Fiber-treating agent

Abstract

To provide a fiber-treating agent that improves water resistance and heat resistance, which are points at issue in naturally derived fibers, imparts thermal shape memory, improves elasticity (tenacity) and surface feel, and does not color naturally derived fibers.SOLUTION: This fiber-treating agent contains the following components (A) and (B). (A): A compound having at least one carboxyl group or a salt thereof and no condensed ring, in which the hydrogen bond term δH of the Hansen solubility parameter is 18.3 MPa1 / 2 or less. (B): Water.SELECTED DRAWING: None

Description

[Technical Field]

[0001] The present invention relates to a fiber treatment agent for imparting water resistance, heat resistance, and thermal shape memory ability to naturally derived fibers, and more preferably to a fiber treatment agent for naturally derived fibers used in textile products such as wigs, hair extensions, and other headwear. [Background technology]

[0002] Natural fibers generally differ from synthetic fibers in that they possess a natural texture and appearance derived from natural materials. Among natural fibers, regenerated protein fibers, such as regenerated collagen fibers, are obtained by solubilizing acid-soluble or insoluble collagen with alkali or enzymes to create a spinning solution, which is then extruded through a spinning nozzle into a coagulation bath to form fibers.

[0003] However, naturally derived fibers generally have higher hydrophilicity than synthetic fibers, resulting in higher water absorption and generally lower mechanical strength when saturated with water. Regenerated protein fibers, in particular, have extremely low mechanical strength. Consequently, their high water absorption during washing significantly reduces their mechanical strength, leading to breakage during subsequent drying and ultimately reducing their suitability as textile products.

[0004] Furthermore, among naturally derived fibers, regenerated protein fibers have the problem of low heat resistance. For example, when using heat styling tools such as hair irons, if they are styled at the same high temperatures as human hair, they can shrink or become frizzy, spoiling their appearance.

[0005] Furthermore, while plastic synthetic fibers retain their shape after heat setting with an iron, etc., even after subsequent washing (they have thermal shape memory), natural fibers lose their shape after a single wash (they lack thermal shape memory). Therefore, they are inferior to conventional plastic synthetic fibers in terms of the degree of freedom in shape setting.

[0006] The points mentioned above have hindered the widespread use of natural fibers, particularly regenerated protein fibers, in textile products such as headwear. The impact of reduced water resistance, specifically the decrease in mechanical strength when wet, was particularly significant. On the other hand, in the field of human hair fibers, which are naturally derived fibers, a method is known in which specific aldehyde derivatives and phenolic compounds are reacted with human hair fibers, which do not inherently possess thermal shape memory ability, to newly impart thermal shape memory ability (Patent Document 1). [Prior art documents] [Patent Documents]

[0007] [Patent Document 1] Japanese Patent Publication No. 2019-143281 [Overview of the Initiative] [Problems that the invention aims to solve]

[0008] However, in the manufacturing of textile products such as headwear, fibers are sometimes stretched strongly, and the technology described in Patent Document 1 sometimes did not result in sufficient elasticity (toughness) of the treated fibers. Therefore, there was a need to improve the elasticity of the treated fibers to prevent breakage during stretching. In addition, the technology described in Patent Document 1 sometimes resulted in discoloration of the fibers.

[0009] Therefore, the present invention relates to a fiber treatment agent that improves the water resistance and heat resistance, which are problems with naturally derived fibers, imparts thermal shape memory ability, improves elasticity (toughness) and surface feel, and does not color the naturally derived fibers. [Means for solving the problem]

[0010] As a result of diligent research, the inventors have discovered that by treating natural fibers with a composition containing a compound having a carboxyl group and a hydrogen bonding term of Hansen's solubility parameter below a certain value, the carboxyl group of the compound that penetrates into the fiber strongly coordinates with the metal (mainly polyvalent metal) in the natural fiber, thereby hydrophobicizing the inside of the fiber while preventing the leakage of the compound from the fiber. As a result, the water resistance and heat resistance in both dry and wet conditions of the natural fibers are improved, and not only can they be shaped by heat setting, but surprisingly, the elasticity (toughness) of the natural fibers is improved compared to before treatment, reaching a level close to that of human hair, and furthermore, no discoloration occurs, thus completing the present invention.

[0011] The present invention provides a fiber treatment agent containing the following components (A) and (B). (A): The hydrogen bonding term δH of Hansen's solubility parameter is 18.3 MPa 1 / 2 The following compounds have at least one carboxyl group or a salt thereof and do not have a fused ring. (B):Water [Effects of the Invention]

[0012] According to the present invention, it is possible to provide a fiber treatment agent that can improve the water resistance and heat resistance, which are problems of naturally derived fibers, impart thermal shape memory ability, improve elasticity (toughness) and surface feel, and without coloring the naturally derived fibers. [Modes for carrying out the invention]

[0013] [Fibers to be processed in this invention] The fibers to be treated with the fiber treatment agent of the present invention are preferably metal-containing fibers, preferably metal-containing naturally derived fibers or metal-containing synthetic fibers, and among these, metal-containing naturally derived fibers are preferred. Naturally derived fibers refer to fibers collected from natural plants and animals, or fibers artificially manufactured using polymers or oligomers such as proteins and polysaccharides derived from keratin, collagen, casein, soybeans, peanuts, corn, silk waste, silk protein (e.g., silk fibroin), etc. Of these, fibers artificially manufactured using polymers or oligomers such as proteins and polysaccharides derived from keratin, collagen, casein, soybeans, peanuts, corn, silk waste, silk protein (e.g., silk fibroin), etc. are preferred, regenerated protein fibers made from proteins derived from keratin, collagen, casein, soybean protein, peanut protein, corn protein, silk protein (e.g., silk fibroin), etc. are more preferred, regenerated protein fibers such as regenerated collagen fibers made from collagen, regenerated silk fibers made from silk fibroin, etc. are even more preferred, and regenerated collagen fibers are even more preferred.

[0014] Regenerated collagen fibers can be manufactured using known technologies, and their composition does not need to be 100% collagen; they may contain natural or synthetic polymers or additives for quality improvement. Furthermore, they may be post-processed regenerated collagen fibers. The preferred form of regenerated collagen fibers is filament. Filaments are generally removed from bobbins or boxes. Alternatively, filaments that come out of the drying process during the manufacturing of regenerated collagen fibers can be used directly.

[0015] Synthetic fibers containing metal may include metal-treated synthetic fibers. Naturally derived fibers containing metal may include those that originally contain metal, such as fibers extracted from natural plants and animals, in which case it is not necessary to add metal again. However, they may also be treated with metal salts, such as the aluminum salt-treated fibers for water resistance described in Japanese Patent Publication No. 2003-027318.

[0016] [Component (A): The hydrogen bonding term δH of Hansen's solubility parameter is 18.3 MPa] 1 / 2 The following compounds have at least one carboxyl group or a salt thereof and do not have a fused ring. Component (A) has a hydrogen bonding term δH of 18.3 MPa in Hansen's solubility parameter. 1 / 2 The following is a compound having at least one carboxyl group or a salt thereof and not having a fused ring. In this invention, the hydrogen bonding term of the Hansen solubility parameter is δH(MPa) calculated at 25°C in the DIY program using the software package HSPiP 4th Edition 4.1.07, based on Hansen Solubility Parameters: A User's Handbook, CRC Press, Boca Raton FL, 2007. 1 / 2 This refers to the energy term due to intermolecular hydrogen bonding. Examples of cases where component (A) is a salt include alkali metal salts such as sodium salts and potassium salts.

[0017] Examples of compounds of component (A) include (A1) and (A2) below. (A1) The hydrogen bonding term δH of Hansen's solubility parameter is 18.3 MPa 1 / 2 The following are aromatic compounds having at least one carboxyl group or a salt thereof and not having a fused ring: (A2) The hydrogen bonding term δH of Hansen's solubility parameter is 11.0 MPa 1 / 2 The above is 18.3 MPa. 1 / 2 The following are compounds (excluding aromatic compounds) that have at least one carboxyl group or a salt thereof and do not have a fused ring:

[0018] Examples of aromatic compounds of component (A1) include compounds represented by the following general formula (1) or general formula (2), or salts thereof.

[0019] [ka]

[0020] [In the formula, =X represents a methylidene group or an oxo group, and R 1 represents a hydrogen atom, a hydroxyl group, or an alkyl group, aryl group, alkoxy group, aryloxy group or aralkyloxy group which may have a substituent, and R 2 represents an o-phenylene group, m-phenylene group, p-phenylene group, benzylidene group, or an alkylene group which may have a substituent. However, when R 2 does not have an aryl group, R 1 is an aryl group, aryloxy group or aralkyloxy group.]

[0021] [Chemical formula]

[0022] [In the formula, A 1 ~A 5 each independently represents a hydrogen atom, an acetyl group, a halogen atom, or a linear or branched alkyl group, alkenyl group, alkoxy group or alkenyloxy group having 1 to 6 carbon atoms.]

[0023] Among the component (A1), examples of the aromatic compound represented by the general formula (1) include compounds represented by the following general formula (1A), (1B) or (1C).

[0024] [Chemical formula]

[0025] [In the formula, B 1 ~B 4 each independently represents a hydrogen atom, an acetyl group, a halogen atom, or a linear or branched alkyl group, alkenyl group, alkoxy group or alkenyloxy group having 1 to 6 carbon atoms, and R 3 represents a hydroxyl group, or a group represented by the following general formula (1A)-a or (1A)-b.]

[0026] [Chemical formula]

[0027] [In the formula, B 5 ~B 9 is the aforementioned B 1 ~B 4 It has the same meaning as R 4 [where n represents a hydrogen atom or a methyl group, and n represents an integer between 0 and 2.]

[0028] [ka]

[0029] [In the formula, D 1 ~D 4 Each of these independently represents a hydrogen atom, an acetyl group, a halogen atom, or a linear or branched alkyl group, alkenyl group, alkoxy group, or alkenyloxy group having 1 to 6 carbon atoms, and E 1 ~E 5 Each is independent of D 1 ~D 4 This indicates a group similar to or represented by general formula (1B)-a.

[0030] [ka]

[0031] [In the formula, m represents an integer between 0 and 4.]

