WO2013005280A1 - Method for producing polyphenol processed fibers - Google Patents

Abstract

Polyphenol processed fibers are obtained bringing fibers into contact with polyphenols and then treating the fibers with an anionic aqueous dispersion of a phenylamide compound. The polyphenols comprise tea-derived polyphenols and/or grape-derived polyphenols, the aqueous dispersion has a polymer component that will disperse, and a polymer component having anions can be used as the polymer component. Furthermore, at least one of antifoaming treatment and acidic post-treatment is further performed in order to control fading as a result of repeated washing. Antifoaming treatment involves exposure to an antifoaming agent during colorfast treatment and acidic post-treatment is treatment of the colorfast fibers using a weakly acidic aqueous solution.

Description

Method for producing polyphenol processed fiber

The present invention relates to a method for producing a polyphenol-processed fiber that can impart to a fiber a dyed color with high fastness by dyeing using a polyphenol compound that is a natural component contained in plants, and in particular, chlorine caused by a water treatment agent or the like. The present invention relates to a method for producing a polyphenol-processed fiber having chlorine fastness capable of maintaining a good dyed color even when washed with contained tap water and durability against repeated washing.

Polyphenol compounds contained in plants and the like are used as natural pigments for traditional plant dyeing. In recent years, processing technology has been developed to fix polyphenols to fibers and impart their functionality (antibacterial properties, etc.) to the fibers. 1) Padding process using binder resin, 2) Metal mordanting using industrial metal salts 3) Technology such as dip dyeing using cationic polymers. In such plant dyeing technology and polyphenol processing, maintaining color fastness while maintaining color development or functionality is an essential condition for commercialization and widespread use. Advances have been made in techniques to improve and develop functions.

However, plant dyeing is a traditional technique that has been carried out since before the development of the water supply and has been passed on since the development of the water supply, so it is not assumed that the dyed cloth will be exposed to chlorine. Also, in polyphenol processing technology that has been developed in recent years, it is common that the requirements of the final delivery destination presented in business customs do not include chlorine resistance, and special features such as swimwear used in pools. Except for special applications, there is little demand for technical studies on chlorine resistance. For this reason, in plant dyeing and polyphenol processing technologies, fastness regarding items such as light resistance, washing, sweat, and friction are examined, but attention is not paid to durability against chlorine, and improvement of chlorine fastness. Has not been fully studied.

On the other hand, with regard to textile dyeing for clothing by general chemical dyeing, as an existing method for improving chlorine fastness, a method of treating with diamines and / or tannic acid (for example, Patent Document 1 below), polycationic substance A method using (ε-polylysine) (for example, the following Patent Document 2), a method for treating with a resin and a thiourea derivative (for example, the following Patent Document 3), a method for treating with a resin and urea or a guanidine compound (for example, Patent Document 4), a method using an allylamine polymer (for example, Patent Document 5 below), a method using a polymer obtained by condensing a polyethylene polyamine and an epihalohydrin (for example, Patent Document 6 below), an epihalohydrin-hydrazide compound. A method using a condensate of (for example, Patent Document 7 below) has been proposed. Further, as a fixing agent for improving chlorine fastness, a cotton reactive dyeing fixing agent, a synthetic tannin-based natural tannin-based fixing agent, and the like are commercially available.

JP-A-56-96971 JP 2006-37324 A JP 50-58374 A Japanese Patent Publication No.57-29593 JP 58-31185 A JP 55-152879 A JP-A-5-195449

In modern consumer life, washing at home is generally done with tap water, so there are many opportunities for textiles to be exposed to chlorine. Therefore, it is necessary to make the textiles widely resistant to chlorine, and it is important to improve the chlorine fastness in a wide range not only for special purposes, but also in plant dyeing and polyphenol processing techniques.

In order to improve the chlorine resistance of plant-dyed and polyphenol-processed fibers, using the above-mentioned fix agent for improving the fastness of chlorine for chemically dyed textile clothing products, the light resistance deteriorates in exchange for the improvement of chlorine resistance. Or a change in hue, or a problem such as polyphenol detachment from the fabric occurs. Further, in the case of a synthetic tannin-based or natural tannin-based fixing agent, the fixing agent itself is dark brown, so processing discoloration becomes a problem, and it is easy to be restricted in color when used.

Therefore, it is necessary to find a treatment method that can improve the fastness of chlorine of vegetation dyeing and polyphenol processed fibers without causing the above-mentioned problems. Further, it is necessary to realize a processing method capable of imparting durability that hardly causes discoloration even after repeated washing.

The object of the present invention is to improve the chlorine resistance while maintaining the color developability, functionality, safety, light resistance, and washing resistance when processing polyphenols into the fibers, and suppress discoloration due to repeated washing, It is to provide a polyphenol-processed fiber having fastness suitable for modern consumer life.

In order to solve the above-mentioned problems, various treatment agent components used in the treatment of dyed fibers have been studied, and the chlorine fastness of polyphenol processed fibers is improved by utilizing components used as processing aids. In addition, the present inventors have found that the discoloration due to repeated washing can be suppressed by applying an antifoaming treatment or an acidic post-treatment, and have reached the method for producing a polyphenol processed fiber of the present invention.

According to one aspect of the present invention, a method for producing a polyphenol-processed fiber includes a fastening treatment in which a fiber in contact with polyphenol is treated with an anionic aqueous dispersion of a phenylamide compound, an antifoaming treatment, and an acidic post-treatment. The antifoaming treatment causes an antifoaming agent to act during the fastening treatment, and the acidic posttreatment comprises treating the fiber after the fastening treatment with an acidic aqueous liquid. Is the gist.

According to the present invention, it is possible to improve the chlorine resistance while maintaining the color developability, functionality, safety, light resistance, and washing resistance of the polyphenol-processed fiber. Improved polyphenol processed fiber can be provided. Therefore, it is useful for application development of products that utilize the functionality of polyphenols, and not only for clothing in general, but also for the addition of polyphenol functions such as antibacterial, deodorant, and antioxidant properties to various products that use fibers. It becomes possible to provide high quality products.

The discoloration of the dyed fiber due to chlorine is due to oxidative discoloration due to active chlorine, and in particular, cotton is more prone to problems than other fibers because the fiber has the property of adsorbing active chlorine.

