JP2003313775A - Method for producing textile product - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing textile products in which the amount of caffeine immobilized on the textile products can be increased and the resistance of the caffeine immobilized on the textile products against washing is increased and the caffeine is gradually released into human bodies. <P>SOLUTION: The textile product is obtained by treating a textile product with tannic acid and caffeine. In order to stably immobilizing the caffeine on the textile product, a complex of caffeine and tannic acid is formed on the textile product by treating the product with an aqueous tannic acid solution and is followed by treatment with an aqueous caffeine solution. Or, caffeine and tannic acid is mixed to form their complex in the solution mixture and a textile product is treated with the aqueous solution containing the complex. Or, after dyeing a textile product, the textile product is subjected to fixing treatment with tannic acid, then treated with tannic acid and treated with an aqueous caffeine solution. Further in another case, after dyeing a textile product, the textile product is subjected to fixing treatment with tannic acid and then treated with an aqueous caffeine solution. <P>COPYRIGHT: (C)2004,JPO

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention is directed to the production of a textile product which is expected to have a wash-resistant skin care effect and a sustained release effect of an active ingredient which is expected to have a skin care effect due to sweat, and which is excellent in texture and hygroscopicity. Regarding the method, this can be suitably used in the field of clothing such as underwear and shirts.

[0002]

2. Description of the Related Art Attempts have been made for a long time to apply an active ingredient used for cosmetics and the like to textile products for the purpose of skin care and to apply it. For example, Japanese Unexamined Patent Publication No. 9-296367 discloses a garment to which a subcutaneous fat adjusting agent and / or microencapsulated subcutaneous fat adjusting agent is attached by a binder, and Japanese Unexamined Patent Publication No. 11-100310 discloses a slimming cosmetic composition. Patent No. 3038
Japanese Patent Laid-Open No. 20 discloses a functional fiber in which a processing agent containing a functional substance, a hydrolyzed protein and a cross-linking agent is applied to and fixed to the fiber, and a method for producing the functional fiber. However, these publications do not disclose the idea of actively and slowly releasing the active ingredient from the fibers to the wearer's skin when worn. The applicant made the invention in Japanese Patent Application Laid-Open No. 2002-61073 and Japanese Patent Application No. 2001-119078 in which an ascorbic acid derivative and α-tocophenol acetate are positively and slowly released from the fiber to the skin of the wearer when worn. ing. These inventions provide an ascorbic acid derivative and α-tocophenol acetate as a surfactant in order to impart contradictory functions such as washing durability and sustained release to the skin of active ingredients used in cosmetics and the like to be used. Is used to treat a textile product with a treatment liquid which is emulsified and dispersed in water and an organic solvent. The above-mentioned conventional techniques have not disclosed the use of caffeine together with tannic acid to gradually release the active ingredient into the skin.

[0003]

Problems to be Solved by the Invention
Japanese Patent Publication No. 73 and Japanese Patent Application No. 2001-119078 disclose a method for immobilizing a sustained-release property on a textile product by utilizing the hydrophobicity and ionicity of an active ingredient used in cosmetics and the like. . However, when trying to apply caffeine to the methods of these inventions, caffeine is, as inferred from its molecular structure,
Ionically, it shows only a very weak basicity due to the four nitrogen atoms of the purine ring, and although it is soluble in water as well as in organic solvents, it is not highly soluble and almost soluble in sebum. Due to such a dissolution property, a fiber product having a sustained release function cannot be obtained even by using a conventional method, and a remarkable devise is required to solve this problem. Also, Patent No. 303
The method of immobilizing the complex of collagen and caffeine on a fiber with an isocyanate cross-linking agent disclosed in Japanese Patent No. 8202 has almost no sustained release effect because caffeine is strongly immobilized on the fiber, and However, there was a problem that the amount immobilized on the fiber was very low. Therefore, the object of the present invention is to exhibit sustained release of caffeine,
An object of the present invention is to provide an effective and improved method for producing a textile product by measuring an increase in the amount of immobilization.