[0032] [ka]

[0033] [In the formula, R 6 represents a hydrogen atom or a group represented by the general formula (1C)-a, G 1 and G 2Each of these independently represents a hydrogen atom, an acetyl group, a halogen atom, an optionally substituted aryl group, a C7-C12 aralkyl group or arylalkenyl group, or a C1-C6 linear or branched alkyl group, alkenyl group, alkoxy group, alkenyloxy group or alloyloxy group. However, R 6 If G is a hydrogen atom, 1 and G 2 At least one of these is an aryl group which may have substituents, an aralkyl group having 7 to 12 carbon atoms, an arylalkenyl group, or an alloyloxy group.

[0034] [ka]

[0035] [During the ceremony, J 1 ~J 5 Each of these independently represents a hydrogen atom, an acetyl group, a halogen atom, or a linear or branched alkyl group, alkenyl group, alkoxy group, or alkenyloxy group having 1 to 6 carbon atoms.

[0036] Among the compounds represented by general formula (1A), R 3 Compounds with a hydroxyl group include 2-carboxybenzoic acid (phthalic acid) (Hansen's solubility parameter, hydrogen bonding term δH: 13.4 MPa). 1 / 2 (The numbers in parentheses after each compound name below indicate the hydrogen bond term δH calculated using the method described above.) Among the compounds represented by general formula (1A), R 3 Compounds in which the group is represented by the general formula (1A)-a include 2-(((4-vinylbenzyl)oxy)carbonyl)benzoic acid (7.0MPa 1 / 2 ) are some examples. Among the compounds represented by general formula (1A), R 3 Compounds in which the group is represented by the general formula (1A)-b include 2-((2-(acryloyloxy)ethoxy)carbonyl)benzoic acid (9.1MPa). 1 / 2), 2-((2-(methacryloyloxy)ethoxy)carbonyl)benzoic acid (8.4MPa) 1 / 2 ) are some examples.

[0037] Compounds represented by general formula (1B) include 2-benzoylbenzoic acid (7.5 MPa). 1 / 2 ), 2-(2-methylbenzoyl)benzoic acid (6.9MPa 1 / 2 ), 2-(3-methylbenzoyl)benzoic acid (6.6MPa 1 / 2 ), 2-(4-methylbenzoyl)benzoic acid (7.2MPa 1 / 2 ), 2-(2-chlorobenzoyl)benzoic acid (7.1MPa 1 / 2 ), 2-(3-chlorobenzoyl)benzoic acid (6.9MPa 1 / 2 ), 2-(4-chlorobenzoyl)benzoic acid (7.5MPa 1 / 2 ), 2-(4-(2-(2-(acryloyloxy)ethoxy)ethoxy)benzoyl)benzoic acid (8.7MPa) 1 / 2 ) are some examples.

[0038] Among the compounds represented by the general formula (1C), R 6 As for compounds where the atom is a hydrogen atom, phenyl succinic acid (15.8 MPa) 1 / 2 ), 2,3-diphenylsuccinic acid (11.9MPa) 1 / 2 ), (+)-di-p-toluyl-D-tartaric acid (10.2MPa) 1 / 2 ) are some examples. Among the compounds represented by the general formula (1C), R 6 Compounds in which the group is represented by the general formula (1C)-a include 4-oxo-4-((4-vinylbenzyl)oxy)butanoic acid (10.1MPa). 1 / 2 ) are some examples.

[0039] In addition, compounds that are not included in general formulas (1A), (1B), and (1C), but are included in general formula (1), include 3-carboxybenzoic acid (isophthalic acid) (12.9 MPa). 1 / 2 ), 4-carboxybenzoic acid (terephthalic acid) (13.7MPa) 1 / 2 ), 3-benzoylbenzoic acid (7.2MPa1 / 2 ), 4-benzoylbenzoic acid (7.9MPa 1 / 2 ) are examples. The numbers in parentheses after each compound name are the hydrogen bond term δH calculated using the method described above.

[0040] Among the components (A1), a specific example of an aromatic compound represented by general formula (2) is benzoic acid (9.5 MPa). 1 / 2 ), 2-methylbenzoic acid (8.4MPa 1 / 2 ), 3-methylbenzoic acid (8.0MPa) 1 / 2 ), 4-methylbenzoic acid (8.8MPa) 1 / 2 ), 2-ethylbenzoic acid (7.7MPa 1 / 2 ), 3-ethylbenzoic acid (7.4MPa 1 / 2 ), 4-ethylbenzoic acid (8.1MPa 1 / 2 ), 2-propylbenzoic acid (7.0MPa 1 / 2 ), 3-propylbenzoic acid (6.7MPa 1 / 2 ), 4-propylbenzoic acid (7.4MPa 1 / 2 ), 2-isopropylbenzoic acid (6.7MPa 1 / 2 ), 3-isopropylbenzoic acid (6.5MPa 1 / 2 ), 4-isopropylbenzoic acid (7.1MPa 1 / 2 ), 2-n-butylbenzoic acid (6.8MPa 1 / 2 ), 3-n-butylbenzoic acid (6.5MPa 1 / 2 ), 4-n-butylbenzoic acid (7.2MPa 1 / 2 ), 2-tert-butylbenzoic acid (6.1MPa 1 / 2 ), 3-tert-butylbenzoic acid (5.9MPa 1 / 2 ), 4-tert-butylbenzoic acid (6.5MPa 1 / 2 ), 2-vinylbenzoic acid (8.0MPa) 1 / 2 ), 3-vinylbenzoic acid (7.7MPa 1 / 2 ), 4-vinylbenzoic acid (8.5MPa) 1 / 2 ), 2-acetylbenzoic acid (8.6MPa 1 / 2 ), 3-acetylbenzoic acid (8.2MPa) 1 / 2 ), 4-acetylbenzoic acid (8.9MPa 1 / 2 ), 2-methoxybenzoic acid (9.7MPa 1 / 2) 3-Methoxybenzoic acid (9.3 MPa 1 / 2 ) 4-Methoxybenzoic acid (10.1 MPa 1 / 2 ) 2-Chlorobenzoic acid (8.7 MPa 1 / 2 ) 3-Chlorobenzoic acid (8.4 MPa 1 / 2 ) 4-Chlorobenzoic acid (9.2 MPa 1 / 2 ) 2-Bromobenzoic acid (9.1 MPa 1 / 2 ) 3-Bromobenzoic acid (8.8 MPa 1 / 2 ) 4-Bromobenzoic acid (10.1 MPa 1 / 2 ) etc. Among them, 4-Ethylbenzoic acid, 4-Vinylbenzoic acid, and Benzoic acid are preferred.

[0041] Further, as compounds other than the general formulas (1) and (2) of the component (A1), Phenylbutanoic acid can be mentioned.

[0042] As the compound of the component (A2), Potassium 2,4-hexadienoate (kPa) (12.5 MPa 1 / 2 ) can be mentioned.

[0043] The hydrogen bonding term δH of the aromatic compound of the component (A1) is preferably 16.0 MPa or less, more preferably 13.5 MPa or less, still more preferably 12.0 MPa or less, still more preferably 10.0 MPa or less, from the viewpoint of moderately hydrophobizing the inside of the fiber, and is preferably 3.0 MPa or more, more preferably 4.0 MPa or more, still more preferably 5.0 MPa or more. 1 / 2 Further, it is more preferably 13.5 MPa or less 1 / 2 Further, it is still more preferably 12.0 MPa or less 1 / 2 Further, it is still more preferably 10.0 MPa or less 1 / 2 Further, it is still more preferably 10.0 MPa or less, and is preferably 3.0 MPa or more 1 / 2 More preferably 4.0 MPa or more 1 / 2 Still more preferably 5.0 MPa or more 1 / 2 It is as follows.

[0044] The hydrogen bonding term δH of the compound of the component (A2) is preferably 16.0 MPa or less, more preferably 15.0 MPa or less, still more preferably 14.0 MPa or less, still more preferably 13.0 MPa or less, from the viewpoint of moderately hydrophobizing the inside of the fiber, and is preferably 11.0 MPa or more. 1 / 2 Further, it is more preferably 15.0 MPa or less 1 / 2 Still more preferably 14.0 MPa or less 1 / 2 Still more preferably 13.0 MPa or less 1 / 2 Further, it is still more preferably 13.0 MPa or less, and is preferably 11.0 MPa or more 1 / 2The above comfort level is 11.5 MPa. 1 / 2 More preferably, 12.0 MPa 1 / 2 That's all.

[0045] The following describes the preferred content of component (A) for each type of component (A). Here, in this invention, the content of component (A) refers to the content of the corresponding acid form when component (A) is a salt. The content of component (A) varies depending on the pH range of the fiber treatment agent, but the range shown below is preferred.

[0046] With regard to component (A), in particular component (A1), which is benzoic acid or its salt (hereinafter sometimes referred to as "component (A1-1)"), when the pH of the fiber treatment agent is 2.0 or higher and less than 6.5, from the viewpoint of imparting high shape retention, water resistance, elasticity (toughness, i.e., high elongation at break when the fiber is tensile), and heat resistance to the natural fiber after treatment, the content of component (A1-1) in the fiber treatment agent is preferably 0.8% by mass or more, more preferably 3.0% by mass or more, even more preferably 5.0% by mass or more, even more preferably 10% by mass or more, even more preferably 15% by mass or more, and even more preferably 20% by mass or more as benzoic acid (acid form). Furthermore, from the viewpoint of improving the feel of the fiber surface, it is preferably 90% by mass or less, more preferably 80% by mass or less, even more preferably 70% by mass or less, even more preferably 50% by mass or less, even more preferably 40% by mass or less, and even more preferably 35% by mass or less.

[0047] In other words, when component (A) is (A1-1) benzoic acid or a salt thereof, and the pH of the fiber treatment agent is 2.0 or higher and less than 6.5, the content of component (A1-1) in the fiber treatment agent of the present invention is, from the above viewpoint, preferably 0.8 to 90% by mass, more preferably 3.0 to 80% by mass, even more preferably 5.0 to 70% by mass, even more preferably 10 to 50% by mass, even more preferably 15 to 40% by mass, and even more preferably 20 to 35% by mass, as benzoic acid (acid form).