Polyphenols are known as antioxidants. In other words, polyphenols easily react with oxidizing substances, and are therefore susceptible to oxidative fading due to active chlorine. In fact, when we measure chlorine fastness (JIS L0884, chlorinated water fastness test A method) for plant-dyed products and conventional polyphenol-treated fibers, it becomes a very low grade judgment from grade 1 to grade 2, It is clear that the polyphenol of the polyphenol processed fiber has low chlorine resistance.

When a conventional fixing agent for improving the fastness of chlorine is used for a polyphenol processed fiber, a hue change may occur, which is an effect caused by a pH change. In addition, polyphenol may be detached from the dough, which is due to the action of the cationic substance, and the cationic substance and polyphenol may combine to form an aggregate to contaminate the dough. Since both are related to the properties of the phenolic hydroxyl group, it is necessary to fully consider the characteristics of the phenolic hydroxyl group when improving the chlorine resistance of the polyphenol processed fiber.

With regard to the above points, it has been found that a phenylamide compound in a specific state is useful for improving the chlorine fastness of a polyphenol processed fiber, and the fiber contacted with polyphenol is treated with the phenylamide compound. The present inventors have found that it is possible to provide a polyphenol-processed fiber with improved chlorine resistance while maintaining color development, functionality, safety, light resistance and washing resistance. Furthermore, in order to improve washing durability of polyphenol processing, defoaming treatment and acidic post-treatment are effective. By applying at least one of these treatments, discoloration due to repeated washing can be suppressed. I found out. The defoaming treatment is a treatment in which an antifoaming agent is allowed to act during polyphenol processing, and the dyeing strength is improved by the polyphenol easily fixing to the fiber. The acidic post-treatment is a treatment in which an acidic aqueous liquid is brought into contact with the fiber after the fastening treatment, and by finally ensuring the ionization suppression of the phenolic hydroxyl group of the polyphenol on the fiber, the coloration of the polyphenol is further stabilized. Turn into.

Hereinafter, a method for producing the polyphenol processed fiber of the present invention will be described. In the following description, polyphenol-processed fibers widely include fibers having polyphenol on the fibers, including general plant-dyed products, etc., and the types of dyeing or polyphenol processing, natural fibers or chemical fibers It doesn't matter. Specifically, as polyphenols that can be used, it is commonly used for plant dyeing and polyphenol processing, as well as tea, grapes, pomegranates, grapes, guava, rose hips, buckwheat, red beans, olives, apples, perilla, loquat leaves. , Polyphenols extracted from leaves, fruits, seeds, flowers, stems, roots, and the like of various plants such as strawberries, chestnuts, coffee, cinnamon, berries, etc., can be selected as appropriate. As tea polyphenol, those contained in fresh leaves, processed tea (non-fermented tea, semi-fermented tea, fermented tea), extract extract, extract powder, post-extraction residue, etc. can be used, and the form is not limited. Tea polyphenols and grape polyphenols are particularly excellent in their functionality and are preferred. Also, the types of fibers that can be used are cellulose fibers, animal fibers, polyester fibers, acetate fibers, nylon fibers, acrylic fibers, rayon fibers, polypropylene fibers, polyvinyl chloride fibers, polylactic acid fibers, polyurethane fibers, etc. Examples thereof include fibers, and the present invention can be applied by appropriately selecting them.

If the polyphenol contacted with the fiber has a polar group on the fiber surface, it will coordinate and interact with the hydroxyl group of the polyphenol via a hydrogen bond or ionic bond, thereby fixing and stabilizing the polyphenol on the fiber. It is thought to act to supplement In order to improve the chlorine fastness of the polyphenol-processed fiber, it is necessary to protect the polyphenol without breaking such bonds.

In the present invention, as a treating agent for improving (fastening) chlorine fastness, an aqueous dispersion of a phenylamide compound having an ester group is a weak dispersion that coexists in and out of the molecule of the phenylamide compound. Those containing acidic anions are used. The mechanism by which the fastening treatment agent used in the present invention improves the chlorine fastness is considered as follows.

Although the reaction mechanism of the antioxidant action of polyphenols has not been completely elucidated, there are a reaction based on hydrogen atom transfer of a phenolic hydroxyl group and a reaction based on electron transfer as part of the mechanism. In the reaction by hydrogen atom transfer, the hydrogen atom radical supplied from the hydroxyl group reacts with the active chlorine radical and deactivates, and proceeds in an aprotic medium, whereas the reaction by electron transfer is supplied from the hydroxyl group. The active chlorine radical accepts the generated electrons and deactivates them as chlorine ions, which proceeds in a protic medium, and the reaction is promoted by metal ions. In an aqueous system where plant dyeing or polyphenol processing is applied, the supply of anions makes it possible to suppress the ionization of phenolic hydroxyl groups, and thus contributes to improving the chlorine fastness of polyphenols by suppressing the electron transfer of phenolic hydroxyl groups. Conceivable. At this time, when the anion to be used is a weakly acidic anion such as a carboxylic acid group or a phosphoric acid group, a change in the colorability of the polyphenol due to a change in pH is suppressed. In the case of an anion dissolved in the medium, it can penetrate into the fiber and affect the dyeing of the polyphenol itself, but this point can be solved by using a dispersible anion, and from the periphery of the polyphenol on the fiber. Acts gently.

The phenylamide compound has a molecular structure with low water solubility and easy coagulation due to the hydrophobicity of the phenyl group and the poor solubility of the amide group and the firm phenylamide skeleton. Polarity is added and it becomes easy to liquefy, and it becomes easy to constitute an aqueous emulsion. The phenyl group has an affinity for polyphenols and is considered to physically protect the polyphenols by blocking the contact of chlorine with a hydrophobic barrier adjacent to the polyphenols. Accordingly, the weakly acidic anion coexists in and out of the molecule of the phenylamide compound, thereby effectively acting to suppress ionization of the phenolic hydroxyl group and to protect the hydrophobicity of the polyphenol.