[0004]

[Means for Solving the Problems] The present inventors have fixed caffeine on textiles with washing durability, and further used caffeine and tannic acid in combination in order to release gradually when worn. The present invention has been made paying attention to the fact that a complex, that is, a complex is formed. Both tannic acid and caffeine are components contained in tea in a large amount, and it is known that a stable complex is formed from both of them. this is,
It is caused by the hydrophobic interaction and weak ionic interaction between the purine ring of caffeine and the aromatic molecule of tannic acid. It is known that this interaction is weakened by an increase in salt concentration and temperature, so when applied to textiles, even if the concentration of salt contained in the sweat of the wearer changes, it is eluted from the textiles. Also, an increase in elution amount due to an increase in body temperature can be expected.

The present invention is a method for producing a fiber product by treating the fiber product with tannic acid and caffeine. Since the method for stably immobilizing caffeine on the textile product of the present invention requires forming a complex of caffeine and tannic acid on the textile product, the textile product is treated with an aqueous tannic acid solution. Then, a method of treating with a caffeine aqueous solution and a method of first forming a complex in a mixed aqueous solution of caffeine and tannic acid and then treating the fiber product with the aqueous solution containing the complex. Further, there are a method of treating a textile product which has been dyed and fixed with tannic acid and then treated with an aqueous solution of caffeine and then a method of treating a textile product which has been dyed and then fixed with tannic acid with an aqueous solution of caffeine.

[0006]

BEST MODE FOR CARRYING OUT THE INVENTION The fiber product used in the present invention is not particularly limited, and as raw fibers, natural fibers such as cotton, wool and silk which are usually used as clothing, rayon, polynosic,
Regenerated fibers such as acetate, synthetic fibers such as polyester, nylon, and acrylic may be used, or one kind or a mixture of two or more kinds thereof may be used. The shape may be any of raw fiber, spun yarn, knitted fabric, and fiber sewn product. When the fiber product of the present invention is a raw fiber, a spun yarn, or a knitted fabric, these are used to make a fiber sewn product for clothing.
Further, a fiber product obtained by dyeing and then fixing with tannic acid is also included. For example, a fiber product obtained by dyeing a nylon product with an acid dye and then fixing with tannic acid, and a cationic dye disclosed by the applicant in JP-A-10-121384. Examples of the fiber product include modified regenerated cellulose fibers treated with tannic acid / tartar tar after dyeing with, and are also suitably used for leg-related fiber products such as panty hose using nylon.

As a method of immobilizing caffeine on a textile product using tannic acid, a method of treating with an aqueous solution of tannic acid, heat treatment, and further treating with an aqueous solution of caffeine, and a method of previously mixing tannic acid and caffeine There is a method of preparing a complex of tannic acid and caffeine in an aqueous solution and then treating the fiber product in the aqueous solution containing the complex. Which is adopted depends on the kind of the fiber material used and the shape of the fiber product. Is appropriately selected depending on the ease of processing.

For the immobilization of tannic acid on a textile product, in the case of a textile product such as nylon capable of specifically binding to tannic acid, adsorption by contact with an aqueous solution of tannic acid is sufficient, and then with an aqueous solution of caffeine. Caffeine can be immobilized by processing. The amount of tannic acid to be pretreated is preferably in the range of 0.5 to 20% by weight based on the weight of fiber, and the amount can be appropriately determined depending on the desired amount of immobilized caffeine. If it is less than 0.5% by weight out of this range, the amount of caffeine immobilized is small regardless of the amount of caffeine used, and if it is more than 20% by weight, the amount of caffeine immobilized is greater than the increase in tannic acid. It is not preferable because the amount of conversion does not increase. The amount of caffeine used is preferably in the range of 60 to 120% by weight with respect to tannic acid,
It is preferred to use caffeine at 100% by weight of tannic acid.

In the case of fibers such as cellulose fibers that cannot specifically bind to tannic acid, tannic acid may be immobilized on a fiber product with a fixing agent such as a crosslinking agent or a resin processing agent.
Caffeine can then be immobilized on the textile by treatment with an aqueous caffeine solution.