[0048] Furthermore, if component (A) is (A1-1) benzoic acid or a salt thereof, and the pH of the fiber treatment agent is 6.5 or higher and 11.0 or lower, from the viewpoint of imparting high shape retention, water resistance, elasticity (toughness, i.e., high elongation at break when the fiber is tensile) and heat resistance to the natural fiber after treatment, the content of component (A1-1) in the fiber treatment agent is preferably 0.8% by mass or more, more preferably 3.0% by mass or more, even more preferably 5.0% by mass or more, even more preferably 10% by mass or more, even more preferably 15% by mass or more, even more preferably 20% by mass or more, even more preferably 25% by mass or more, even more preferably 26% by mass or more, even more preferably 28% by mass or more, and even more preferably 30% by mass or more, and from the viewpoint of improving the feel of the fiber surface, it is preferably 90% by mass or less, more preferably 80% by mass or less, even more preferably 70% by mass or less, even more preferably 50% by mass or less, even more preferably 45% by mass or less, and even more preferably 40% by mass or less.

[0049] That is, when component (A) is (A1-1) benzoic acid or a salt thereof, and the pH of the fiber treatment agent is 6.5 or higher and 11.0 or lower, the content of component (A1-1) in the fiber treatment agent of the present invention is, from the above viewpoint, preferably 0.8 to 90% by mass, more preferably 3.0 to 80% by mass, even more preferably 5.0 to 70% by mass, even more preferably 10 to 70% by mass, even more preferably 15 to 50% by mass, even more preferably 20 to 50% by mass, even more preferably 25 to 45% by mass, even more preferably 26 to 45% by mass, even more preferably 28 to 40% by mass, and even more preferably 30 to 40% by mass, as benzoic acid (acid form).

[0050] Of component (A), component (A1) other than benzoic acid or its salt (hereinafter sometimes referred to as "component (A1-2)") is used when the pH of the fiber treatment agent is 2.0 or higher and less than 6.5. From the viewpoint of imparting high shape retention, water resistance, elasticity (toughness, i.e., high elongation at break when the fiber is tensile), and heat resistance to the natural fiber after treatment, the content of component (A1-2) in the fiber treatment agent is preferably 0.1% by mass or more, more preferably 0.2% by mass or more, even more preferably 0.5% by mass or more, and even more preferably 1.0% by mass or more. Furthermore, from the viewpoint of improving the feel of the fiber surface, the content is preferably 70% by mass or less, more preferably 60% by mass or less, even more preferably 50% by mass or less, and even more preferably 45% by mass or less.

[0051] In other words, when component (A) is component (A1) other than (A1-2) benzoic acid or its salt, and the pH of the fiber treatment agent is 2.0 or higher and less than 6.5, the content of component (A1-2) in the fiber treatment agent of the present invention is, from the above viewpoint, preferably 0.1 to 70% by mass, more preferably 0.2 to 60% by mass, even more preferably 0.5 to 50% by mass, and even more preferably 1.0 to 45% by mass.

[0052] Furthermore, if component (A) is component (A1) other than (A1-2)benzoic acid or its salt, and the pH of the fiber treatment agent is 6.5 or higher and 11.0 or lower, from the viewpoint of imparting high shape retention, water resistance, elasticity (toughness, i.e., high elongation at break when the fiber is tensile), and heat resistance to the natural fiber after treatment, the content of component (A1-2) in the fiber treatment agent is preferably 1.0% by mass or more, more preferably 2.0% by mass or more, even more preferably 5.0% by mass or more, and even more preferably 10% by mass or more. Also, from the viewpoint of improving the feel of the fiber surface, it is preferably 70% by mass or less, more preferably 60% by mass or less, even more preferably 50% by mass or less, and even more preferably 40% by mass or less.

[0053] In other words, when component (A) is component (A1) other than (A1-2) benzoic acid or its salt, and the pH of the fiber treatment agent is 6.5 or higher and 11.0 or lower, the content of component (A1-2) in the fiber treatment agent of the present invention is, from the above viewpoint, preferably 1.0 to 70% by mass, more preferably 2.0 to 60% by mass, even more preferably 5.0 to 50% by mass, and even more preferably 10 to 40% by mass.

[0054] When component (A) is component (A2) and the pH of the fiber treatment agent is 2.0 or higher and less than 6.5, from the viewpoint of imparting high shape retention, water resistance, elasticity (toughness, i.e., high elongation at break when the fiber is tensile) and heat resistance to the natural fiber after treatment, the content of component (A2) in the fiber treatment agent is preferably 0.1% by mass or more, more preferably 0.2% by mass or more, even more preferably 0.5% by mass or more, and even more preferably 1.0% by mass or more. Furthermore, from the viewpoint of improving the feel of the fiber surface, it is preferably 60% by mass or less, more preferably 50% by mass or less, even more preferably 40% by mass or less, and even more preferably 30% by mass or less.

[0055] In other words, when component (A) is component (A2) and the pH of the fiber treatment agent is 2.0 or higher and less than 6.5, the content of component (A2) in the fiber treatment agent of the present invention is, from the above viewpoint, preferably 0.1 to 60% by mass, more preferably 0.2 to 50% by mass, even more preferably 0.5 to 40% by mass, and even more preferably 1.0 to 30% by mass.

[0056] When component (A) is component (A2) and the pH of the fiber treatment agent is 6.5 or higher and 11.0 or lower, from the viewpoint of imparting high shape retention, water resistance, elasticity (toughness, i.e., high elongation at break when the fiber is tensile) and heat resistance to the natural fiber after treatment, the content of component (A2) in the fiber treatment agent is preferably 1.0% by mass or more, more preferably 2.0% by mass or more, even more preferably 5.0% by mass or more, and even more preferably 10% by mass or more. Furthermore, from the viewpoint of improving the feel of the fiber surface, it is preferably 70% by mass or less, more preferably 60% by mass or less, even more preferably 50% by mass or less, and even more preferably 40% by mass or less.

[0057] In other words, when component (A) is component (A2) and the pH of the fiber treatment agent is 6.5 or higher and 11.0 or lower, the content of component (A2) in the fiber treatment agent of the present invention is, from the above viewpoint, preferably 1.0 to 70% by mass, more preferably 2.0 to 60% by mass, even more preferably 5.0 to 50% by mass, and even more preferably 10 to 40% by mass.

[0058] Furthermore, when a fiber treatment agent contains two or more compounds as component (A), the overall solubility of component (A) tends to increase. For this reason, it is preferable that the fiber treatment agent contains two or more compounds as component (A) in order to improve the overall solubility of component (A), reduce the turbidity of the fiber treatment agent, enable uniform treatment of fibers, and thereby improve the feel of the fiber surface after treatment. When the fiber treatment agent contains two or more compounds as component (A), at least one of them is preferably an aromatic compound represented by general formula (2), and more preferably benzoic acid or a salt thereof. When an aromatic compound represented by general formula (2) is included in component (A), it is preferable that the content of this compound is the highest among component (A), and when benzoic acid or a salt thereof is included, it is even more preferable that the content of this compound is the highest among component (A).

[0059] When the pH of the fiber treatment agent is 2.0 or higher and less than 6.5, and the fiber treatment agent contains two or more compounds as component (A), the content of the remaining component (A) in the fiber treatment agent, after removing the compound with the highest concentration among all components (A), is preferably 0.1% by mass or more, more preferably 0.5% by mass or more, even more preferably 1.0% by mass or more, and also preferably 20% by mass or less, more preferably 10% by mass or less, and even more preferably 5.0% by mass or less.

[0060] Furthermore, if the pH of the fiber treatment agent is 6.5 or higher and 11.0 or lower, and the fiber treatment agent contains two or more compounds as component (A), the content of the remaining component (A) in the fiber treatment agent, excluding the compound with the highest concentration among all components (A), is preferably 0.5% by mass or more, more preferably 1.0% by mass or more, even more preferably 2.0% by mass or more, and also preferably 30% by mass or less, more preferably 20% by mass or less, and even more preferably 10% by mass or less.

[0061] In any case of the pH of the fiber treatment agent, if the fiber treatment agent contains two or more compounds as component (A), the mass ratio of the remaining component (A) excluding the compound with the highest concentration in all component (A) in the fiber treatment agent (mass of the remaining component (A) excluding the compound with the highest concentration in all component (A)) / (mass of the compound with the highest concentration in component (A)) is preferably 0.01 or higher, more preferably 0.05 or higher, even more preferably 0.10 or higher, and also preferably 1.0 or lower, more preferably 0.5 or lower, and even more preferably 0.25 or lower, from the viewpoint of improving the overall solubility of component (A), reducing the turbidity of the fiber treatment agent, enabling uniform treatment of fibers, and thereby improving the feel of the fiber surface after treatment.

[0062] [Component (B): Water] The fiber treatment agent of the present invention uses water as a medium. The content of component (B) in the fiber treatment agent of the present invention is preferably 10% by mass or more, more preferably 20% by mass or more, even more preferably 30% by mass or more, even more preferably 40% by mass or more, and also preferably 99% by mass or less, more preferably 95% by mass or less, even more preferably 90% by mass or less, and even more preferably 85% by mass or less. In other words, the content of component (B) in the fiber treatment agent of the present invention is preferably 10 to 99% by mass, more preferably 20 to 95% by mass, even more preferably 30 to 90% by mass, and even more preferably 40 to 85% by mass.

[0063] [Cationic surfactants] The fiber treatment agent of the present invention may contain a cationic surfactant to the extent that it does not impair the effects of the present invention. The cationic surfactant is preferably a monolong-chain alkylquaternary ammonium salt having one C8-C24 alkyl group and three C1-C4 alkyl groups.

[0064] Preferably, at least one monolong-chain alkylquaternary ammonium surfactant is selected from compounds represented by the following general formula (3).

[0065] [ka]

[0066] [In the formula, R 7 R is a saturated or unsaturated linear or branched alkyl group having 8 to 22 carbon atoms. 11 -CO-NH-(CH2) m - or R 11 -CO-O-(CH2) m -(R 11 (where p represents an integer from 1 to 4, and R represents a saturated or unsaturated linear or branched alkyl chain having 7 to 21 carbon atoms.) 8 , R 9 and R 10 These independently represent an alkyl group having 1 to 4 carbon atoms, or a hydroxylalkyl group having 1 to 4 carbon atoms, and An - This represents chloride ions, bromide ions, metosulfate ions, or ethosulfate ions.