In accordance with the above, the phenylamide compound specifically has a phenylamide skeleton, and has substituents bonded to the nitrogen atom and the carbonyl carbon atom of the amide group, respectively, each of these substituents having a carbon number. 1 to 50 chain or cyclic saturated aliphatic groups which may contain an oxygen atom and / or a nitrogen atom, and may be bonded with an aromatic group. The at least one substituent includes an ester group, and the ester group may be a chain or may form a cyclic group. It is preferable that the substituent has an ether bond because the flexibility of the molecule is improved. The phenyl group of the phenylamide skeleton may be substituted with one or more methyl groups or halogen atoms, and the effect of eliminating active chlorine is enhanced by the bulk of the molecule. Anionic aqueous dispersions of the phenylamide compounds as described above are available on the market. For example, Takeuchi Shoten Co., Ltd. (Tokyo Branch: 2-2-47 Kamikoido, Suginami-ku, Tokyo) is available. Anion-made phenylamide fiber processed material (product number: ITN003M), Amorden (trade name) series fiber treatment agent manufactured by Daiwa Chemical Industry Co., Ltd. (3-1-11 Kamishinjo, Higashiyodogawa-ku, Osaka-shi, Osaka) . It can select from such a product suitably and can be used as a toughening processing agent in this invention. Specific examples of phenylamide compounds include metalaxyl [methyl N- (2-methoxyacetyl) -N- (2,6-xylyl) -DL-alaninate], oxadixyl [2-methoxy-N- (2-oxo-1 , 3-Oxazolidin-3-yl) aceto-2 ′, 6′-xylidide], off-race [(±) -α-2-chloro-N- (2,6-xylylacetamido) -γ-butyrolactone], Benalaxyl [methyl N-phenylacetyl-N- (2,6-xylyl) -DL-alaninate], furalaxyl [methyl N- (2-furoyl) -N- (2,6-xylyl) -DL-alaninate], cyprofuran [(±) -α- {N- (3-chlorophenyl) cyclopropanecarboxamide} -γ-butyrolactone] and the like, which are compounds that can also be used as an antibacterial agent component.

The fastening treatment agent used in the present invention may further contain a water-dispersible polymer component as long as the action of the phenylamide compound and the anion is not inhibited, and an anionic system containing a carboxy group or a phosphate group. The polymer or the like acts as a carrier for supplying an anion. It also acts as a physical protector for polyphenols. From such a point, preferred polymer components include polymers such as acrylic polymers or copolymers containing a carboxy group in the molecule or outside the molecule. Accordingly, as the fastening treatment agent in the present invention, for example, an aqueous dispersion containing a phenylamide compound based on an anionic polymer dispersion such as an anionic acrylic resin emulsion mixed with the phenylamide compound. Can be suitably used. In such a polymer dispersion, the anion and the phenylamide compound do not dissolve in water and exist together with the dispersed polymer, so that they do not easily penetrate into the inside of the fiber, and contact from the outer periphery of the polyphenol on the fiber surface. Works. Therefore, it is possible to avoid taking the polyphenol dyeing seat from the inside of the fiber and detaching the polyphenol, and it acts gently from the dispersed particles and does not cause a rapid change in the polyphenol. From the viewpoint of dispersion stability and the like, the fastening treatment agent preferably has a non-volatile content concentration of about 1 to 50% by mass, preferably 5 to 30% by mass. Is about 1.0 to 7.0, preferably about 2.5 to 5.5. The nonvolatile component includes a phenylamide compound, an anion component (when present separately from the phenylamide compound), and the above-described polymer component.

¡By bringing the above-mentioned fastening agent into contact with the fiber dyed or processed with polyphenol, the chlorine fastness of the polyphenol on the fiber is improved. Fastening with the treatment agent may be performed after the polyphenol comes into contact with the fiber. After the polyphenol is dyed or processed, the polyphenol may be applied individually after removing the extra polyphenol, or continuously after the dyeing or processing. May be performed in a state where coexists. That is, the treatment agent may be added to a bath in which polyphenols are dyed on fibers. The fastening treatment is desirably performed at a weakly acidic to neutral pH of 4.1 to 7.0.

Polyphenol processed fiber is obtained by bringing the fiber into contact with an aqueous solution of polyphenol, dyeing the polyphenol, and washing away the excess polyphenol with water. The surface of the fiber is activated by bringing the agent and, if necessary, an alkali into contact with the fiber, and after sufficiently washing with water, polyphenol processing is applied. The polyphenol processing of cotton is implemented as follows, for example.

Specifically, the fiber fabric that has undergone refining and bleaching is soaked in water, and an aqueous cationic agent solution is added at a ratio of about 10% by mass with respect to the fiber and brought into contact with the fiber for about 10 minutes. After adding and impregnating at a ratio of about 2% by mass with respect to the fiber, the temperature is gradually raised to about 80 ° C. and maintained for about 30 minutes. Thereafter, it is sufficiently washed with water, and the fiber is immersed again in water. The polyphenol is about 0.1 to 7% by mass, preferably 0.3 to 2% by mass, more preferably 0.5% by mass with respect to the fiber. A polyphenol aqueous solution is added at a ratio of approximately, heated to about 30 ° C., dyed on the fiber for about 20 minutes at pH 6-7, washed with water to remove excess polyphenol.

When fastening with the above-mentioned treatment agent as post-processing of the polyphenol-processed fiber, the fastening treatment agent is added to the fiber soaked in water, and the pH is 4.5 or more weakly acidic region (less than pH 7), preferably pH 6 To 6.9), the polyphenol-processed fibers are brought into contact with each other and heated to about 35 to 95 ° C., preferably about 50 to 80 ° C., more preferably about 60 ° C., whereby the fastening treatment is suitably performed. The addition amount of the fastening treatment agent is set to be about 0.1 to 10% by mass, preferably about 0.5 to 7% by mass, and more preferably about 1 to 3% by mass with respect to the fiber. The time is generally about 10 to 60 minutes, preferably around 30 minutes, and the treated fibers are thoroughly washed with water.

When fibers such as cotton, from which polyphenols are easily detached, are toughened with the above-mentioned treatment agent in the same bath continuously with polyphenol processing, they can be treated in the range of pH 3 to 11, and the properties of polyphenols can be reduced. In consideration, a weakly acidic range of pH 4.1 or higher (less than pH 7) is preferable. In the treatment in the same bath, it is preferable to use a mordant in order to increase the affinity of the polyphenol with respect to the fibers to facilitate fixing. For example, it can be carried out using sodium stannate as a metal mordant as follows.