A method of preparing a complex in an aqueous solution of tannic acid and caffeine, treating the fiber product in the aqueous solution, and immobilizing the complex on the fiber product is a method of treating the fiber product on the fiber product in a single treatment. The complex can be immobilized. In the method for preparing the complex of tannic acid and caffeine, the complex can be easily formed by adding the aqueous solution of tannic acid to the liquid while stirring the aqueous solution of caffeine. In this case, the mixing ratio of caffeine to tannic acid is preferably in the range of 60 to 120% by weight, but it is preferable to use 100% by weight of tannic acid, that is, the same amount of caffeine. Within this range, the higher the proportion of caffeine, the higher the aggregation rate of the complex. However, if it is outside this range, 60% by weight or less will cause coloring, and if it is 120% by weight or more, the aggregation rate will be high. Absent. Further, the pH at the time of preparing the complex is preferably 7 or less. If the pH is 7 or more, the re-decomposition of aggregates generated is remarkable, which is not preferable. The concentration at the time of preparing the complex also affects the complex formation, and the concentration at this time is preferably in the range of 0.5 to 20% by weight. If the amount is less than 0.5% by weight out of this range, it becomes difficult to prepare a composite, and if it exceeds 20% by weight, it is difficult to prepare a uniform composite due to severe aggregation.

As a method of treating a textile product with tannic acid and caffeine of the present invention, a pad-dry method or a batch method which is usually used can be applied. In the bad-dry method, first, a complex of tannic acid and caffeine may be prepared and then a fixing agent selected from a suitable crosslinking agent, resin processing agent and binder may be added, and a fiber product may be added to this complex-containing aqueous solution. After dipping for 0.5 seconds or more and squeezing at a squeezing ratio of 60 to 120%, a drying treatment may be performed at a temperature of 80 to 200 ° C. for 1 to 30 minutes. A fixing agent selected from a crosslinking agent, a resin processing agent, and a binder used at this time may be appropriately selected according to the fiber product to be processed. An epoxy-based cross-linking agent is suitable as the cross-linking agent, and an isocyanate-based cross-linking agent is not preferable because the sustained release property is impaired by the reaction with caffeine. The resin processing agent is preferably an N-methylol resin, and the binder is preferably an acrylic, urethane or ester binder.

In the batch method, the fiber product is mixed with a bath ratio of 1:10.
Immerse in the treatment liquid at 1:30, and 5 to 6 at a temperature of 20 to 90 ° C.
It should be processed for 0 minutes. When discoloration due to tannic acid is feared during the processing of the textile product, tartarite may be added to the treatment liquid, or after the treatment with the tannic acid aqueous solution, the post-treatment with the tartaric acid aqueous solution may be performed.

When using a textile product which has been fixed with tannic acid after dyeing, it is treated with an aqueous solution of tannic acid and then with an aqueous solution of caffeine according to the desired immobilization amount of caffeine. When the residual amount of acid is sufficient, caffeine can be immobilized by treating with an aqueous caffeine solution. If the residual amount of tannic acid on the textile product that has been fixed with tannic acid after dyeing is unknown, use a solution of known caffeine concentration at three levels: low concentration, medium concentration, and high concentration as a preliminary test. After the treatment, the amount of immobilization of caffeine in the initial stage of processing and the amount of immobilization after 10 times of washing are measured. From this result, it was confirmed whether the tannic acid used for the fix treatment of the sample remained, and when all three levels did not reach the desired immobilization amount of caffeine, it was treated with an aqueous tannic acid solution, and then an aqueous caffeine solution. Is applied, and if any of the three levels satisfies the desired immobilization amount of caffeine, tannic acid that immobilizes caffeine is assumed to remain, and it is treated with an aqueous caffeine solution. The method can be adopted.

The textile thus treated can be washed with water and then subjected to the usual final finishing. The textile product obtained by the method of the present invention has an immobilized amount of caffeine of 50% or more even after washing 10 times, and exhibits excellent washing durability. It is speculated that this is because caffeine strongly forms a complex with tannic acid and the complex is not broken by ordinary washing.

The fiber product obtained by the method of the present invention is
The elution of caffeine due to washing is suppressed, and because caffeine dissolves well in ionic liquids such as sweat, caffeine is gradually released into the human body's skin, and is eventually taken into the skin, thereby providing skin care. It is expected to be effective.

