JP2009041169A - Method for applying antibacterial treatment having washing resistance to textile product - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide textile products not lowering water-absorbing property and capable of sufficiently keeping antibacterial effectiveness even after repeated washing without adding a binder when applying antibacterial treatment of the surfaces to the textile products. <P>SOLUTION: The method for applying antibacterial treatment to the textile products comprises carrying out exhaustion treatment at 50-100°C under ordinary pressure in the case of natural fibers, carrying out exhaustion treatment at 110-130°C under pressure, or carrying out immersion treatment or spray treatment under ordinary pressure in the case of synthetic fibers by using a treating liquid composed of an extracted solution of grape fruit seed in which pH is controlled to 6-13, and then carrying out heat treatment of treated fibers at 130-230°C. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

TECHNICAL FIELD The present invention relates to an antibacterial processing method for textile products, and more specifically, a textile product that is safe and sufficiently retains antibacterial properties even after repeated washing when the textile product is subjected to antimicrobial treatment against microorganisms such as bacteria. The present invention relates to an antibacterial processing method.

As a method for imparting antibacterial properties having washing resistance to a textile product, a method using an organic silicon-based quaternary ammonium salt reactive to cellulose is well known. (For example, see Non-Patent Document 1) Since this organosilicon quaternary ammonium salt can be chemically bonded to the primary hydroxyl group of cellulose, it can impart antibacterial properties with washing resistance to cellulose fiber products. Is possible. However, it is extremely difficult to impart antibacterial properties having washing resistance to synthetic fibers having no hydroxyl group. In addition, it has been pointed out that fiber products treated with such chemicals generally have a high water repellency, which reduces the ability to absorb moisture (water absorption).

As other drugs, polyhexamethylene biguanidine hydrochloride, chlorhexidine gluconate and the like are known. (For example, refer nonpatent literature 2) When a textile product is processed using polyhexamethylene biguanidine hydrochloride or chlorhexidine gluconate, it does not reduce water absorption with respect to an object to be processed, It is difficult to impart a certain antibacterial property to an object to be processed by a normal method.

In addition, there is an example in which grapefruit seed extract, which is a food additive rather than a chemical system, is treated on a plastic film or paper for bactericidal and antifungal purposes (for example, see Patent Document 1). Since it is not a textile product, there is no need for washing resistance as in clothing, and at pH 2.5 to 3 described in Patent Document 1, for example, simply coating a grapefruit seed extract on a textile product does not provide washing resistance. I can't get it.

A functional agent that aims to prevent aging and anti-atopy by combining ferulic acid or its derivatives with grapefruit, etc., microencapsulating or encapsulating with cyclodextrin, and then treating the fiber with a binder. Although there is an example (for example, refer to Patent Document 2), it is necessary to microencapsulate or cyclodextrin, and in order to obtain washing resistance, it is necessary to use a binder together. By adding a binder, there are problems of coloring such as hardening of the texture and yellowing, and depending on the amount of the binder used, there are problems such as deterioration in performance because the binder covers the surface of the drug.

“All about Antibacterials” (Textile) September 5, 1997, P603-606 “All about Antibacterials” (Textiles) Issued on September 5, 1997 P146-147 Japanese Patent Laid-Open No. 02-193901 JP 2004-324026 A

Problems to be solved by the invention

Under such circumstances, the present invention is an antibacterial property that does not decrease water absorption in natural fiber products and synthetic fiber products, and that antibacterial properties are sufficiently retained even after repeated washing without using a binder. It provides textile products.

Means for solving the problem

The present invention uses a treatment solution comprising a grapefruit seed extract adjusted to a pH of 6 to 13, exhausting at a temperature of 50 ° C. to 100 ° C. under normal pressure for natural fibers, and adding for a synthetic fiber. Exhaust treatment is performed at a temperature of 110 to 130 ° C. under pressure, or a treatment product comprising a grapefruit seed extract with a pH adjusted to 6 to 13 under normal pressure and a pH of 6 to 13 is used. This can be easily achieved by heat treatment at ˜230 ° C.

Examples of the fiber product that is the subject of the present invention include natural fiber products such as cellulose fibers and natural polyamide fibers, and synthetic fiber products such as polyester fibers, synthetic polyamide fibers, acrylic fibers, and polyolefin fibers.

As a method for producing an antibacterial fiber product, it is produced by a conventional method such as a dipping method, an exhaust method, or a spray method.

Since the grapefruit seed extract has a pH of 2.5 to 5, an alkaline agent is added to adjust the pH from 6 to 13.