Specifically, the fiber fabric that has undergone refining and bleaching is immersed in water, and the polyphenol aqueous solution has a polyphenol content of about 0.1 to 7% by mass, preferably about 0.5 to 3.0% by mass, based on the fiber. The polyphenol is first contacted with the fiber by adding in proportions. Thereafter, the mixture is heated to a temperature of about 35 to 95 ° C., preferably about 80 to 95 ° C., and an aqueous solution in which citric acid and sodium stannate are dissolved is about 1 to 10% by mass of citric acid, preferably about Is added at a ratio of about 2 to 4% by mass, sodium stannate about 0.5 to 5% by mass, preferably about 1 to 2% by mass and maintained for about 10 minutes to dye the polyphenol. Thereafter, the fastening treatment agent is added, and the treatment agent is kept for about 30 minutes while maintaining the temperature at about 35 to 95 ° C., preferably about 80 to 95 ° C. at about pH 3 to 11, preferably about 4 to 5. It can process suitably when it is made to contact. The treated fiber is washed with water as appropriate. The addition amount of the fastening treatment agent may be set to be about 0.2 to 7% by mass, preferably about 0.5 to 3% by mass with respect to the fiber.

The antifoaming treatment that improves the washing durability of the polyphenol processing is a treatment in which an antifoaming agent acts during the polyphenol processing. The antifoaming agent is added to the aqueous liquid during the polyphenol processing, and the polyphenol is added in the presence of the antifoaming agent. Is brought into contact with the fiber, so that contact inhibition by bubbles or residual air in the fiber is reduced and dyeing proceeds easily. The dyeing strength is improved by the fact that the polyphenol is easily fixed on the fiber. Even in the case of using an antifoaming agent, the fastening treatment may be performed continuously with the polyphenol processing or as a post-processing.
As an antifoaming agent generally applied to an aqueous liquid, there are an organic antifoaming agent and a silicone antifoaming agent, and the organic antifoaming agent includes a surfactant type antifoaming agent and an emulsion type antifoaming agent. Examples of silicone antifoaming agents include oil compound types, emulsion types, and self-emulsifying types. Also in the present invention, it can be appropriately selected from antifoaming agents that are generally applicable to aqueous liquids. Specifically, as an active ingredient of an organic antifoaming agent, higher alcohols such as 2-ethylhexanol, fatty acid esters such as sorbitan ester, ethers such as diisooctyl ether, ethoxy group or propoxy group are repeatedly used. Examples include ether-type, ester-type, ether-ester-type, and ester-ester-type polymers contained as units. Examples of the active ingredient of the silicone-based antifoaming agent include methylpolysiloxane, dimethylpolysiloxane, polysiloxane having a polyether chain or a polypropylene-modified polyether chain introduced at the terminal, such as ethylene oxide-modified polysiloxane. Various antifoaming products using the active ingredients as described above are provided on the market, and can be appropriately selected and used from them. In the case where the fastening treatment is performed continuously after the polyphenol processing, a nonionic and dispersible antifoaming agent is preferable in order not to disturb the dispersibility and ionicity of the fastening treatment agent. An emulsifying silicone antifoaming agent is preferably used. The use amount of the antifoaming agent is preferably set to a ratio of about 0.05 to 3%, more preferably about 0.1 to 1% with respect to the fiber weight.

The acidic post-treatment for improving the washing durability of the polyphenol processing is a treatment in which an acidic aqueous liquid is brought into contact with the fiber after the fastening treatment, and the pH of the fiber is 2.5 to 5.5, preferably 3.0. Adjust to ~ 4.0. The acidic post-treatment is performed separately from the fastening treatment. In other words, it is preferable to remove the treatment liquid from the fastened fiber and wash it with water as necessary, in a state where there is no surplus hardening agent or the like. By acidifying the polyphenol and the phenylamide compound on the fiber surface in a stable state, ionization of the phenolic hydroxyl group of the polyphenol is effectively suppressed. The acidic aqueous liquid used for the acidic post-treatment is an aqueous solution of a weak acidic compound, and various organic acids and phosphoric acid compounds can be used as the weak acidic compound. Specifically, formic acid, acetic acid, propionic acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, oleic acid, fumaric acid, maleic acid, glycolic acid, lactic acid, tartronic acid, glyceric acid, 1-, 2-, 3- or γ-hydroxybutyric acid, malic acid, tartaric acid, citramalic acid, citric acid, isocitric acid, leucine acid, mevalonic acid, pantoic acid, ricinoleic acid, ricinaleic acid, cerebronic acid, quinic acid, shikimic acid, ascorbine Water-soluble aliphatic carboxylic acids such as acids and hydroxy acids, and phosphoric acid compounds such as phosphoric acid can be suitably used, and citric acid is particularly preferred from the viewpoint of cost, fragrance, skin irritation and the like. The weak acidic compound concentration in the acidic aqueous liquid is preferably about 0.05 to 3 g / L, more preferably about 0.1 to 1 g / L. The fiber is sufficiently immersed in the acidic aqueous liquid and held for a certain period of time, preferably heated to about 30 to 80 ° C., more preferably about 50 ° C., preferably about 0.5 to 30 minutes, more preferably 10 It is good to hold about minutes.
By applying at least one of the above-described defoaming treatment and post-acidification treatment, the coloration stability of the polyphenol is increased, and discoloration due to repeated washing is suppressed. When both treatments are performed, durability against repeated washing is further improved.

The polyphenol processed fiber subjected to the above-mentioned fastening treatment has improved chlorine fastness to about the third grade. In addition, the Kawai-type patch test shows semi-negative, and even in the Oeko-Tex dissolution test, heavy metals and pesticide components are below the detection limit, so safety is high. The anti-bacterial properties, deodorizing properties, and antioxidant properties that are functions of polyphenols are also exhibited well, and the UV cut effect is also suitable. Furthermore, by applying at least one of defoaming treatment and post-acidification treatment, discoloration due to repeated washing is suppressed, and JIS L0804 dyeing fastness test grade determination with a gray scale for discoloration is improved to grade 4 or higher. .