[0016]

EXAMPLES The present invention will be specifically described below with reference to examples, but the present invention is not limited to this range. The measuring method and evaluation in this example were performed based on the following methods. -Method for measuring the amount of immobilized caffeine The sample was placed in a solution of artificial sweat (JIS L0848-5.1) and shaken at 37 ° C for 2 hours, and then the supernatant was HP.
The amount of caffeine adhering to the sample was calculated from the peak area of caffeine obtained by measuring by LC (high performance liquid chromatography).・ Washing durability calculation method Caffeine immobilization amount in the initial sample of processing and JIS L
0217-1995 “Display term and display method for handling textile products” 2.2 (1) From the immobilized amount of caffeine in a sample obtained by repeatedly washing 10 times based on washing number 103 and then drying. The washing durability was calculated by the formula.

[Equation 1] ・ Caffeine sustained-release evaluation method Artificial sweat (JIS L0848-5.1) A white cloth attached to cotton for dyeing fastness test immersed in an aqueous solution was brought into contact with the sample, and sandwiched between two hard plastic plates After squeezing
After applying a pressure of about 12.5 kPa and allowing it to stand for 30 minutes, JIS L0217-1995, 2.2. (1) The sample was washed based on washing method number 103. The sample after drying after washing once, after washing 4 times, and after washing 10 times was measured by the above-mentioned method for measuring the amount of immobilization of caffeine, and the presence or absence of sustained release was evaluated from the change in the numerical value of the amount of immobilization. .

Example 1 1.55 tex polyurethane elastic yarn [trade name: Fujibo Spandex, manufactured by Fuji Spinning Co., Ltd.] as a core, 1.11 tex (5 filaments) nylon [trade name: Miracosmo, Toray ( stock)
S twist single-covered yarn (hereinafter referred to as S
CY). Similarly 1.655tex
1.11tex (5
Z-twisted SCY coated with nylon (filament) was manufactured and used as a raw yarn for pantyhose.

The S twist SCY and the Z twist SCY described above are alternately fed one by one to a panty hose knitting machine having 400 needles, and the panty hose is knitted at a rotation speed of 500 rpm, and the temperature is set by a preset machine. After heat treatment at 80 ° C. for 10 minutes, sewing was performed to obtain 9 pairs of panty hose. The pantyhose obtained is nylon 62.2.
%, And the polyurethane elastic yarn was 37.8%.

Then, each pair of panty hose is treated with a treatment liquid containing 0.5 g / l of a penetrating agent for refining [trade name: Espitol BSconc, manufactured by Sun Kagaku Co., Ltd.] at a bath ratio of 1:
Soaping was carried out at 20 and a temperature of 95 ° C. Tannic acid [trade name: reagent tannic acid, manufactured by Kanto Kagaku Co., Ltd.] per weight of one pair of pantyhose was 0.1% owf, 0.
5% owf, 1.0% owf, 3.0% owf, 5.0
% Owf, 10.0% owf, 20.0% owf, 3
Eight types of aqueous solution containing 0.0% owf were prepared, and one pair of panty hose in the treatment liquid was used in a bath ratio of 1:20 and a temperature of 8
It was treated at 0 ° C. for 20 minutes. Next, caffeine (trade name: reagent caffeine, manufactured by Kanto Kagaku Co., Ltd.) listed in Table 1 was added to 0.1% owf, 0.5% owf, and 1.0% ow, respectively.
f, 3.0% owf, 5.0% owf, 10.0% ow
f, 20.0% owf, 30.0% owf aqueous solution treatment bath, each pantyhose with a bath ratio of 1:20,
It was treated at a temperature of 60 ° C. for 30 minutes and then washed with water. Then, each panty hose is treated with a finishing agent [trade name: Evaphanol N-20, manufactured by Nichika Kagaku Co., Ltd.] of an aqueous solution containing 4.0% owf at a bath ratio of 1:20 and a temperature of 40 ° C. for 15 minutes. After that, the sample was spin-dried and dried with warm air of 80 ° C. for 30 minutes to obtain sample No. 1-No. Got 8. For comparison, one pair of pantyhose was not treated with an aqueous solution of tannic acid, 5.0% owf of caffeine, and a finishing agent 4.
Comparative sample No. 1 was treated with an aqueous solution containing 0% owf. 1
Got

The amount of caffeine immobilized was measured using these samples, and JIS L0217-1995 "Indication terms and indication methods for handling textiles" 2.2
(1) Based on washing method No. 103, the amount of immobilized caffeine in a sample obtained by repeatedly washing 10 times and then drying was measured, and the results of calculating the washing durability are shown in Table 1.
Further, the amount of immobilized caffeine of each sample obtained by the sustained release evaluation method was measured, and the results are shown in Table 1.