[0067] Suitable cationic surfactants include, for example, long-chain quaternary ammonium compounds such as cetyltrimethylammonium chloride, myristyltrimethylammonium chloride, behentrimonium chloride, cetyltrimethylammonium bromide, and stearamidopropyltrimonium chloride, which can be used individually or as mixtures thereof.

[0068] The content of the cationic surfactant in the fiber treatment agent of the present invention is preferably 0.05% by mass or more, more preferably 0.10% by mass or more, and also preferably 10% by mass or less, more preferably 5.0% by mass or less, from the viewpoint of improving the feel of the surface of the natural fiber after treatment and further enhancing the effects of the present invention.

[0069] 〔silicone〕 Furthermore, the fiber treatment agent of the present invention may contain silicone to improve the feel of the surface of the treated natural fiber and to improve its cohesiveness. Preferably, the silicone is one or more selected from dimethylpolysiloxane and amino-modified silicones.

[0070] Any cyclic or acyclic dimethylpolysiloxane polymer can be used as the dimethylpolysiloxane, and examples include the SH200 series, BY22-019, BY22-020, BY11-026, B22-029, BY22-034, BY22-050A, BY22-055, BY22-060, BY22-083, FZ-4188 (all from Toray Dow Corning Co., Ltd.), KF-9088, KM-900 series, MK-15H, and MK-88 (all from Shin-Etsu Chemical Co., Ltd.).

[0071] Any silicone having an amino group or an ammonium group can be used as the amino-modified silicone. Examples include amino-modified silicone oil in which all or some of the terminal hydroxyl groups are terminally encapsulated with methyl groups, etc., and amodimethicone that is not terminally encapsulated. From the viewpoint of improving the feel of the surface of the natural fiber after treatment and improving its cohesiveness, preferred amino-modified silicones include, for example, the compound shown in the following formula.

[0072] [ka]

[0073] [In the formula, R' is a hydrogen atom, a hydroxyl group or R X Show, R Xrepresents a substituted or unsubstituted monovalent hydrocarbon group having 1 to 20 carbon atoms, and J is R X , R"-(NHCH2CH2) a NH2, OR X Or it represents a hydroxyl group, R'' represents a divalent hydrocarbon group having 1 to 8 carbon atoms, a represents a number from 0 to 3, and b and c represent a number such that their sum is number-average of 10 or more and less than 20,000, preferably 20 or more and less than 3,000, more preferably 30 or more and less than 1,000, and even more preferably 40 or more and less than 800.

[0074] Suitable commercially available amino-modified silicones include amino-modified silicone oils such as SF8452C and SS3551 (both from Toray Dow Corning Co., Ltd.), KF-8004, KF-867S, and KF-8015 (all from Shin-Etsu Chemical Co., Ltd.), and amodimethicone emulsions such as SM8704C, SM8904, BY22-079, FZ-4671, and FZ4672 (all from Toray Dow Corning Co., Ltd.).

[0075] The silicone content in the fiber treatment agent of the present invention is preferably 0.1% by mass or more, more preferably 0.2% by mass or more, even more preferably 0.5% by mass or more, and also preferably 20% by mass or less, more preferably 10% by mass or less, and even more preferably 5.0% by mass or less, from the viewpoint of improving the feel of the surface of the treated natural fiber and further enhancing the effects of the present invention.

[0076] [Cationic polymers] Furthermore, the fiber treatment agent of the present invention may contain a cationic polymer from the viewpoint of improving the surface feel of the natural fiber after treatment.

[0077] Cationic polymers are polymers having a cationic group or a group that can be ionized into a cationic group, and also include amphoteric polymers that are cationic overall. Specifically, they are aqueous solutions containing an amino group or an ammonium group in the side chain of the polymer chain, or containing diallyl quaternary ammonium salt as a constituent unit, such as cationized cellulose derivatives, cationic starch, cationized guar gum derivatives, polymers or copolymers of diallyl quaternary ammonium salt, and quaternized polyvinylpyrrolidone derivatives. Of these, from the viewpoint of improving the softness, smoothness and ease of handling during rinsing and shampooing, ease of manageability and moisturizing properties during drying, and the stability of the agent, one or more selected from polymers containing diallyl quaternary ammonium salt as a constituent unit, quaternized polyvinylpyrrolidone derivatives, and cationized cellulose derivatives are preferred, and one or more selected from polymers or copolymers of diallyl quaternary ammonium salt and cationized cellulose derivatives are more preferred.

[0078] Specific examples of suitable polymers or copolymers of diallyl quaternary ammonium salts include dimethyldiallylammonium chloride polymer (Polyquaternium-6, e.g., Merquart 100; Lubrizol Advanced Materials), dimethyldiallylammonium chloride / acrylic acid copolymer (Polyquaternium-22, e.g., Merquart 280, 295; Lubrizol Advanced Materials), and dimethyldiallylammonium chloride / acrylamide copolymer (Polyquaternium-7, e.g., Merquart 550; Lubrizol Advanced Materials).

[0079] Specific examples of suitable quaternized polyvinylpyrrolidone derivatives include polymers obtained by polymerizing vinylpyrrolidone copolymer and dimethylaminoethyl methacrylate (polyquaternium-11, e.g., Gaffcut 734, Gaffcut 755, Gaffcut 755N (all from Ashland)).

[0080] Suitable examples of cationized cellulose include polymers obtained by loading hydroxycellulose with glycidyltrimethylammonium chloride (Polyquaternium-10, e.g., Leoguard G, GP (both from Lion Corporation), Polymer JR-125, JR-400, JR-30M, LR-400, LR-30M (all from Amarcol)), and hydroxyethylcellulose dimethyldiallylammonium chloride (Polyquaternium-4, e.g., Cellcoat H-100, L-200 (both from AkzoNobel)).

[0081] The content of the cationic polymer in the fiber treatment agent of the present invention is preferably 0.001% by mass or more, more preferably 0.01% by mass or more, even more preferably 0.05% by mass or more, and also preferably 20% by mass or less, more preferably 10% by mass or less, from the viewpoint of improving the feel of the surface of the natural fiber after treatment.

[0082] Furthermore, the fiber treatment agent of the present invention may contain antioxidants such as ascorbic acid; and pH adjusters such as sodium hydroxide, potassium hydroxide, phosphoric acid, and hydrochloric acid.

[0083] [Iss] The pH of the fiber treatment agent of the present invention is preferably 2.0 or higher, more preferably 3.0 or higher, even more preferably 3.5 or higher, even more preferably 4.0 or higher, and also preferably 11.0 or lower, more preferably 10.0 or lower, and even more preferably 9.0 or lower, from the viewpoint of suppressing damage to natural fibers and improving durability. Note that the pH values ​​in the present invention are those at 25°C. In other words, the pH of the fiber treatment agent of the present invention is preferably 2.0 to 11.0, more preferably 3.0 to 10.0, even more preferably 3.5 to 9.0, and even more preferably 4.0 to 9.0, from the viewpoint of suppressing damage to natural fibers and improving their durability.

[0084] [Storage method for fiber treatment agents] When transporting and storing the fiber treatment agent manufactured as described above before applying it to fibers, or when transporting and storing the raw materials before preparing the fiber treatment agent, the storage temperature may be set to cold or high, or the voids in the storage container may be filled with nitrogen, in order to prevent unintended reaction or recrystallization of component (A) during transport.

[0085] The storage temperature for the fiber treatment agent is preferably 1°C or higher, more preferably 2°C or higher, and even more preferably 5°C or higher, from the viewpoint of preventing freezing and recrystallization. Furthermore, from the viewpoint of preventing oxidative discoloration and unintended reaction progression, it is preferably 25°C or lower, more preferably 20°C or lower, and even more preferably 15°C or lower.

[0086] Furthermore, the storage temperature of the fiber treatment agent is preferably 20°C or higher, more preferably 30°C or higher, and even more preferably 40°C or higher, from the viewpoint of preventing recrystallization of high-concentration solutions, and preferably 80°C or lower, more preferably 70°C or lower, and even more preferably 60°C or lower, from the viewpoint of preventing oxidative discoloration and unintended reaction progression.

[0087] [Fiber processing method] (Basic procedures) By treating naturally derived fibers using the fiber treatment agent of the present invention in a manner including the following step (i), it is possible to improve the water resistance and heat resistance, which are problems of naturally derived fibers, impart thermal shape memory ability, and improve elasticity (toughness) and surface feel. Step (i) Step of immersing natural fibers in the fiber treatment agent of the present invention.

[0088] In step (i), the natural fibers to be immersed in the fiber treatment agent may be dry or wet. The amount of fiber treatment agent used to immerse the natural fibers is preferably 2 or more, more preferably 3 or more, even more preferably 5 or more, even more preferably 10 or more, even more preferably 20 or more, and also preferably 500 or less, more preferably 250 or less, and even more preferably 100 or less, in terms of the bath ratio to the mass of the natural fibers (mass of fiber treatment agent / mass of natural fibers). In other words, the bath ratio is preferably 2 to 500, more preferably 3 to 250, even more preferably 5 to 100, even more preferably 10 to 100, and even more preferably 20 to 100.

[0089] Furthermore, in step (i), the natural fibers may be fixed in advance with a curler or the like, and then immersed in the fiber treatment agent of the present invention under heating. In this way, the natural fibers can be given a desired shape simultaneously, in addition to thermal shape memory and high durability.

[0090] In step (i), the immersion of the natural fiber into the fiber treatment agent is preferably carried out under heating, and this heating is performed by warming the fiber treatment agent. This heating may be carried out by immersing the natural fiber into the heated fiber treatment agent, or by immersing the natural fiber into the low-temperature fiber treatment agent and then heating it. The temperature of the fiber treatment agent is preferably 20°C or higher, more preferably 35°C or higher, and even more preferably 45°C or higher, in order to obtain the effects of the present invention by increasing the interaction between component (A) and the fiber constituent molecules in the natural fiber, such as protein molecules. Furthermore, in order to prevent the natural fiber from denatured and degraded by heat, the temperature is preferably less than 100°C, more preferably 80°C or lower, even more preferably 70°C or lower, and even more preferably 60°C or lower.