Alkaline agents include alkaline substances such as sodium carbonate, potassium carbonate, sodium hydroxide, potassium hydroxide, sodium tripolyphosphate, potassium tripolyphosphate, etc., or sodium bicarbonate, potassium bicarbonate, sodium trichloroacetate, potassium trichloroacetate, etc. And the like which generate an alkali by heating. The alkali agent is not particularly limited as long as it is an alkaline substance or an alkali-generating substance.

The grapefruit seed extract is obtained by pulverizing grapefruit seed and extracting it by a heating distillation method, a hydrolysis method, a solvent extraction method, a pressing method or the like. Such liquids are well known as described in JP-A-6-40834 and the like, and the main components are fatty acids and flavonoids, and are mixed with glycerin 1: 1 or 1: 2 for product stabilization. It is used as a liquid and is recognized as an existing additive in the Food Sanitation Law.

For example, when the grapefruit seed extract is obtained as a 1: 2 (weight ratio) mixture with glycerin, the physical properties are: viscosity: 50 to 150 (mPa · S), pH 2.5 to 5.0, specific gravity (25 ° C. ) 1.1-1.2.

The following is an example of a method for producing antibacterial textile products having wash resistance.
Grapefruit seed extract obtained as described above is used in an aqueous solution containing 0.01% to 10.0%, preferably 0.1% to 5.0%. By spraying or spraying. If the amount used is less than this range, sufficient antibacterial efficacy will not be exhibited, and even if used in excess, the cost will be high and there will be no benefit.

When natural fibers are treated by the exhaust method, the temperature of the treatment solution is usually 50 ° C. to 100 ° C. under normal pressure, and the treatment time is usually 5 to 60 minutes, preferably 20 to 60 minutes.

When the synthetic fiber is treated by the exhaust method, the temperature of the treatment liquid is usually 110 ° C. to 130 ° C. under pressure, and the treatment time is usually 5 minutes to 60 minutes, preferably 20 minutes to 60 minutes.

The treatment pH is 6.0 to 13.0, preferably 8.0 to 12.0. At pH lower than pH 6.0, the antibacterial agent has high water solubility, and washing resistance cannot be obtained. Moreover, when higher than pH13.0, it is not good also from the surface of the safety | security at the time of a process. When antibacterial treatment is performed at the same time as dyeing at a pH lower than 6.0, antibacterial properties with washing resistance cannot be obtained, so it is necessary to perform antibacterial processing in a separate bath from dyeing. Regarding drying after exhaustion treatment, the drying temperature is not particularly limited, but is usually dried at 50 to 120 ° C.

In the case of treatment by the dipping method or spray method, the fiber product is dipped or sprayed in a treatment solution at normal temperature under normal pressure, then squeezed with a mangle as necessary, a predetermined amount of processing agent is applied, and then heat treatment is fixed. A treatment pH of 6.0 to 13.0 is necessary to obtain washing durability. Therefore, antibacterial properties can be obtained in the same way as the exhaust method when antibacterial treatment is performed simultaneously with dyeing at a lower pH. Since there is no antibacterial treatment in a separate bath from dyeing. The drying temperature is usually 50 ° C to 120 ° C and there is no particular limitation. In order to obtain fiber durability for the synthetic fiber, it is necessary to perform a heat treatment after drying. The heat treatment temperature is usually 130 ° C to 230 ° C, preferably 160 ° C to 200 ° C, and the treatment time is 30 seconds to 30 minutes.

EXAMPLES Hereinafter, although an Example demonstrates this invention in detail, this invention is not limited to these Examples.

Example 1
Grapefruit seed extract having a specific gravity of 1.15 (20 ° C.) (produced by Release Kagaku Kogyo Co., Ltd.) was diluted with ion-exchanged water to a concentration of 0.3%, and the pH was adjusted to 7 with 1N aqueous sodium hydroxide solution. . A polyester jersey was immersed in this aqueous solution, drawn to 100% with a mangle, dried at 100 ° C. for 3 minutes, and then heat-treated at 180 ° C. for 5 minutes to obtain an antibacterial fiber product. Thereafter, a washing test was performed, and antibacterial tests of antibacterial activity before and after the washing test were performed using test cloths for antibacterial tests. The results are shown in Table-1.

Example 2
The same procedure as in Example 1 was conducted except that the polyester jersey was changed to a 6-nylon jersey and the heat treatment temperature was changed from 180 ° C. for 5 minutes to 160 ° C. for 5 minutes. The results are shown in Table-2.