[0021]

[Table 1]

From Table 1, it can be seen from Sample No. 1 that the treatment concentration of the tannic acid and caffeine aqueous solution is 0.1% owf. In No. 1, the amount of caffeine immobilized in the initial stage of processing was as small as 0.02 mg / g, and the washing durability was poor. Sample No. in which the treatment concentration of the tannic acid and caffeine solution was 30.0% owf. Sample No. 8 has a treatment liquid concentration of 20.0% owf. The amount of initial immobilization was almost the same as that of No. 7, and the effect of increasing the treatment concentration was not observed. Sample No.
2 to No. In No. 7, the amount of immobilization of caffeine in the initial stage of processing increased with the increase in the treatment concentration of tannic acid and caffeine aqueous solution. In addition, the amount of caffeine immobilized after 10 times of washing also increases with the increase in the treatment concentration of the tannic acid and caffeine aqueous solution. Their wash durability is 56.4% to 7
All samples showed high washing durability of 3.0%, and the samples washed after contact treatment with the cotton-attached white cloth containing artificial sweat that had been subjected to the method for evaluating the sustained release property of caffeine, had the washing durability. The degree of immobilization of caffeine is larger than that of the sample used in Example 1 and gradually decreases with repeated washing, and thus it is clear that caffeine has a sustained release property against artificial sweat. For comparison, a comparative sample No. which was treated only with an aqueous solution containing 5.0% owf of caffeine and 4.0% owf of a finishing agent without treating the aqueous solution of tannic acid and tartarite. 1 has a fixed amount of 0.324 mg /
g and the sample No. This is only one tenth of the immobilization amount of 6, and it is clear from this that tannic acid is deeply involved in the immobilization of caffeine.

Example 2 Eight pairs of panty hose were obtained in the same manner as in Example 1, and each pair of panty hose was treated with the same treatment liquid containing 0.5 g / l of the same scouring penetrant as in Example 1 at a bath ratio. After soaping at a temperature of 1:20 and a temperature of 95 ° C., one pair of panty hose and 0.1% of the tannic acid and caffeine described in Example 1 were used per fiber weight.
owf, 0.5% owf, 1.0% owf, 3.0% o
wf, 5.0owf, 10.0% owf, 20.0% o
An aqueous solution containing a complex of tannic acid and caffeine obtained in the mixed aqueous solution by preparing the aqueous solution so that wf is 30.0% owf, and then mixing the aqueous solutions with stirring as shown in Table 2. It was treated in a bath ratio of 1:20 and a temperature of 80 ° C. for 20 minutes. Then 4.0% of the finish described in Example 1
Each panty hose was treated with a treatment bath of an aqueous solution containing owf at a bath ratio of 1:20 and a temperature of 40 ° C. for 15 minutes, then centrifugally dehydrated, and dried with warm air of 80 ° C. for 30 minutes to obtain sample N.
o. 9-No. I got 16.

The caffeine immobilization amount was measured using these samples, and the caffeine immobilization amount of the sample obtained by repeatedly washing 10 times and then drying was measured, and the washing durability was calculated. Is shown in Table 2. Further, the amount of immobilized caffeine of each sample obtained by the sustained release evaluation method was measured, and the results are shown in Table 2. Sample N using an aqueous solution containing tannic acid and caffeine at the respective concentrations of 30.0% owf
o. In No. 16, the pantyhose could not be treated sufficiently because the aggregation of the complex was so severe that the amount of caffeine immobilized and the sustained release were not measured.