[0091] The immersion time in step (i) is adjusted as appropriate depending on the heating temperature, but for example, from the viewpoint of exhibiting an effect of improving the elasticity of natural fibers, it is preferably 15 minutes or more, more preferably 30 minutes or more, and even more preferably 1 hour or more, and in order to suppress damage to natural fibers, it is preferably 48 hours or less, more preferably 24 hours or less, and even more preferably 12 hours or less.

[0092] Step (i) is preferably carried out in an environment in which the evaporation of moisture is suppressed. Specific means of suppressing the evaporation of moisture include covering the container of the fiber treatment agent in which the natural fibers are immersed with a film-like substance, cap, lid, etc., made of a material that does not allow water vapor to pass through.

[0093] After step (i), the natural fibers may be rinsed or not, but rinsing is preferable from the viewpoint of preventing a decrease in the surface feel of the natural fibers due to excess component (A).

[0094] These processes are thought to cause various effects by allowing component (A) to penetrate into the naturally derived fibers and strongly coordinate with metals within the fibers, such as polyvalent metals.

[0095] [Further processing may be added] In addition to the above-mentioned step (i), one or more additional treatments may be performed, selected from decolorization, dyeing, surface finishing for hydrophobicity and friction reduction, and heat treatment for further improvement of fiber elasticity (toughness).

[0096] In this case, the decolorization and dyeing processes may be performed before or after step (i) described above. Furthermore, multiple processes can be combined and added. If both decolorization and dyeing are added, the order of the processes does not matter, except that decolorization must be performed before dyeing. Another process can also be performed between decolorization and dyeing.

[0097] On the other hand, surface finishing for hydrophobicity and friction reduction, and heat treatment for further improvement of fiber elasticity (toughness) must be performed after step (i) described above, but the order of these processes with decolorization and dyeing is not particularly limited. Also, surface finishing for hydrophobicity and friction reduction, and heat treatment for further improvement of fiber elasticity (toughness) may be performed in either order.

[0098] (bleaching) Decolorization is carried out by immersing natural fibers in a decolorizing agent composition containing an alkaline agent, an oxidizing agent, and water. The decolorizing agent composition is usually in two parts: the first part contains an alkaline agent and water, and the second part contains an oxidizing agent and water. These two parts are typically stored separately and mixed before immersing the natural fibers.

[0099] Suitable alkaline agents include, but are not limited to, ammonia and its salts; alkanolamines (monoethanolamine, isopropanolamine, 2-amino-2-methylpropanol, 2-aminobutanol, etc.) and their salts; alkanediamines (1,3-propanediamine, etc.) and their salts; and carbonates (guanidine carbonate, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, etc.) and mixtures thereof.

[0100] The content of the alkaline agent in the decolorizing agent composition (in the case of a two-part type, a mixture of the first and second components) is preferably 0.1% by mass or more, more preferably 0.5% by mass or more, even more preferably 1.0% by mass or more, and also preferably 15% by mass or less, more preferably 10% by mass or less, and even more preferably 7.5% by mass or less.

[0101] Suitable oxidizing agents include, but are not limited to, hydrogen peroxide, urea peroxide, melamine peroxide, and sodium bromate. Among these oxidizing agents, hydrogen peroxide is preferred.

[0102] The content of the oxidizing agent in the decolorizing agent composition is preferably 1% by mass or more, more preferably 2% by mass or more, and also preferably 15% by mass or less, more preferably 12% by mass or less, and even more preferably 9% by mass or less.

[0103] When the first and second agents are stored separately, the pH of the second agent at 25°C is preferably 2.0 or higher, more preferably 2.5 or higher, and also preferably 6.0 or lower, more preferably 4.0 or lower. This pH can be adjusted with a suitable buffer. The pH of the decolorizing agent composition at 25°C is preferably 6 or higher, more preferably 6.5 or higher, even more preferably 6.8 or higher, and also preferably 11.0 or lower, more preferably 10.5 or lower, and even more preferably 10.0 or lower.

[0104] (staining) Dyeing is carried out by immersing natural fibers in a dyeing composition. The dyeing composition contains dyes and may optionally contain alkaline agents, acids, oxidizing agents, etc. Examples of dyes include direct dyes, oxidation dyes, and combinations thereof.

[0105] The type of direct dye is not particularly limited, and any direct dye suitable for dyeing can be used. Examples of direct dyes include anionic dyes, nitro dyes, disperse dyes, cationic dyes, and dyes having an azophenol structure selected from the group consisting of HC Red 18, HC Blue 18, and HC Yellow 16, as well as salts thereof and mixtures thereof.

[0106] [ka]

[0107] Examples of cationic dyes include, but are not limited to, Basic Blue 6, Basic Blue 7, Basic Blue 9, Basic Blue 26, Basic Blue 41, Basic Blue 99, Basic Brown 4, Basic Brown 16, Basic Brown 17, Natural Brown 7, Basic Green 1, Basic Orange 31, Basic Red 2, Basic Red 12, Basic Red 22, Basic Red 51, Basic Red 76, Basic Violet 1, Basic Violet 2, Basic Violet 3, Basic Violet 10, Basic Violet 14, Basic Yellow 57, and Basic Yellow 87, as well as mixtures thereof. Basic Red 51, Basic Orange 31, Basic Yellow 87, and mixtures thereof are particularly preferred.

[0108] Examples of anionic dyes include Acid Black 1, Acid Blue 1, Acid Blue 3, Acid Blue 5, Acid Blue 7, Acid Blue 9, Acid Blue 74, Acid Orange 3, Acid Orange 4, Acid Orange 6, Acid Orange 7, Acid Orange 10, Acid Red 1, Acid Red 14, Acid Red 18, Acid Red 27, Acid Red 33, Acid Red 50, Acid Red 52, Acid Red 73, Acid Red 87, Acid Red 88, Acid Red 92, Acid Red 155, Acid Red 180, Acid Violet 2, Acid Violet 9, Acid Violet 43, Acid Violet 49, Acid Yellow 1, Acid Examples include, but are not limited to, Yellow 10, Acid Yellow 23, Acid Yellow 3, Food Yellow No. 8, D&C Brown No. 1, D&C Green No. 5, D&C Green No. 8, D&C Orange No. 4, D&C Orange No. 10, D&C Orange No. 11, D&C Red No. 21, D&C Red No. 27, D&C Red No. 33, D&C Violet 2, D&C Yellow No. 7, D&C Yellow No. 8, D&C Yellow No. 10, FD&C Red 2, FD&C Red 40, FD&C Red No. 4, FD&C Yellow No. 6, FD&C Blue 1, Food Black 1, Food Black 2, as well as alkali metal salts of these (sodium salts, potassium salts, etc.) and mixtures thereof.

[0109] Among these, preferred anionic dyes are Acid Black 1, Acid Red 52, Acid Violet 2, Acid Violet 43, Acid Red 33, Acid Orange 4, Acid Orange 7, Acid Red 27, Acid Yellow 3, and Acid Yellow 10, as well as their salts. More preferred anionic dyes are Acid Red 52, Acid Violet 2, Acid Red 33, Acid Orange 4, and Acid Yellow 10, as well as their salts and mixtures.

[0110] Examples of nitro dyes include HC Blue No. 2, HC Blue No. 4, HC Blue No. 5, HC Blue No. 6, HC Blue No. 7, HC Blue No. 8, HC Blue No. 9, HC Blue No. 10, HC Blue No. 11, HC Blue No. 12, HC Blue No. 13, HC Brown No. 1, HC Brown No. 2, HC Green No. 1, HC Orange No. 1, HC Orange No. 2, HC Orange No. 3, HC Orange No. 5, HC Red BN, HC Red No. 1, HC Red No. 3, HC Red No. 7, HC Red No. 8, HC Red No. 9, HC Red No. 10, HC Red No. 11, HC Red No. 13, HC Red No. 54, HC Red No. 14, HC Violet BS, HC Examples include, but are not limited to, Violet No. 1, HC Violet No. 2, HC Yellow No. 2, HC Yellow No. 4, HC Yellow No. 5, HC Yellow No. 6, HC Yellow No. 7, HC Yellow No. 8, HC Yellow No. 9, HC Yellow No. 10, HC Yellow No. 11, HC Yellow No. 12, HC Yellow No. 13, HC Yellow No. 14, HC Yellow No. 15, 2-amino-6-chloro-4-nitrophenol, picramic acid, 1,2-diamino-4-nitrobenzol, 1,4-diamino-2-nitrobenzol, 3-nitro-4-aminophenol, 1-hydroxy-2-amino-3-nitrobenzol, and 2-hydroxyethylpicramic acid, as well as mixtures thereof.

[0111] Examples of disperse dyes include, but are not limited to, Disperse Blue 1, Disperse Black 9, and Disperse Violet 1, and mixtures thereof.

[0112] These direct dyes can be used individually or in combination of two or more, and direct dyes with different ionic properties can also be used together.

[0113] From the viewpoint of obtaining sufficient dyeing properties, the content of direct dyes in the dyeing agent composition is preferably 0.001% by mass or more, more preferably 0.01% by mass or more, and even more preferably 0.05% by mass or more. From the viewpoint of compatibility, it is preferably 10% by mass or less, more preferably 7.5% by mass or less, even more preferably 5.0% by mass or less, and even more preferably 3.0% by mass or less.

[0114] If the dyeing composition contains only direct dyes as dyes, an oxidizing agent is not necessary to dye natural fibers. However, if you want to lighten the color of natural fibers, you can include an oxidizing agent in the composition.

[0115] When a dyeing composition contains an oxidative dye, it is usually a two-part system. The first part contains an oxidative dye intermediate (precursor and coupler) and an alkaline agent, while the second part contains an oxidizing agent such as hydrogen peroxide. These two parts are usually stored separately and mixed before immersing the natural fiber.

[0116] There are no particular restrictions on the oxidation dye intermediate; any known precursor and coupler commonly used in dyed products can be suitably used.