Washing test The washing test was performed using a household washing machine in accordance with the test specified in JIS 10217 (1976) 103. After washing for 5 minutes in 28 liters (bath ratio 1:30) of 40 ° C. water containing 1.33 g / liter of JAFET standard detergent provided by the Fiber Evaluation Technical Council as a detergent, rinse for 2 minutes, dehydrate, The same operation was repeated 10 times by rinsing for 2 minutes and dehydration once.

Antibacterial test method In the antibacterial test, the number of viable bacteria and the bacteriostatic activity value were measured according to the JIS L1902 bacterial solution absorption method. The smaller the number of viable bacteria, the higher the antibacterial activity, and the higher the bacteriostatic activity value, the higher the antibacterial property. The results are shown in Tables 1 and 2. As a test bacterium, K. pneumoniae (ATCC4352) was used.

Example 3
The same procedure as in Example 1 was performed except that the pH was adjusted to 6 with a 1 N aqueous sodium hydroxide solution. The results are shown in Table-1.

Example 4
The same procedure as in Example 1 was performed except that the pH was adjusted to 8 with a 1 N aqueous sodium hydroxide solution. The results are shown in Table-1.

Example 5
The same procedure as in Example 1 was carried out except that the pH was adjusted to 12 with a 1 N aqueous sodium hydroxide solution and heat-treated at 130 ° C. for 10 minutes. The results are shown in Table-1.

Example 6
The same procedure as in Example 1 was performed except that the pH was adjusted to 9 with a 1N aqueous sodium hydroxide solution and the concentration of the grapefruit seed extract was adjusted to 0.5%. The results are shown in Table-1.

Example 7
The same procedure as in Example 1 was performed except that the pH was adjusted to 11 with a 1 N aqueous sodium hydroxide solution and the concentration of the grapefruit seed extract was adjusted to 0.5%. The results are shown in Table-1.

Example 8
The same procedure as in Example 1 was performed except that the pH was adjusted to 8 with a 1 N aqueous sodium hydroxide solution and the concentration of the grapefruit seed extract was adjusted to 1.0%. The results are shown in Table-1.

Example 9
The same procedure as in Example 1 was performed except that the pH was adjusted to 8 with a 1 N aqueous sodium carbonate solution and the concentration of the grapefruit seed extract was adjusted to 5.0%. The results are shown in Table-1.

Example 10
The same procedure as in Example 1 was performed except that the pH was adjusted to 8 with a 1 N aqueous sodium carbonate solution and the concentration of the grapefruit seed extract was adjusted to 8.0%. The results are shown in Table-1.

Example 11
The same procedure as in Example 1 was performed except that the pH was adjusted to 9 with a 1 N aqueous sodium hydroxide solution, the grapefruit seed extract concentration was 0.5%, and heat treatment was performed at 230 ° C. for 90 seconds. The results are shown in Table-1.

Example 12
The same procedure as in Example 1 was performed except that the pH was adjusted to 9 with a 1 N aqueous sodium hydroxide solution, the concentration of the grapefruit seed extract was 0.5%, and heat treatment was performed at 150 ° C. for 5 minutes. The results are shown in Table-1.

Example 13
The same procedure as in Example 1 was performed except that the pH was adjusted to 9 with a 1 N aqueous sodium hydroxide solution, the grapefruit seed extract concentration was 0.5%, and heat treatment was performed at 130 ° C. for 10 minutes. The results are shown in Table-1.

Comparative Example 1
The same procedure as in Example 1 was performed except that a 0.5% aqueous solution of 3- (methoxysilyl) propyloctadecyldimethylammonium chloride was used instead of the 0.3% concentration of grapefruit seed extract. The results are shown in Table-1.

Comparative Example 2
The same procedure as in Example 1 was performed except that a 1.0% aqueous solution of polyhexamethylene biguanidine hydrochloride was used instead of the 0.3% concentration of grapefruit seed extract. The results are shown in Table-1.

Comparative Example 3
The same procedure as in Example 1 was performed except that the pH was adjusted to 2 with a 1N aqueous hydrochloric acid solution instead of adjusting the pH to 7 with a 1N aqueous sodium hydroxide solution. The results are shown in Table-1.

Comparative Example 4
The same procedure as in Example 1 was conducted except that the pH was not adjusted instead of 7 with a 1 N aqueous sodium hydroxide solution. The results are shown in Table-1.

Comparative Example 5
The same procedure as in Example 1 was performed except that the pH was adjusted to 9 with a 1 N aqueous sodium hydroxide solution and the concentration of the grapefruit seed extract was 0.5% at 180 ° C. for 5 minutes instead of heat treatment at 100 ° C. for 5 minutes. It was. The results are shown in Table-1.