[0025]

[Table 2]

From Table 2, sample No. 1 using an aqueous solution containing tannic acid and caffeine at respective concentrations of 0.1% owf. 9
The initial immobilization amount of caffeine was 0.01 mg / g, which was very small, and the washing durability was poor. Sample No. 1
0-No. In No. 15, as the concentration of the aqueous tannic acid solution and the aqueous caffeine solution increased, the immobilization amount of caffeine in the initial stage of processing also increased, and the washing durability thereof was 54.3% to 65.6.
%, And all the samples showed high washing durability. Also, the amount of caffeine immobilized on the sample washed with the cotton-attached white cloth containing the artificial sweat that had been subjected to the contact treatment with the method for evaluating the sustained release of caffeine was higher than that on the sample subjected to the washing durability. Since the degree of decrease is large and gradually decreases by washing,
It is clear that caffeine has a sustained release property against artificial sweat.

Example 3 Using the same tannic acid and caffeine as in Example 1, the aqueous caffeine solution was added while stirring the aqueous tannic acid solution, and the concentration of each tannic acid was 1.0% by weight. An aqueous solution containing a complex of caffeine and caffeine is prepared, and an immobilizing agent [trade name: deconal E is added to the aqueous solution.
X-810, manufactured by Nagase Chemtex Co., Ltd.] 100% cotton broad woven fabric [11.81t] which has been added and mixed with 2.0% by weight of polymerization and then subjected to quiking, desizing, scouring and bleaching under normal conditions.
ex x 11.81 tex / 144 (book / inch) x 76
(Pieces / inch)] was dipped and squeezed at a squeezing ratio of 100%, and then dried at a temperature of 120 ° C. for 10 minutes. Next, tartar [Product name: Reagent tartar, manufactured by Kanto Chemical Co., Ltd.] 1.0
Immerse in an aqueous solution of 10% by weight, squeeze at a squeezing rate of 100%, dry at a temperature of 120 ° C for 10 minutes, and further at 150 ° C
After heat treatment for 10 minutes, it was washed thoroughly with water and dried at a temperature of 120 ° C. for 10 minutes to obtain a sample No. I got 17.

The caffeine immobilization amount was measured using the obtained sample, the caffeine immobilization amount of the sample obtained by repeatedly washing 10 times and then drying was measured, and the washing durability was calculated. Further, the amount of immobilized caffeine of each sample obtained by the evaluation method of sustained release was measured, and the results are shown in Table 3.

[0029]

[Table 3]

From Table 3, it is clear that 100% cotton broad woven fabric can also fix caffeine and exhibit a sustained release effect. Since the woven fabric was treated with an aqueous tartar solution, it was not contaminated with tannic acid.

Example 4 Four pairs of pantyhose sewn after heat treatment in the same manner as in Example 1 were obtained. 2 pairs of pantyhose with acid dye [Kayanol Y
ellow N3R, Kayanol Red 3B
L, Kayanol Navy BlueR, manufactured by Nippon Kayaku Co., Ltd.] A dyeing bath containing 0.8% owf and ammonium sulfate 3% owf was dyed at a bath ratio of 1:20 and a temperature of 90 ° C., and then washed with water.
Then, the same treatment liquid containing 0.5% owf of tannic acid as in Example 1 was subjected to a fix treatment for 20 minutes at a bath ratio of 1:20 and a temperature of 80 ° C., and then 0.25% of the same tartarite as in Example 3.
Treatment liquid containing owf: 20 at bath ratio 1:20, temperature 80 ° C
Processed for a minute. Then, each panty hose was treated with the same treatment bath of an aqueous solution containing 3.0% owf of the same finishing agent as in Example 1 at a bath ratio of 1:20 and a temperature of 40 ° C. for 15 minutes.
After centrifugal dehydration, the sample was dried with warm air at 80 ° C. for 30 minutes, dyed with an acid dye concentration of 0.8% owf, and fixed with tannic acid. 18-No. I got 19.

Sample No. After washing 18 with warm water of 90 ° C. for 15 minutes, 0.5% of caffeine as in Example 1 was added.
After being treated with the treatment liquid containing f under the same conditions, treated with the same treatment bath of an aqueous solution containing 2.0% owf of the same finishing agent as in Example 1, and then subjected to centrifugal dehydration and a temperature of 80 ° C. After drying with air for 30 minutes, the sample No. I got 18 '.