[0117] Precursors include, for example, paraphenylenediamine, toluene-2,5-diamine, 2-chloro-paraphenylenediamine, N-methoxyethyl-paraphenylenediamine, N-phenylparaphenylenediamine, N,N-bis(2-hydroxyethyl)-paraphenylenediamine, 2-(2-hydroxyethyl)-paraphenylenediamine, 2,6-dimethyl-paraphenylenediamine, 4,4'-diaminodiphenylamine, 1,3-bis(N-(2-hydroxyethyl)-N-(4-aminophenyl)amino)-2-propanol, PEG-3,3,2'-paraphenylenediamine, para-aminophenol, para-methylaminophenol, 3 Examples include, but are not limited to, methyl-4-aminophenol, 2-aminomethyl-4-aminophenol, 2-(2-hydroxyethylaminomethyl)-4-aminophenol, orthoaminophenol, 2-amino-5-methylphenol, 2-amino-6-methylphenol, 2-amino-5-acetamidophenol, 3,4-diaminobenzoic acid, 5-aminosalicylic acid, 2,4,5,6-tetraaminopyrimidine, 2,5,6-triamino-4-hydroxypyrimidine, 4,5-diamino-1-(4'-chlorobenzyl)pyrazole, 4,5-diamino-1-hydroxyethylpyrazole, and salts of these substances and mixtures thereof.

[0118] Examples of couplers include metaphenylenediamine, 2,4-diaminophenoxyethanol, 2-amino-4-(2-hydroxyethylamino)anisole, 2,4-diamino-5-methylphenethole, 2,4-diamino-5-(2-hydroxyethoxy)toluene, 2,4-dimethoxy-1,3-diaminobenzene, 2,6-bis(2-hydroxyethylamino)toluene, 2,4-diamino-5-fluorotoluene, 1,3-bis(2,4-diaminophenoxy)propane, metaaminophenol, 2-methyl-5-aminophenol, 2-methyl-5-(2-hydroxyethylamino)phenol, 2,4-dichloro-3-aminophenol, 2-chloro-3-amino-6-methylphenol, 2-methyl-4-chloro-5-aminophenol, N-cyclopentyl-methaminophenol, 2-methyl-4-methoxy-5-(2-hydroxyethylamino)phenol, 2-methyl-4-fluoro-5-aminophenol, para-amino-o-toxylethanolamine Zol, resorcinol, 2-methylresorcinol, 4-chlororesorcinol, 1-naphthol, 1,5-dihydroxynaphthalene, 1,7-dihydroxynaphthalene, 2,7-dihydroxynaphthalene, 2-isopropyl-5-methylphenol, 4-hydroxyindole, 5-hydroxyindole, 6-hydroxyindole, 7-hydroxyindole, 6-hydroxybenzomorpholine, 3,4-methylenedioxyphenol, 2-bromo-4,5-methylenedioxyphenol Examples include, but are not limited to, 3,4-methylenedioxyaniline, 1-(2-hydroxyethyl)amino-3,4-methylenedioxybenzene, 2,6-dihydroxy-3,4-dimethylpyridine, 2,6-dimethoxy-3,5-diaminopyridine, 2,3-diamino-6-methoxypyridine, 2-methylamino-3-amino-6-methoxypyridine, 2-amino-3-hydroxypyridine, 2,6-diaminopyridine, and salts of these substances and mixtures thereof.

[0119] The content of precursor and coupler in the dyeing agent composition is preferably 0.01% by mass or more, more preferably 0.1% by mass or more, and also preferably 10% by mass or less, more preferably 7.5% by mass or less, and even more preferably 5.0% by mass or less.

[0120] If the dyeing composition contains an oxidation dye, it further contains an alkaline agent. Suitable alkaline agents include, but are not limited to, ammonia and its salts; alkanolamines (monoethanolamine, isopropanolamine, 2-amino-2-methylpropanol, 2-aminobutanol, etc.) and their salts; alkanediamines (1,3-propanediamine, etc.) and their salts; and carbonates (guanidine carbonate, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, etc.); and mixtures thereof.

[0121] The content of the alkaline agent in the dyeing agent composition is preferably 0.1% by mass or more, more preferably 0.5% by mass or more, even more preferably 1.0% by mass or more, and also preferably 15% by mass or less, more preferably 10% by mass or less, and even more preferably 7.5% by mass or less.

[0122] When the dyeing composition contains an oxidative dye, the oxidizing agent composition (second agent) is stored separately from the oxidative dye composition (first agent) and mixed before immersing the natural fiber. Suitable oxidizing agents include, but are not limited to, hydrogen peroxide, urea peroxide, melamine peroxide, and sodium bromate. Among these oxidizing agents, hydrogen peroxide is preferred.

[0123] The content of the oxidizing agent in the dyeing agent composition is preferably 1% by mass or more, more preferably 2% by mass or more, and also preferably 15% by mass or less, more preferably 12% by mass or less, and even more preferably 9% by mass or less.

[0124] When the first and second agents are stored separately, the pH of the second agent at 25°C is preferably 2 or higher, more preferably 2.5 or higher, and also preferably 6 or lower, more preferably 4 or lower. This pH can be adjusted with a suitable buffer. The pH of the dyeing composition obtained by mixing the first and second agents at 25°C is preferably 6 or higher, more preferably 6.5 or higher, even more preferably 6.8 or higher, and also preferably 11 or lower, more preferably 10.5 or lower, and even more preferably 10 or lower.

[0125] If the dyeing composition contains an oxidation dye, it may further contain the direct dyes exemplified above.

[0126] The dyeing composition may preferably further contain the following surfactants, conditioning components, etc., and may preferably take the form of a solution, emulsion, cream, paste, or mousse.

[0127] The temperature of the dyeing agent composition is preferably 0°C or higher, more preferably 10°C or higher, even more preferably 20°C or higher, and also preferably 90°C or lower, more preferably 80°C or lower, from the viewpoint of efficiently penetrating and diffusing the dyeing agent composition into the natural fiber and further enhancing the dyeing effect.

[0128] (Post-heating: Heat treatment to further improve fiber elasticity (toughness)) Furthermore, from the viewpoint of more effectively improving the elasticity of natural fibers, natural fibers can be heated while being stretched under tension. For small quantities of natural fibers, it is preferable to use a hair iron for this heating, and for large quantities, equivalent results can be obtained by applying tension with a winding machine while heating with hot air.

[0129] The fiber stretch rate during heating is preferably 0.1% or more, more preferably 0.2% or more, and even more preferably 0.5% or more, from the viewpoint of more effectively improving the elasticity of the fibers, and from the viewpoint of suppressing damage to the fibers, it is preferably 10% or less, more preferably 5.0% or less, and even more preferably 2.0% or less.

[0130] The heating temperature is preferably 120°C or higher, more preferably 140°C or higher, and even more preferably 160°C or higher, from the viewpoint of more effectively improving the elasticity of the fibers, and preferably 240°C or lower, more preferably 220°C or lower, and even more preferably 200°C or lower, from the viewpoint of suppressing damage to the fibers.

[0131] The heating time is preferably 1 second or more, more preferably 3 seconds or more, and even more preferably 5 seconds or more, from the viewpoint of more effectively improving the elasticity of the fibers, and from the viewpoint of suppressing damage to the fibers, it is preferably 60 seconds or less, more preferably 30 seconds or less, and even more preferably 20 seconds or less.

[0132] After heating, the natural fibers can be subjected to tension and stretched while being left to stand in water, in order to more effectively improve their elasticity.

[0133] The elongation rate in this case is preferably 0.1% or more, more preferably 0.2% or more, and even more preferably 0.5% or more, from the viewpoint of more effectively improving the elasticity of the fibers, and from the viewpoint of suppressing damage to the fibers, it is preferably 10% or less, more preferably 5.0% or less, and even more preferably 2.0% or less.

[0134] From the viewpoint of more effectively improving the elasticity of the fibers, the water temperature is preferably 5°C or higher, more preferably 20°C or higher, and even more preferably 30°C or higher. Furthermore, from the viewpoint of suppressing damage to the fibers, the water temperature is preferably 80°C or lower, more preferably 60°C or lower, and even more preferably 50°C or lower.

[0135] The standing time in water is preferably 1 minute or more, more preferably 5 minutes or more, and even more preferably 30 minutes or more, from the viewpoint of more effectively improving the elasticity of the fibers, and from the viewpoint of suppressing damage to the fibers, it is preferably 48 hours or less, more preferably 24 hours or less, and even more preferably 3 hours or less.

[0136] This operation, depending on the processing conditions in step (i), can achieve elasticity comparable to human hair during fiber drying.

[0137] The fibers that have undergone the various treatments described above can then have their texture improved by conventional post-treatments, such as treatment with fabric softeners or other fiber treatment agents, or treatment with conditioners or hair treatments.

[0138] By processing natural fibers using the above fiber processing method, component (A) is incorporated into the fibers, allowing them to be shaped by heat setting, resulting in fibers with excellent water resistance, heat resistance, and tensile modulus, and highly improved elasticity (toughness) of natural fibers. These fibers, preferably for headwear products, can be manufactured, and various textile products, preferably headwear products, can be manufactured using these fibers. Suitable headwear products in this invention include, for example, hair wigs, hairpieces, weaving, hair extensions, braided hair, hair accessories, doll hair, and the like.

[0139] With respect to the embodiments described above, preferred embodiments of the present invention are further disclosed below.

[0140] <1> A fiber treatment agent containing the following components (A) and (B). (A): The hydrogen bonding term δH of Hansen's solubility parameter is 18.3 MPa 1 / 2 The following compounds have at least one carboxyl group or a salt thereof and do not have a fused ring. (B):Water

[0141] <2> Preferably, component (A) is one or more compounds selected from the group consisting of the following components (A1) and (A2). <1> The fiber treatment agent described above. (A1) The hydrogen bonding term δH of Hansen's solubility parameter is 18.3 MPa 1 / 2 The following are aromatic compounds having at least one carboxyl group or a salt thereof and not having a fused ring: (A2) The hydrogen bonding term δH of Hansen's solubility parameter is 11.0 MPa 1 / 2 The above is 18.3 MPa. 1 / 2 The following are compounds (excluding aromatic compounds) that have at least one carboxyl group or a salt thereof and do not have a fused ring:

[0142] <3> Component (A1) is a compound represented by the following general formula (1) or general formula (2), or a salt thereof, or phenylbutanoic acid. <2> The fiber treatment agent described above.

[0143] [ka]

[0144] [In the formula, =X represents a methylidene group or an oxo group, R 1 R represents a hydrogen atom, a hydroxyl group, or an alkyl group, aryl group, alkoxy group, aryloxy group, or aralkyloxy group which may have substituents. 2 represents an o-phenylene group, an m-phenylene group, a p-phenylene group, a benzylidene group, or an alkylene group which may have a substituent. However, R 2 If it does not have an aryl group, then R 1 This is an aryl group, an aryloxy group, or an aralkyloxy group.