In accordance with the following operations, polyphenol processed fibers (samples 1 to 5), polyphenol processed fibers that have been fastened with phenylamide (samples 1A, 2A to 2C, 3A to 6A) and polyphenol processed that have been processed with a commercially available fix agent Fibers (Samples 7 to 9) were prepared and examined for the fastness of chlorine and the presence or absence of color change of the polyphenol.

(Sample 1)
1 kg of cotton fabric subjected to refining and bleaching was immersed in about 15 L of water in a dyeing bath and sufficiently impregnated with water. To this was added 100 g of a cationic agent (trade name: Cationone KCN, manufactured by Otsuka Kogyo Co., Ltd., quaternary ammonium salt) and stirred for 10 minutes. Further, a solution in which 20 g of sodium hydroxide was dissolved in about 1 L of water was prepared, added to the dye bath, and stirred for 10 minutes. About 3 L of water was added to adjust the amount of liquid in the dye bath to 20 L, heated to 80 ° C., and the cotton fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dyebath solution was discharged, and the washing water was discharged while the cotton fabric was carefully washed with running water and neutralized.

About 15 L of water was poured into the dye bath to immerse the cotton fabric. 5 g of tea-extracted polyphenol (trade name: Teafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water and added to the dye bath, and water was added to adjust the amount of the dye bath to 20 L. This was heated and heated up to 30 ° C., and the cotton fabric was sufficiently immersed while maintaining the temperature and stirring for 30 minutes. Thereafter, the dyebath solution was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric.

The light fastness (JIS L0842) and chlorine fastness (JIS L0884 A method) of the polyphenol-treated cotton fabric obtained above were measured. The light fastness was grade 3 and the chlorine fastness was grade 1-2.

(Sample 1A)
1 kg of the polyphenol-treated cotton fabric obtained in Sample 1 was immersed in about 15 L of water in a dye bath and sufficiently impregnated with water. To this, 20 g of a dispersible phenylamide treating agent (trade name: ITN003M, Takeuchi Shoten Co., Ltd., anionic phenylamide fiber processing agent, resin-containing acidic aqueous solution) was added and stirred for 10 minutes. Water was added to adjust the amount of the dye bath to 20 L (pH 6.7). This was heated and heated up to 50 ° C., and the cotton fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dyebath solution was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric after phenylamide treatment.

The light fastness and chlorine fastness of the obtained polyphenol-treated cotton fabric were measured. The light fastness was grade 3 and the chlorine fastness was grade 3.

(Sample 2)
1 kg of cotton fabric subjected to refining and bleaching was immersed in about 15 L of water in a dyeing bath and sufficiently impregnated with water. To this, 5 g of tea-extracted polyphenol (trade name: Teafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water, and this was heated and heated to 80 ° C. An aqueous solution prepared by dissolving 10 g of sodium stannate and 20 g of citric acid in about 1 L of water is added to the dyeing bath, water is added to adjust the amount of the dyeing bath to 20 L, and cotton is stirred at 80 ° C. for 30 minutes. The dough was fully immersed. Thereafter, the dyebath solution was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric.

The light fastness and chlorine fastness of the polyphenol-treated cotton fabric obtained above were measured. The light fastness was grade 3 and the chlorine fastness was grade 2-3.

(Sample 2A)
1 kg of cotton fabric subjected to refining and bleaching was immersed in about 15 L of water in a dyeing bath and sufficiently impregnated with water. To this, 5 g of tea-extracted polyphenol (trade name: Teafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water, and this was heated and heated to 80 ° C. An aqueous solution obtained by dissolving 10 g of sodium stannate and 20 g of citric acid in about 1 L of water is added to the dyeing bath, water is added to adjust the amount of the dyeing bath to 20 L, and cotton is stirred at 80 ° C. for 10 minutes. The dough was fully immersed. To this was added 30 g of a dispersible phenylamide treatment agent (trade name: ITN003M, Takeuchi Shoten Co., Ltd., anionic phenylamide fiber processing agent, resin-containing acidic aqueous solution) (pH 4.5), 80 ° C. For 30 minutes. Thereafter, the dye bath was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a phenylamide-treated polyphenol-treated cotton fabric.

The light fastness and chlorine fastness of the obtained polyphenol-treated cotton fabric were measured. The light fastness was grade 3 and the chlorine fastness was grade 3-4.

(Sample 2B)
In the operation of Sample 2A, a phenylamide-treated polyphenol-treated cotton fabric was prepared in the same manner except that the amount of the dispersible phenylamide treatment agent added to the dye bath was changed from 30 g to 100 g. In the dye bath to which a dispersible phenylamide treating agent was added, the solution had a pH of 4.4.

The obtained polyphenol-treated cotton fabric was measured for chlorine fastness and found to be 3-4 grade. However, during the hardening process, the treatment liquid overflowed due to foaming that seems to be caused by excess of the treatment agent, which was a problem in terms of work.

(Sample 2C)
In the operation of Sample 2A, a phenylamide-treated polyphenol-treated cotton fabric was prepared in the same manner except that the amount of the dispersible phenylamide treatment agent added to the dye bath was changed from 30 g to 1 g. In the dye bath to which the acidic phenylamide treating agent was added, the solution had a pH of 5.1.

When the chlorine fastness of the obtained polyphenol-treated cotton fabric was measured, it was grade 3. However, the fabric color was slightly dull, which may be caused by the pH of the treatment liquid in the fastening treatment.

(Sample 3)
1 kg of the smelted polyester fabric was immersed in about 15 L of water in a dye bath and sufficiently impregnated with water. To this was added 70 g of a cationic agent (trade name: Cationone KCN, manufactured by Otsuka Kogyo Co., Ltd., quaternary ammonium salt) and stirred for 10 minutes. Further, about 3 L of water was added to adjust the amount of liquid in the dye bath to 20 L, heated to 50 ° C., and the polyester fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dyebath solution was discharged, and the washing water was discharged while the fabric was carefully washed with running water and neutralized.

About 15 L of water was poured into the dye bath to immerse the polyester fabric. 10 g of tea-extracted polyphenol (trade name: Theafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water and poured into the dye bath, and water was added to adjust the liquid volume of the dye bath to 20 L. This was heated up to 50 ° C., and the polyester fabric was sufficiently immersed while stirring for 20 minutes while maintaining the temperature. Thereafter, the dye bath was discharged, the polyester fabric was carefully washed with running water, the fabric was taken out, dehydrated and dried to obtain a polyphenol-treated polyester fabric.