Sample No. 19 was washed with warm water at 90 ° C. for 15 minutes, and tannic acid 0.5 was added under the same conditions as described above.
After treatment with a treatment liquid containing% owf, 0.25% tartarite
Treated with a treatment liquid containing owf under the same conditions, then treated with a treatment liquid containing 1.0% owf of caffeine, treated with a treatment bath of an aqueous solution containing 2.0% owf of a finishing agent, and then centrifugally dehydrated. , Sample No.
I got 19 '.

Similarly, the remaining two pairs of panty hose were treated with the same acid dyes as above, 2.3% owf and ammonium sulfate 3% ow.
After dyeing in a dyeing bath containing f under the same conditions, a fixing solution containing 1.0% owf of tannic acid was fixed under the same conditions as described above, and then a treating liquid containing 0.5% owf of tartarite. And then treated with the same treatment bath of an aqueous solution containing the same finishing agent 3.0% owf as described above under the same conditions, followed by centrifugal dehydration and drying with warm air at 80 ° C. for 30 minutes to obtain an acid dye concentration of 2 Sample No. 3 dyed with 3% owf and fixed with tannic acid 20-No. I got 21.

Sample No. After washing 20 with warm water at 90 ° C. for 15 minutes, caffeine 1.0% o under the same conditions as above
The sample No. was treated with a treatment liquid containing wf, treated with the same treatment bath of an aqueous solution containing 2.0% owf of the same finishing agent as in Example 1, then centrifugally dehydrated, and dried with hot air at 80 ° C. for 30 minutes. ．
I got 20 '.

Sample No. 21 was washed with warm water at 90 ° C. for 15 minutes, and then tannic acid 4.0% o was prepared under the same conditions as above.
After treatment with a treatment liquid containing wf, tartarite 2.0% owf
And then caffeine 5.0% ow
After treatment with the treatment liquid containing f, the same treatment bath as in Example 1 containing 2.0% owf of the finishing agent was used.
Centrifuge and dehydrate, and dry with warm air at 80 ° C for 30 minutes.
o. I got 21 '.

The immobilization amount of caffeine was measured using these samples, the immobilization amount of caffeine in the sample obtained by repeatedly washing 10 times and then drying was measured, and the washing durability was calculated. Is shown in Table 4. Further, the amount of immobilized caffeine of each sample obtained by the sustained release evaluation method was measured, and the results are shown in Table 4.

[0038]

[Table 4]

From Table 4, sample No. No. 1 in which panty hose dyed with an acid dye was fixed with tannic acid and tartar stone was used. 18 and sample No. Sample No. 20 obtained by processing an aqueous solution of caffeine. 18 'and sample N
o. The amount of immobilized caffeine of 20 'was the same as that of tannic acid described in Example 1 for sample No. 2 and sample No. Almost the same amount of caffeine as 3 was fixed, and washing 1
The amount of immobilization after 0 times, the washing durability and the sustained release showed almost the same results.

Sample No. in which panty hose dyed with an acid dye was fixed with tannic acid 1
9 and sample No. 21 was treated again with an aqueous tannic acid solution, then with an aqueous tartar solution, and then with an aqueous caffeine solution. The immobilized amount of caffeine in Sample No. 19 ′ and Sample No. 21 ′ is the same as that in Sample No. 1 described in Example 1. 3 and sample No. 3 Compared to 5, almost the same amount of caffeine was fixed, and the fixed amount after 10 washes and the durability of washing
Sustained release shows almost the same results, and it is clear that the total concentration of tannic acid used as a fixing agent and tannic acid further treated contributes to the amount of caffeine immobilized. Acid also contributes to the immobilization of caffeine.