[0145] [ka]

[0146] [In the ceremony, A 1 ~A 5Each of these independently represents a hydrogen atom, an acetyl group, a halogen atom, or a linear or branched alkyl group, alkenyl group, alkoxy group, or alkenyloxy group having 1 to 6 carbon atoms.

[0147] <4> The compound represented by general formula (1) is the compound represented by general formula (1A), (1B), or (1C) shown below, 3-carboxybenzoic acid (isophthalic acid), 4-carboxybenzoic acid (terephthalic acid), 3-benzoylbenzoic acid, or 4-benzoylbenzoic acid. <3> The fiber treatment agent described above.

[0148] [ka]

[0149] [In the formula, B 1 ~B 4 Each of these independently represents a hydrogen atom, an acetyl group, a halogen atom, or a linear or branched alkyl group, alkenyl group, alkoxy group, or alkenyloxy group having 1 to 6 carbon atoms, and R 3 represents a hydroxyl group, or a group represented by the following general formula (1A)-a or (1A)-b.

[0150] [ka]

[0151] [In the formula, B 5 ~B 9 is the aforementioned B 1 ~B 4 It has the same meaning as R 4 [where n represents a hydrogen atom or a methyl group, and n represents an integer between 0 and 2.]

[0152] [ka]

[0153] [In the formula, D 1 ~D 4Each of these independently represents a hydrogen atom, an acetyl group, a halogen atom, or a linear or branched alkyl group, alkenyl group, alkoxy group, or alkenyloxy group having 1 to 6 carbon atoms, and E 1 ~E 5 Each is independent of D 1 ~D 4 This indicates a group similar to or represented by general formula (1B)-a.

[0154] [ka]

[0155] [In the formula, m represents an integer between 0 and 4.]

[0156] [ka]

[0157] [In the formula, R 6 represents a hydrogen atom or a group represented by the general formula (1C)-a, G 1 and G 2 Each of these independently represents a hydrogen atom, an acetyl group, a halogen atom, an optionally substituted aryl group, a C7-C12 aralkyl group or arylalkenyl group, or a C1-C6 linear or branched alkyl group, alkenyl group, alkoxy group, alkenyloxy group or alloyloxy group. However, R 6 If G is a hydrogen atom, 1 and G 2 At least one of these is an aryl group which may have substituents, an aralkyl group having 7 to 12 carbon atoms, an arylalkenyl group, or an alloyloxy group.

[0158] [ka]

[0159] [During the ceremony, J 1 ~J 5Each of these independently represents a hydrogen atom, an acetyl group, a halogen atom, or a linear or branched alkyl group, alkenyl group, alkoxy group, or alkenyloxy group having 1 to 6 carbon atoms.

[0160] <5> The compound represented by general formula (1A) is preferably 2-carboxybenzoic acid (phthalic acid), 2-(((4-vinylbenzyl)oxy)carbonyl)benzoic acid, 2-((2-(acryloyloxy)ethoxy)carbonyl)benzoic acid, or 2-((2-(methacryloyloxy)ethoxy)carbonyl)benzoic acid. <4> The fiber treatment agent described above.

[0161] <6> The compound represented by general formula (1B) is preferably 2-benzoylbenzoic acid, 2-(2-methylbenzoyl)benzoic acid, 2-(3-methylbenzoyl)benzoic acid, 2-(4-methylbenzoyl)benzoic acid, 2-(2-chlorobenzoyl)benzoic acid, 2-(3-chlorobenzoyl)benzoic acid, 2-(4-chlorobenzoyl)benzoic acid, or 2-(4-(2-(2-(acryloyloxy)ethoxy)ethoxy)benzoyl)benzoic acid. <4> The fiber treatment agent described above.

[0162] <7> The compound represented by general formula (1C) is preferably phenylsuccinic acid, 2,3-diphenylsuccinic acid, (+)-di-p-thuloyl-D-tartaric acid, or 4-oxo-4-((4-vinylbenzyl)oxy)butanoic acid. <4> The fiber treatment agent described above.

[0163] <8> The compound represented by general formula (2) is benzoic acid, 2-methylbenzoic acid, 3-methylbenzoic acid, 4-methylbenzoic acid, 2-ethylbenzoic acid, 3-ethylbenzoic acid, 4-ethylbenzoic acid, 2-propylbenzoic acid, 3-propylbenzoic acid, 4-propylbenzoic acid, 2-isopropylbenzoic acid, 3-isopropylbenzoic acid, 4-isopropylbenzoic acid, 2-n-butylbenzoic acid, 3-n-butylbenzoic acid, 4-n-butylbenzoic acid, 2-tert-butylbenzoic acid, 3-tert-butylbenzoic acid Aromatic acid, 4-tert-butylbenzoic acid, 2-vinylbenzoic acid, 3-vinylbenzoic acid, 4-vinylbenzoic acid, 2-acetylbenzoic acid, 3-acetylbenzoic acid, 4-acetylbenzoic acid, 2-methoxybenzoic acid, 3-methoxybenzoic acid, 4-methoxybenzoic acid, 2-chlorobenzoic acid, 3-chlorobenzoic acid, 4-chlorobenzoic acid, 2-bromobenzoic acid, 3-bromobenzoic acid, or 4-bromobenzoic acid, more preferably 4-ethylbenzoic acid, 4-vinylbenzoic acid, or benzoic acid. <3> The fiber treatment agent described above.

[0164] <9> The hydrogen bond term δH of the aromatic compound of component (A1) is preferably 16.0 MPa. 1 / 2 More preferably, 13.5 MPa 1 / 2 More preferably, 12.0 MPa 1 / 2 More preferably, 10.0 MPa 1 / 2 The following, and preferably 3.0 MPa 1 / 2 More preferably 4.0 MPa 1 / 2 More preferably, 5.0 MPa 1 / 2 That's all. <2> ~ <8> A fiber treatment agent as described in any one of the items.

[0165] <10> The component (A2) is potassium 2,4-hexadienate. <2> The fiber treatment agent described above.

[0166] <11> The hydrogen bonding term δH of the compound of component (A2) is preferably 16.0 MPa. 1 / 2 More preferably, 15.0 MPa 1 / 2More preferably, 14.0 MPa 1 / 2 More preferably, 13.0 MPa 1 / 2 The following, and preferably 11.0 MPa 1 / 2 The above comfort level is 11.5 MPa. 1 / 2 More preferably, 12.0 MPa 1 / 2 That's all. <2> or <10> The fiber treatment agent described above.

[0167] <12> The content of component (B) is preferably 10% by mass or more, more preferably 20% by mass or more, even more preferably 30% by mass or more, even more preferably 40% by mass or more, and also preferably 99% by mass or less, more preferably 95% by mass or less, even more preferably 90% by mass or less, and even more preferably 85% by mass or less. <1> ~ <11> A fiber treatment agent as described in any one of the items.

[0168] <13> The pH at 25°C is preferably 2.0 or higher, more preferably 3.0 or higher, even more preferably 3.5 or higher, even more preferably 4.0 or higher, and also preferably 11.0 or lower, more preferably 10.0 or lower, and even more preferably 9.0 or lower. <1> ~ <12> A fiber treatment agent as described in any one of the items.

[0169] <14> Component (A) contains (A1-1) benzoic acid or a salt thereof. <1> ~ <13> A fiber treatment agent as described in any one of the items.

[0170] <15> The pH of the fiber treatment agent is 2.0 or higher and less than 6.5, and the content of component (A1-1) in the fiber treatment agent is preferably 0.8% by mass or more, more preferably 3.0% by mass or more, even more preferably 5.0% by mass or more, even more preferably 10% by mass or more, even more preferably 15% by mass or more, even more preferably 20% by mass or more, and also preferably 90% by mass or less, more preferably 80% by mass or less, even more preferably 70% by mass or less, even more preferably 50% by mass or less, even more preferably 40% by mass or less, and even more preferably 35% by mass or less. <14> The fiber treatment agent described above.

[0171] <16> The pH of the fiber treatment agent is 6.5 or higher and 11.0 or lower, and the content of component (A1-1) in the fiber treatment agent is preferably 0.8% by mass or more, more preferably 3.0% by mass or more, even more preferably 5.0% by mass or more, even more preferably 10% by mass or more, even more preferably 15% by mass or more, even more preferably 20% by mass or more, even more preferably 25% by mass or more, even more preferably 26% by mass or more, even more preferably 28% by mass or more, even more preferably 30% by mass or more, and also preferably 90% by mass or less, more preferably 80% by mass or less, even more preferably 70% by mass or less, even more preferably 50% by mass or less, even more preferably 45% by mass or less, and even more preferably 40% by mass or less. <14> The fiber treatment agent described above.

[0172] <17> Component (A) contains component (A1) other than (A1-2) benzoic acid or its salt, <1> ~ <13> A fiber treatment agent as described in any one of the items.

[0173] <18> The pH of the fiber treatment agent is 2.0 or higher and less than 6.5, and the content of component (A1-2) in the fiber treatment agent is preferably 0.1% by mass or more, more preferably 0.2% by mass or more, even more preferably 0.5% by mass or more, even more preferably 1.0% by mass or more, and also preferably 70% by mass or less, more preferably 60% by mass or less, even more preferably 50% by mass or less, and even more preferably 45% by mass or less. <17> The fiber treatment agent described above.

[0174] <19> The pH of the fiber treatment agent is 6.5 or higher and 11.0 or lower, and the content of component (A1-2) in the fiber treatment agent is preferably 1.0% by mass or more, more preferably 2.0% by mass or more, even more preferably 5.0% by mass or more, even more preferably 10% by mass or more, and also preferably 70% by mass or less, more preferably 60% by mass or less, even more preferably 50% by mass or less, and even more preferably 40% by mass or less. <17> The fiber treatment agent described above.

[0175] <20> Component (A) contains component (A2), <1> ~ <13> A fiber treatment agent as described in any one of the items.