The light fastness and chlorine fastness of the polyphenol-treated polyester fabric obtained above were measured. The light fastness was grade 3 and the chlorine fastness was grade 2-3.

(Sample 3A)
1 kg of the polyphenol-treated polyester fabric obtained in Sample 3 was immersed in about 15 L of water in a dye bath and sufficiently impregnated with water. To this, 20 g of a dispersible phenylamide treating agent (trade name: ITN003M, Takeuchi Shoten Co., Ltd., anionic phenylamide fiber processing agent, resin-containing acidic aqueous liquid) was added and stirred for 10 minutes, and water was added. Then, the amount of the dye bath was adjusted to 20 L (pH 6.7). This was heated and heated up to 80 ° C., and the polyester fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dye bath was discharged, the polyester fabric was carefully washed with running water, the fabric was taken out, dehydrated and dried to obtain a polyphenol-treated polyester fabric after phenylamide treatment.

The light fastness and chlorine fastness of the resulting polyphenol-treated polyester fabric were measured. The light fastness was grade 3 and the chlorine fastness was grade 3-4.

(Sample 4)
1 kg of the refined nylon fabric was immersed in about 15 L of water in a dye bath and sufficiently impregnated with water. 5 g of tea-extracted polyphenol (trade name: Teafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water and added to the dye bath, and water was added to adjust the amount of the dye bath to 20 L. This was heated to 80 ° C., and the nylon fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dye bath was discharged, the nylon fabric was carefully washed with running water, the fabric was taken out, dehydrated and dried to obtain a polyphenol-treated nylon fabric.

When the chlorine fastness of the polyphenol-treated nylon cloth obtained above was measured, it was grade 4.

(Sample 4A)
1 kg of the refined nylon fabric was immersed in about 15 L of water in a dye bath and sufficiently impregnated with water. 5 g of tea-extracted polyphenol (trade name: Theafuran 30F, manufactured by ITO EN Co., Ltd.) is dissolved in about 1 L of water and poured into a dyeing bath. Product name: ITN003M, Takeuchi Shoten Co., Ltd., anionic phenylamide fiber processing agent, resin-containing acidic aqueous liquid) 30 g is added and stirred for 10 minutes, water is added to bring the dye bath volume to 20 L Adjusted (pH 6.7). This was heated to 80 ° C., and the nylon fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dye bath was discharged, the nylon fabric was carefully washed with running water, the fabric was taken out, dehydrated and dried to obtain a polyphenol-treated nylon fabric after phenylamide treatment.

When the chlorine fastness of the obtained polyphenol-treated nylon cloth was measured, it was grade 4.

(Sample 5)
1 kg of cotton fabric subjected to refining and bleaching was immersed in about 15 L of water in a dyeing bath and sufficiently impregnated with water. To this was added 100 g of a cationic agent (trade name: Cationone KCN, manufactured by Otsuka Kogyo Co., Ltd., quaternary ammonium salt) and stirred for 10 minutes. Further, a solution in which 20 g of sodium hydroxide was dissolved in about 1 L of water was prepared, added to the dye bath, and stirred for 10 minutes. About 3 L of water was added to adjust the amount of liquid in the dye bath to 20 L, heated to 80 ° C., and the cotton fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dyebath solution was discharged, and the washing water was discharged while the cotton fabric was carefully washed with running water and neutralized.

About 15 L of water was poured into the dye bath to immerse the cotton fabric. Grape polyphenol (5 g) was dissolved in about 1 L of water and poured into a dye bath, and water was added to adjust the amount of the dye bath to 20 L. This was heated and heated up to 30 ° C., and the cotton fabric was sufficiently immersed while stirring for 20 minutes while maintaining the temperature. Thereafter, the dyebath solution was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric.

When the chlorine fastness of the polyphenol-treated cotton fabric obtained above was measured, it was second grade.

(Sample 5A)
1 kg of the polyphenol-treated cotton fabric obtained in Sample 5 was immersed in about 15 L of water in a dye bath and sufficiently impregnated with water. To this, 20 g of a dispersible phenylamide treating agent (trade name: ITN003M, Takeuchi Shoten Co., Ltd., anionic phenylamide fiber processing agent, resin-containing acidic aqueous solution) was added and stirred for 10 minutes. Water was added to adjust the amount of the dye bath to 20 L (pH 6.7). This was heated and heated up to 50 ° C., and the cotton fabric was sufficiently immersed while stirring for 30 minutes while maintaining the temperature. Thereafter, the dyebath solution was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric after phenylamide treatment.

The chlorine fastness of the obtained polyphenol-treated cotton fabric was measured and it was 2-3.

(Sample 6A)
A cotton fabric subjected to refining bleaching was previously dyed with a chemical dye to prepare a dyed cotton fabric. 1 kg of this dyed cotton fabric was immersed in about 15 L of water in a dye bath and sufficiently impregnated with water. To this, 5 g of tea-extracted polyphenol (trade name: Theafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water and poured into a dye bath, which was heated to 80 ° C. An aqueous solution obtained by dissolving 10 g of sodium stannate and 20 g of citric acid in about 1 L of water is put into a dye bath, and then a dispersible phenylamide treatment agent (trade name: ITN003M, sold by Takeuchi Shoten Co., Ltd., anionic phenylamide type) 30 g of fiber processing agent and resin-containing acidic aqueous liquid were added (pH 4.5), and the mixture was stirred at 80 ° C. for 10 minutes. Water was added to adjust the dye bath volume to 20 L, and the cotton fabric was sufficiently immersed while stirring at 80 ° C. for 30 minutes. Thereafter, the dye bath was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a phenylamide-treated polyphenol-treated cotton fabric.

The light fastness and chlorine fastness of the obtained polyphenol-treated cotton fabric were measured. The light fastness was grade 3 and the chlorine fastness was grade 4-5.