Example 14
The same procedure as in Example 2 was performed except that the pH was adjusted to 6 with a 1 N aqueous sodium hydroxide solution. The results are shown in Table-2.

Example 15
The same procedure as in Example 2 was performed except that the pH was adjusted to 8 with a 1 N aqueous sodium hydroxide solution. The results are shown in Table-2.

Example 16
The same procedure as in Example 2 was carried out except that the pH was adjusted to 12 with a 1 N aqueous sodium hydroxide solution and heat-treated at 130 ° C. for 10 minutes. The results are shown in Table-2.

Example 17
The same procedure as in Example 2 was performed except that the pH was adjusted to 9 with a 1N aqueous sodium hydroxide solution and the concentration of the grapefruit seed extract was adjusted to 0.5%. The results are shown in Table-2.

Example 18
The same procedure as in Example 2 was performed except that the pH was adjusted to 11 with a 1N aqueous sodium hydroxide solution and the concentration of the grapefruit seed extract was adjusted to 0.5%. The results are shown in Table-2.

Example 19
The same procedure as in Example 2 was performed except that the pH was adjusted to 8 with a 1 N aqueous sodium hydroxide solution and the concentration of the grapefruit seed extract was adjusted to 1.0%. The results are shown in Table-2.

Example 20
The same procedure as in Example 2 was performed except that the pH was adjusted to 8 with a 1 N aqueous sodium carbonate solution and the concentration of the grapefruit seed extract was adjusted to 5.0%. The results are shown in Table-2.

Example 21
The same procedure as in Example 2 was performed except that the pH was adjusted to 8 with a 1 N aqueous sodium carbonate solution and the concentration of the grapefruit seed extract was adjusted to 8.0%. The results are shown in Table-2.

Example 22
The same procedure as in Example 2 was conducted except that the pH was adjusted to 9 with a 1 N aqueous sodium hydroxide solution, the grapefruit seed extract concentration was 0.5%, and heat treatment was performed at 230 ° C. for 90 seconds. The results are shown in Table-2.

Example 23
The same procedure as in Example 2 was performed except that the pH was adjusted to 9 with a 1 N aqueous sodium hydroxide solution, the concentration of the grapefruit seed extract was 0.5%, and heat treatment was performed at 150 ° C. for 5 minutes. The results are shown in Table-2.

Example 24
The same procedure as in Example 2 was performed except that the pH was adjusted to 9 with a 1 N aqueous sodium hydroxide solution, the concentration of the grapefruit seed extract was 0.5%, and heat treatment was performed at 130 ° C. for 10 minutes. The results are shown in Table-2.

Comparative Example 6
The same procedure as in Example 2 was performed except that a 0.5% aqueous solution of 3- (methoxysilyl) propyloctadecyldimethylammonium chloride was used instead of the 0.3% concentration of grapefruit seed extract. The results are shown in Table-2.

Comparative Example 7
It carried out like Example 2 except having used the 1.0% aqueous solution of polyhexamethylene biguanidine hydrochloride instead of the 0.3% concentration of grapefruit seed extract. The results are shown in Table-2.

Comparative Example 8
The same procedure as in Example 2 was performed except that the pH was adjusted to 2 with a 1N aqueous hydrochloric acid solution instead of adjusting the pH to 7 with a 1N aqueous sodium hydroxide solution. The results are shown in Table-2.

Comparative Example 9
The same procedure as in Example 2 was performed except that the pH was not adjusted instead of 7 with a 1 N aqueous sodium hydroxide solution. The results are shown in Table-2.

Comparative Example 10
The procedure was as in Example 2, except that the pH was adjusted to 9 with 1N aqueous sodium hydroxide solution and the concentration of the grapefruit seed extract was 0.5% at 160 ° C. for 5 minutes instead of heat treatment at 100 ° C. for 5 minutes. It was. The results are shown in Table-2.

As is clear from Tables 1 and 2, the examples of the present invention showed excellent antibacterial properties even after washing.

Example 25
Cotton knit bath ratio 1:30, reactive dye per fabric weight (Sumifix Brilliant Red 3BF 150% (Sumitomo Chemical Co., Ltd.)), grapefruit seed extract (Release Kagaku Kogyo Co., Ltd.) 0.5%, carbonic acid After dyeing with sodium 15 g / l, anhydrous sodium sulfate 40 g / l, 60 ° C. for 30 minutes, and exhausting, it was dried at 100 ° C. The washing test was conducted in the same manner as in Example 1. In the antibacterial test, Staphylococcus aureus (IFO12732) was used in place of Klebsiella pneumoniae (ATCC4352) as a test bacterium. The results are shown in Table-3.

