, and the increase / decrease value with respect to the number of inoculated cells was determined. In addition, a standard cloth was used as the unprocessed cloth. A. The number of bacteria recovered (N) immediately after planting of unprocessed cloth (standard cloth)
= 3) B. B. Number of bacteria collected after 18 hours of cultivation of unprocessed cloth (standard cloth) (average of 3 times) Number of bacteria collected after cultivation of the bacteriostatically processed cloth for 18 hours (average of 3 times) The evaluation was made as a standard of the antibacterial and deodorant effect. As the test cloth, the treated cloths obtained in Examples 1 and 2 and Comparative Examples 1, 2, and 3 were combined with Monogen Uni (1.4 cc / Daiichi Kogyo Seiyaku).
At l, the product after home washing 10 times was used.

Comparison of Effects The effects of the treated cloths obtained in Examples 1 and 2 and Comparative Examples 1, 2, and 3 were compared, and the results are shown in the following table. -The antibacterial activity against the Staphylococcus aureus of the treated cloths obtained in Examples 1 and 2 passed the standard value of "antibacterial deodorant effect" of SEK, but the treated cloths obtained in Comparative Examples 1 and 2 Antibacterial activity was poor. The treated cloth obtained in Comparative Example 3 has remarkably good catechin adsorption and high antibacterial activity. However, the treated cloth obtained by this treatment method has a dark reddish brown hue, which causes inconvenience. -The treated cloth obtained in Comparative Example 1 was inferior in antibacterial activity, had a hard texture, and also exhibited a decrease in strength.

[0024]

The fiber product obtained by immobilizing catechins on the fiber product by pretreatment with the compound having the coordination ability of the present invention has excellent antibacterial properties and does not become hard. Therefore, it can be widely used for clothing applications.

Claims (2)

[Claims] 1. A pretreatment is performed by contacting a cellulosic fiber product with a treatment solution containing a metal salt having coordination binding ability, and then contacting with a treatment solution containing catechins of tea leaf extract to extract tea leaves. An antibacterial processing method for textile products, comprising fixing an object on a fiber. 2. Pretreatment of a cellulosic fiber product with a metal salt having a coordination binding ability of 0.5 to 5.0% by weight, and a catechin of a tea leaf extract of 0.1 to 5.0% by weight. The antibacterial processing method according to claim 1, wherein the antibacterial treatment is carried out by immobilizing on the fiber with the treatment liquid.