(Sample 7)
1 kg of the polyphenol-treated cotton fabric obtained in Sample 1 was immersed in about 20 L of water in a dye bath and sufficiently impregnated with water. To this was added 30 g of a commercially available chlorine fastness-fixing agent (trade name: Morillon WS, manufactured by Morin Chemical Industry Co., Ltd., an anionic brown liquid), and this was heated to 40 ° C. to maintain the temperature. The cotton fabric was sufficiently immersed while stirring for 10 minutes. Thereafter, the dye bath was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric after the fixer treatment.

The light fastness and chlorine fastness of the obtained polyphenol-treated cotton fabric were measured. The light fastness was grade 1 and the chlorine fastness was grade 3.

(Sample 8)
1 kg of the polyphenol-treated cotton fabric obtained in Sample 1 was immersed in about 20 L of water in a dye bath and sufficiently impregnated with water. To this was added 30 g of a commercially available chlorine fastness improving fix agent (trade name: Dunfix 5000, manufactured by Nittobo Co., Ltd., a cationic light yellow acidic liquid) (pH 4.0), and this was heated to 40 ° C. The temperature was raised and the cotton fabric was sufficiently immersed while stirring for 10 minutes while maintaining the temperature. Thereafter, the dye bath was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric after the fixer treatment.

The light fastness and chlorine fastness of the obtained polyphenol-treated cotton fabric were measured. The light fastness was grade 3 and the chlorine fastness was grade 3. However, the decolorization of polyphenol considered to be caused by the acid of the fixing agent occurred.

(Sample 9)
1 kg of the polyphenol-treated cotton fabric obtained in Sample 1 was immersed in about 20 L of water in a dye bath and sufficiently impregnated with water. To this was added 30 g of a commercially available chlorine fastness-fixing agent (trade name: Dunfix 7000, manufactured by Nittobo Co., Ltd., a cationic light yellow alkaline liquid) (pH 8.0), and this was heated to 40 ° C. The temperature was raised and the cotton fabric was sufficiently immersed while stirring for 10 minutes while maintaining the temperature. Thereafter, the dye bath was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric after the fixer treatment.

The light fastness and chlorine fastness of the obtained polyphenol-treated cotton fabric were measured. The light fastness was grade 3 and the chlorine fastness was grade 3. However, the color haze of polyphenol considered to be caused by the alkali of the fixing agent occurred.

(Sample 10)
1 kg of cotton fabric subjected to refining and bleaching was immersed in about 15 L of water in a dyeing bath and sufficiently impregnated with water. To this, 5 g of tea-extracted polyphenol (trade name: Teafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water, and this was heated and heated to 80 ° C. An aqueous solution obtained by dissolving 10 g of sodium stannate and 20 g of citric acid in about 1 L of water is added to the dyeing bath, water is added to adjust the amount of the dyeing bath to 20 L, and cotton is stirred at 80 ° C. for 10 minutes. The dough was fully immersed. To this was added 30 g of a water-soluble phenylamide treatment agent (trade name: Amorden MCM-400, manufactured by Daiwa Chemical Co., Ltd., anionic phenylamide fiber processing agent, acidic aqueous solution) (pH 6.5), 80 ° C. For 30 minutes. Thereafter, the dyebath solution was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric.

Measured chlorine fastness of the obtained polyphenol-treated cotton fabric did not satisfy the third grade standard, and no improvement in chlorine fastness was observed.

(Sample 11)
1 kg of cotton fabric subjected to refining and bleaching was immersed in about 15 L of water in a dyeing bath and sufficiently impregnated with water. To this, 5 g of tea-extracted polyphenol (trade name: Teafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water, and this was heated and heated to 80 ° C. An aqueous solution obtained by dissolving 10 g of sodium stannate and 20 g of citric acid in about 1 L of water is added to the dyeing bath, water is added to adjust the amount of the dyeing bath to 20 L, and cotton is stirred at 80 ° C. for 10 minutes. The dough was fully immersed. To this, 30 g of a dispersible acrylic resin treatment agent (trade name: Phicoat N-125, manufactured by Daiwa Chemical Co., Ltd., an anionic acrylic resin fiber processing agent, weakly acidic liquid) was added (pH 5.0), Stir at 80 ° C. for 30 minutes. Thereafter, the dyebath solution was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a polyphenol-treated cotton fabric.

Measured chlorine fastness of the obtained polyphenol-treated cotton fabric did not satisfy the third grade standard, and no improvement in chlorine fastness was observed.

(Physical properties and functionality of polyphenol processed fiber)
Various fastnesses, antibacterial properties, deodorizing properties, ultraviolet shielding ability, antioxidant properties, and safety were examined for the fastened polyphenol-treated cotton fabric obtained in Sample 2A. The results are shown in Table 1 below.

As is clear from Table 1, by applying a fastening treatment using dispersible phenylamide to the polyphenol-processed fiber, the fastness to washing, the fastness to sweat, and the fastness to friction are not reduced. Certain antibacterial properties, deodorant properties, and antioxidant properties are also maintained, and the ultraviolet shielding ability is improved. It also maintains safety for the body and the environment.

(Sample 2Aa)
1 kg of cotton fabric subjected to refining and bleaching was immersed in about 15 L of water in a dyeing bath and sufficiently impregnated with water. To this, 5 g of tea-extracted polyphenol (trade name: Teafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water, and this was heated and heated to 80 ° C. An aqueous solution obtained by dissolving 10 g of sodium stannate and 20 g of citric acid in about 1 L of water is added to the dyeing bath, water is added to adjust the amount of the dyeing bath to 20 L, and cotton is stirred at 80 ° C. for 10 minutes. The dough was fully immersed. To this was added 30 g of a dispersible phenylamide treatment agent (trade name: ITN003M, Takeuchi Shoten Co., Ltd., anionic phenylamide fiber processing agent, resin-containing acidic aqueous solution) (pH 4.5), 80 ° C. For 30 minutes. Thereafter, the dyebath solution is discharged, the cotton fabric is carefully washed with running water, 20 L of citric acid aqueous solution with a concentration of 0.5 g / L is added and immersed, and acidic post-treatment is performed at a temperature of 50 ° C. for 10 minutes. The cotton fabric was washed thoroughly with running water. The cotton fabric was taken out, dehydrated and dried to obtain a phenylamide-treated polyphenol-treated cotton fabric.
When the light fastness and chlorine fastness of the obtained polyphenol-treated cotton fabric were measured, the light fastness was grade 3 and the chlorine fastness was grade 3-4.