Example 26
The same procedure as in Example 25 was performed except that the concentration of the grapefruit seed extract was 1.0%, 50 ° C., and dyed by the exhaust method for 60 minutes. The results are shown in Table-3.

Example 27
Polyester jersey with a bath ratio of 1:30 and disperse dye per fabric weight (Kayalon Polyester Yellow Brown 3RL200 0.33%, Kayalon Polyester Rubin 3GL-S150 0.44%, Kayalon Polyester Blue BR-SF 0.66% Formulation (Nippon Kayaku Co., Ltd.)), 0.5% of grapefruit seed extract (Release Kagaku Kogyo Co., Ltd.) and 1 g / l of Escor T-150 (leveling agent: Senka Co., Ltd.) were added. Next, the pH was adjusted to 9 with Senka Buffer 600 (pH adjuster: Senka Co., Ltd.), subjected to high-pressure exhaust dyeing at 130 ° C. for 60 minutes, then subjected to reduction washing, water washing and drying. The washing test was conducted in the same manner as in Example 1. In the antibacterial test, Staphylococcus aureus (IFO12732) was used as a test bacterium. The results are shown in Table-3.

Example 28
The same operation as in Example 27 was performed except that the concentration of the grapefruit seed extract was 1.0%. The results are shown in Table-3.

Example 29
6% nylon jersey was added with 1.0% grapefruit seed extract (Release Kagaku Kogyo Co., Ltd.) at a bath ratio of 1:30. The pH was adjusted to 9 with 1N sodium hydroxide, then subjected to high-pressure exhaustion at 110 ° C. for 30 minutes, and then dried at 100 ° C. for 3 minutes. The washing test was conducted in the same manner as in Example 1. In the antibacterial test, Staphylococcus aureus (IFO12732) was used as a test bacterium. The results are shown in Table-3.

Example 30
Grapefruit seed extract (Release Kagaku Kogyo Co., Ltd.) 1.0% and sodium carbonate 15 g / L were added at a bath ratio of 1:30 to cotton knit. Next, after exhausting at 100 ° C. for 60 minutes, drying was performed at 100 ° C. for 3 minutes. The washing test was conducted in the same manner as in Example 1. In the antibacterial test, Staphylococcus aureus (IFO12732) was used as a test bacterium. The results are shown in Table-3.

Comparative Example 11
The same procedure as in Example 25 was performed except that a 0.5% aqueous solution of 3- (methoxysilyl) propyloctadecyldimethylammonium chloride was used instead of the grapefruit seed extract 0.5% concentration. The results are shown in Table-3.

Comparative Example 12
2% disperse dye per dough weight (Sumikaron Red SE-RPD (Sumitomo Chemical Co., Ltd.)), 0.5% grapefruit seed extract (Release Kagaku Kogyo Co., Ltd.) Escor T-150 (leveling agent: Senka Co., Ltd.) 1 g / l was added. Next, the pH was adjusted to 4 with 0.5 g / l of acetic acid, and high-pressure exhaust dyeing was performed at 130 ° C. for 60 minutes, followed by reduction washing, water washing and drying. The results are shown in Table-3.

Comparative Example 13
The same procedure as in Comparative Example 12 was performed except that the concentration of the grapefruit seed extract was 1.0%. The results are shown in Table-3.

Comparative Example 14
The same procedure as in Example 27 was performed except that a 0.5% aqueous solution of 3- (methoxysilyl) propyloctadecyldimethylammonium chloride was used instead of the 0.5% concentration of grapefruit seed extract. The results are shown in Table-3.

Comparative Example 15
The same procedure as in Example 27 was performed, except that a 1.0% aqueous solution of polyhexamethylene biguanidine hydrochloride was used instead of the 0.5% concentration of grapefruit seed extract. The results are shown in Table-3.

As is clear from Table 3, the examples of the present invention showed excellent antibacterial properties even after washing.

Claims (4)

A washing-resistant antibacterial processing method for textiles, characterized by treating with a treatment liquid comprising a grapefruit seed extract adjusted to pH 6-13. The method for washing antibacterial antibacterial processing for synthetic fibers according to claim 1, wherein the fiber product is heated with the treatment liquid under pressure at a temperature of 110 to 130 ° C. 2. The method for washing antibacterial antibacterial processing for natural fibers according to claim 1, wherein the fiber product is subjected to a heat treatment at 50 to 100 [deg.] C. under normal pressure with the treatment liquid. The laundry-resistant antibacterial processing method for synthetic fibers according to claim 1, wherein a heat treatment is performed at a temperature of 130 to 230 ° C under normal pressure after the textile product is treated with the treatment liquid.