Example 5 Two pairs of commercially available beige pantyhose [manufactured by Atsugi Co., Ltd.] were prepared and sample N was prepared.
o. It was set to 22. Further, two pairs of commercially available black pantyhose [manufactured by Atsugi Co., Ltd.] were prepared, and sample No. 23. Sample No. 22 and sample No. 22. 3 for each pair of 23
The sample was cut into pieces, treated with warm water at 95 ° C. for 15 minutes, and then dried, and the sample No. 22-1, sample No. 22-2, sample N
o. 22-3 and sample No. 22-3. 23-1, Sample No. 23
-2, sample No. 23-3 was obtained. Sample No. 22-1
And sample No. 23-1 is an aqueous solution containing 0.5% owf of the same aqueous caffeine solution as in Example 1, and the bath ratio is 1: 2.
Treatment at 0.degree. C. for 20 minutes at a temperature of 60.degree.
After treatment for 15 minutes at 0 ° C and 40 ° C, spin-drying is performed and
After drying with warm air of 0 ° C. for 30 minutes, the sample No. 22-1 '
And sample No. 23-1 'was obtained. Similarly, Sample 22-2 and Sample No. 23-2 is a caffeine aqueous solution 1.0% owf
Sample No. 22-2 'and sample No23-
I got 2 '. Similarly, the sample No. 22-3 and sample N
o. Sample No. 23-3 was treated with an aqueous caffeine solution of 3.0% owf, then with a finishing agent, centrifugally dehydrated and dried. 22-3 ′ and sample No. 23-3 'was obtained. The 6 samples thus obtained were used to measure the initial immobilization amount of caffeine and the immobilization amount of caffeine in the samples obtained by repeatedly washing 10 times and drying, and the results are shown in Table 5.

[0042]

[Table 5]

From Table 5, sample No. 22-1'-No. Two
The initial immobilized amount of 2-3'caffeine is 0.091-
0.097 mg / g, and the amount of immobilization after washing 10 times was also 0.
It was as low as 067 to 0.069 mg / g, and it was confirmed that this panty hose had a small amount of tannic acid used in the fixing treatment after dyeing. In addition, the sample No. Two
The initial amount of caffeine immobilized in 3-1 'is 0.095 mg /
As low as g, the initial immobilization amount of caffeine in samples No23-2 'to No23-3' is 0.205 mg / g to 0.21.
Since it was a sufficiently high value of 1 mg / g, it was confirmed that the tannic acid used for the fixing treatment after dyeing remained sufficiently.

Based on the above results, in order to set the amount of caffeine immobilized to 0.2 mg / g, the remaining pair of beige-colored pantyhose contained the same tannic acid 0.5% owf as in Example 1. After the same treatment with the treatment liquid containing
The same treatment as in Example 1 was conducted using the same treatment liquid containing 1.0% owf of caffeine, centrifugally dehydrated, and dried to obtain Sample N.
I got o22 '. Further, the remaining one pair of black panty hose was not treated with the aqueous tannic acid solution, but was similarly treated with a treatment liquid containing 1.0% owf of caffeine, centrifugally dehydrated and dried to obtain Sample No. I got 23 '.

Using these samples, the amount of immobilization of caffeine in the initial stage of processing and the amount of immobilization after 10 times of washing were measured to calculate the washing durability, and the cafe was obtained by the evaluation method of sustained release. The immobilization amount of in was measured, and the results are shown in Table 6.
It was shown to.

[0046]

[Table 6]

As is clear from Table 6, with regard to the pantyhose available on the market, a fiber product having a desired immobilization amount of caffeine was obtained.

[0048]

INDUSTRIAL APPLICABILITY The present invention is a method of immobilizing caffeine on a textile product using tannic acid, and the textile product obtained by this method is a cafe which ordinary textile products do not have in the field of clothing. It is a textile product that has a fixed inn, has an effect of excellent washing durability, and has excellent texture and hygroscopicity. Further, the immobilized caffeine can be expected to be gradually released to the skin of the human body by an ionic liquid such as sweat and taken into the skin to exert a skin care effect.

Claims (5)

[Claims] 1. A method for producing a textile product, which comprises treating the textile product with tannic acid and caffeine. 2. A textile product is treated with an aqueous tannic acid solution,
Next, the method for producing a textile product according to claim 1, wherein the textile product is treated with an aqueous caffeine solution. 3. The complex of tannic acid and caffeine is prepared in an aqueous solution in which tannic acid and caffeine are mixed, and the fiber product is treated with the complex-containing aqueous solution. Textile manufacturing method. 4. A method for producing a textile product, which comprises treating a textile product after dyeing and fixed with tannic acid with an aqueous tannic acid solution, and then with an aqueous caffeine solution. 5. A method for producing a textile product, which comprises treating a textile product after dyeing and fixed with tannic acid with an aqueous caffeine solution.