(Sample 2Ab)
1 kg of cotton fabric subjected to refining and bleaching was immersed in about 15 L of water in a dyeing bath and sufficiently impregnated with water. To this, 5 g of tea-extracted polyphenol (trade name: Theafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water and added thereto. A silicone-based antifoaming agent (trade name: SENKA ANTI HOME 4B, SENKA CORPORATION Manufactured, nonionic emulsion antifoaming agent) 1.5 g was added, and this was heated to 80 ° C. An aqueous solution obtained by dissolving 10 g of sodium stannate and 20 g of citric acid in about 1 L of water is added to the dyeing bath, water is added to adjust the amount of the dyeing bath to 20 L, and cotton is stirred at 80 ° C. for 10 minutes. The dough was fully immersed. To this was added 30 g of a dispersible phenylamide treatment agent (trade name: ITN003M, Takeuchi Shoten Co., Ltd., anionic phenylamide fiber processing agent, resin-containing acidic aqueous solution) (pH 4.5), 80 ° C. For 30 minutes. Thereafter, the dye bath was discharged, the cotton fabric was carefully washed with running water, the cotton fabric was taken out, dehydrated and dried to obtain a phenylamide-treated polyphenol-treated cotton fabric.
When the light fastness and chlorine fastness of the obtained polyphenol-treated cotton fabric were measured, the light fastness was grade 3 and the chlorine fastness was grade 3-4.

(Sample 2Ac)
1 kg of cotton fabric subjected to refining and bleaching was immersed in about 15 L of water in a dyeing bath and sufficiently impregnated with water. To this, 5 g of tea-extracted polyphenol (trade name: Theafuran 30F, manufactured by ITO EN Co., Ltd.) was dissolved in about 1 L of water and added thereto. A silicone-based antifoaming agent (trade name: SENKA ANTI HOME 4B, SENKA CORPORATION (Made) 1.5g was added and this was heated and heated up to 80 degreeC. An aqueous solution obtained by dissolving 10 g of sodium stannate and 20 g of citric acid in about 1 L of water is added to the dyeing bath, water is added to adjust the amount of the dyeing bath to 20 L, and cotton is stirred at 80 ° C. for 10 minutes. The dough was fully immersed. To this was added 30 g of a dispersible phenylamide treatment agent (trade name: ITN003M, Takeuchi Shoten Co., Ltd., anionic phenylamide fiber processing agent, resin-containing acidic aqueous solution) (pH 4.5), 80 ° C. For 30 minutes. Thereafter, the dyebath solution is discharged, the cotton fabric is carefully washed with running water, 20 L of citric acid aqueous solution with a concentration of 0.5 g / L is added and immersed, and acidic post-treatment is performed at a temperature of 50 ° C. for 10 minutes. The cotton fabric was washed thoroughly with running water. The cotton fabric was taken out, dehydrated and dried to obtain a phenylamide-treated polyphenol-treated cotton fabric.
When the light fastness and chlorine fastness of the obtained polyphenol-treated cotton fabric were measured, the light fastness was grade 3 and the chlorine fastness was grade 3-4.

(Discoloration due to repeated washing)
For the polyphenol-treated cotton fabrics of Samples 2A, 2Aa, 2Ab and 2Ac, washing was repeated 10 times according to JIS L0217 103 using JAFET standard detergent. The sample 2A was grade 3, the samples 2Aa and 2Ab were grade 4, and the sample 2Ac was grade 4-5.
Accordingly, both the defoaming treatment and the acidic post-treatment are effective for suppressing discoloration caused by repeated washing, and the durability of polyphenol processing for repeated washing is further improved by combining them.

The chlorine fastness can be improved while maintaining the light fastness of the polyphenol-processed fiber without impairing the dyeability and function of the polyphenol, so that it can be used for general clothing and clothing, kitchen utensils using fabrics, ornaments, and amenities. It can be widely applied to various fiber-utilizing products such as products to provide high-quality products, and the use development of products utilizing the functionality of polyphenols can be promoted. Therefore, it is useful for the spread of polyphenol processed fiber products.

Claims (8)

1. The fiber contacted with the polyphenol has a fastening treatment for treating the fiber with an anionic aqueous dispersion of a phenylamide compound, and at least one of an antifoaming treatment and an acidic post-treatment, An antifoaming agent is allowed to act during the fastening treatment, and in the acidic post-treatment, the fiber after the fastening treatment is treated with an acidic aqueous liquid.
2. The said polyphenol contains tea origin polyphenol and / or grape origin polyphenol, The said aqueous dispersion has a polymer component to disperse | distribute, The said polymer component contains an anion, The manufacture of the polyphenol processed fiber of Claim 1 Method.
3. The polyphenol is supplied to and brought into contact with the fiber as an aqueous liquid containing 0.1 to 7% by mass of the polyphenol with respect to the fiber, and the anionic aqueous dispersion for treating the fiber is in contact with the fiber. The method for producing a polyphenol-processed fiber according to claim 1 or 2, wherein the polyphenol-processed fiber is supplied at a ratio of 0.5 to 7% by mass.
4. 4. The fastening treatment is performed under the conditions of pH 4.5 to 6.9 and temperature 35 to 95 ° C. after removing polyphenol not adhering to the fiber from the fiber in contact with the polyphenol. Of producing polyphenol processed fiber.
5. The polyphenol processing according to any one of claims 1 to 3, wherein the fastening treatment is performed under the conditions of pH 3 to 11 and temperature 35 to 95 ° C without removing polyphenol that does not adhere to the fiber from the fibers that have contacted the polyphenol. A method for producing fibers.
6. The antifoaming agent is a silicone-based antifoaming agent, and the acidic post-treatment is performed at a pH of 2.5 to 5.5 using an aqueous citric acid solution having a concentration of 0.05 to 3 g / L as the acidic aqueous solution. The method for producing a polyphenol processed fiber according to any one of claims 1 to 5, which is adjusted.
7. The method for producing a polyphenol processed fiber according to claim 5, wherein the antifoaming agent is a nonionic emulsion antifoaming agent.
8. A polyphenol processed fiber having a phenylamide compound obtained by the production method according to any one of claims 1 to 7.