[0176] <21> The pH of the fiber treatment agent is 2.0 or higher and less than 6.5, and the content of component (A2) in the fiber treatment agent is preferably 0.1% by mass or more, more preferably 0.2% by mass or more, even more preferably 0.5% by mass or more, even more preferably 1.0% by mass or more, and also preferably 60% by mass or less, more preferably 50% by mass or less, even more preferably 40% by mass or less, and even more preferably 30% by mass or less. <20> The fiber treatment agent described above.

[0177] <22> The pH of the fiber treatment agent is 6.5 or higher and 11.0 or lower, and the content of component (A2) in the fiber treatment agent is preferably 1.0% by mass or more, more preferably 2.0% by mass or more, even more preferably 5.0% by mass or more, even more preferably 10% by mass or more, and also preferably 70% by mass or less, more preferably 60% by mass or less, even more preferably 50% by mass or less, and even more preferably 40% by mass or less. <20> The fiber treatment agent described above.

[0178] <23> The component (A) contains two or more compounds. <1> ~ <22> A fiber treatment agent as described in any one of the items.

[0179] <24> At least one of component (A) is preferably an aromatic compound represented by general formula (2), and more preferably benzoic acid or a salt thereof. <23> The fiber treatment agent described above.

[0180] <25> Preferably, the content of the aromatic compound represented by general formula (2) is highest among component (A), and more preferably, the content of benzoic acid or its salt is highest among component (A). <24> The fiber treatment agent described above.

[0181] <26> The pH of the fiber treatment agent is 2.0 or higher and less than 6.5, and the content of the remaining component (A) in the fiber treatment agent, after removing the compound with the highest concentration among all components (A), is preferably 0.1% by mass or more, more preferably 0.5% by mass or more, even more preferably 1.0% by mass or more, and also preferably 20% by mass or less, more preferably 10% by mass or less, and even more preferably 5.0% by mass or less. <23> ~ <25> A fiber treatment agent as described in any one of the items.

[0182] <27> The pH of the fiber treatment agent is 6.5 or higher and 11.0 or lower, and the content of the remaining component (A) in the fiber treatment agent, after removing the compound with the highest concentration among all components (A), is preferably 0.5% by mass or more, more preferably 1.0% by mass or more, even more preferably 2.0% by mass or more, and also preferably 30% by mass or less, more preferably 20% by mass or less, and even more preferably 10% by mass or less. <23> ~ <25> A fiber treatment agent as described in any one of the items.

[0183] <28> The mass ratio of the remaining component (A) after removing the compound with the highest concentration in all component (A) in the fiber treatment agent (mass of the remaining component (A) after removing the compound with the highest concentration in all component (A)) / (mass of the compound with the highest concentration in component (A)) is preferably 0.01 or more, more preferably 0.05 or more, even more preferably 0.10 or more, and also preferably 1.0 or less, more preferably 0.5 or less, and even more preferably 0.25 or less. <23> ~ <27> A fiber treatment agent as described in any one of the items.

[0184] <29> A fiber processing method including the following step (i). Step (i) A step of immersing natural fibers in a composition containing the following components (A) and (B). (A): The hydrogen bonding term δH of Hansen's solubility parameter is 18.3 MPa 1 / 2 The following compounds have at least one carboxyl group or a salt thereof and do not have a fused ring. (B):Water

[0185] <30> A fiber processing method including the following step (i). Step (i) A step of immersing natural fibers in a composition containing the following components (A1-2) and (B). (A1-2): The hydrogen bonding term δH of Hansen's solubility parameter is 18.3 MPa 1 / 2 The following compounds have at least one carboxyl group or a salt thereof and do not have a fused ring (excluding benzoic acid and its salts): (B):Water

[0186] <31> Use as a fiber treatment agent for a composition containing the following components (A) and (B). (A): A compound having at least one carboxy group or a salt thereof and no condensed ring, wherein the hydrogen bonding term δH of Hansen's solubility parameter is 18.3 MPa 1 / 2 (B): Water

[0187] <32> Use as a fiber treatment agent for a composition containing the following components (A1-2) and (B). (A1-2): A compound having at least one carboxy group or a salt thereof and no condensed ring (excluding benzoic acid and its salts), wherein the hydrogen bonding term δH of Hansen's solubility parameter is 18.3 MPa 1 / 2 (B): Water

Examples

[0188] Examples 1 to 22, Comparative Examples 1 to 3 Using the compositions with the formulations shown in Tables 1 and 2, regenerated collagen fibers were treated according to the following method, and various evaluations were performed. The pH of each composition was measured directly with a pH meter (HORIBA, F-52) at room temperature (25°C).

[0189] <Treatment method> 1. A 0.50 g tuft of regenerated collagen fibers (※) with a length of 22 cm was immersed in a container containing a fiber treatment agent in the bath ratio shown in the table, the mouth of the container was sealed, and the container was immersed in a water bath (manufacturer: Toyo Seisakusho Co., Ltd. / model number: TBS221FA) at the temperature shown in the table and heated for the time shown in the table. ※: Regenerated collagen fibers manufactured by Kaneka were purchased in the form of a commercial extension product, and the fibers were cut from it and divided into small tufts for use in the evaluation. In this evaluation, Ultima 100% was used as the fiber type in the extension product, and the white with a color number of 30 and a straight shape was used. 2. The container containing the tuft was taken out of the water bath and returned to room temperature.​​ 3. Remove the hair strands from the container, rinse with 30°C running tap water for 30 seconds, lather with the evaluation shampoo for 60 seconds, rinse with 30°C running tap water for 30 seconds, lightly towel dry, and then dry the hair strands with a warm air dryer (Tescom Nobby White NB3000) while combing.

[0190] <Formula for the evaluation shampoo> Ingredients (mass%) Sodium laureth sulfate 15.5 Lauramide DEA 1.5 EDTA-2Na 0.3 Amount of phosphoric acid to adjust pH to 7 Ion-exchanged water Balance Total 100

[0191] <Increase in average elongation at break during fiber tension> As indicators of water resistance and elasticity (toughness), the average elongation at break during fiber tension, that is, the percentage of the original fiber length at which breakage occurs when the fiber is stretched under tension, was evaluated using the average value obtained from multiple fibers (10 fibers). The evaluation was performed using hair bundles immediately after treatment with the above-mentioned <treatment method>, following the procedure below. 1. Ten fibers were cut from the base of the hair bundle. A 3cm fiber piece was taken from the middle of the base and tip of each fiber, resulting in a total of 10 3cm hair pieces. 2. The fiber samples were placed in a DIA-STRON limited "MTT690 Automatic Fiber Tensile Tester". After being left immersed in water for 30 minutes, automatic measurement was started, and the average elongation at break while the fibers were immersed in water was determined. A higher value indicates greater elasticity, superior toughness, and superior durability. According to the following formula, the average elongation at break (A%) when fibers are pulled taut in their untreated state (untreated; Comparative Example 1) is used as the baseline. The table shows the percentage increase (C%) in the average elongation at break (B%) of treated hair bundles compared to the untreated state, as indicated by "Percentage increase in average elongation at break [%]". C(%) = B(%) - A(%)

[0192] <Increase in average breaking load during fiber tension> As an indicator of water resistance, the average breaking load under fiber tensile stress was used. The evaluation was performed using fiber bundles immediately after treatment using the above-described <treatment method>. Furthermore, the average value obtained when evaluating multiple fibers (10 fibers) was used as the numerical value. The evaluation was performed according to the following procedure. 1. Ten fibers were cut from the base of the hair bundle. A 3cm fiber piece was taken from the middle of the base and tip of each fiber, resulting in a total of 10 3cm hair pieces. 2. The fiber samples were placed in a DIA-STRON limited "MTT690 Automatic Fiber Tensile Testing Machine". After being left immersed in water for 30 minutes, automatic measurement was started, and the breaking load when the fiber was stretched while immersed in water was determined. A higher value indicates greater stiffness and resilience, greater resistance to stretching by external forces, and superior durability. According to the following formula, the average breaking load (W0(gf)) when the fibers were tensed in their untreated state (untreated; Comparative Example 1) was used as the baseline. The table shows the increase in the average breaking load (W1(gf)) of the treated fiber bundles from the untreated state, indicated as "Increase in average breaking load when fibers are tensed [gf]". Y(gf) = W1(gf) - W0(gf)

[0193] <Shrinkage rate when using a high-temperature iron> As an indicator of heat resistance, the shrinkage rate during high-temperature ironing was used. The evaluation was performed using hair bundles immediately after treatment using the above-described <treatment method>. Furthermore, the average value obtained when evaluating multiple fibers (5 strands) was used as the numerical value. The evaluation was performed according to the following procedure. 1. Immediately after the above processing method, five fibers were cut from the base of the hair bundle and marked. The length of these five processed fibers was measured and the average value was recorded (let's call it length L1). Next, these five marked processed fibers were bundled together with two separate bundles of unprocessed regenerated collagen fibers (totaling 1g), sandwiching them between them to create a new hair bundle (hereinafter referred to as the large hair bundle). A flat iron (manufactured by Miki Electric Industry Co., Ltd. / model number: AHI-938) set to 180°C was applied to the entire large hair bundle three times at a speed of 5cm / sec. 2. After the ironing process, five marked treated fibers were taken from the large bundle of hair, and the length of each of these five marked treated fibers was measured again and the average value was recorded (denoted as length L2). 3. Shrinkage rate when ironing at high temperature: S dry We defined it as = { 1 - (L2 / L1)} x 100 [%]. dry The closer the value is to 0%, the less likely it is to shrink due to dry heat, indicating superior heat resistance.

[0194] <Shrinkage rate when heated with hot water> As an indicator of water resistance and heat resistance, the shrinkage rate during hot water heating was used. The evaluation was performed using hair bundles immediately after treatment using the above-described <treatment method>. Furthermore, the average value obtained when evaluating multiple fibers (5 strands) was used as the numerical value. The evaluation was performed according to the following procedure. 1. Five fibers were cut from the base of the hair bundle, the average length of each fiber was recorded (referred to as length L1), and then the bundle was immersed in a 90°C water bath (manufacturer: Toyo Seisakusho Co., Ltd. / model number: TBS221FA) and heated for 1 minute. 2. After the heating process, five fibers were removed, lightly dried with a towel, and dried at room temperature and humidity for 30 minutes. The average length of each fiber was then recorded (denoted as length L2). 3. The shrinkage rate during hot water heating was defined as Swet = { 1 - (L2 / L1)} x 100 [%]. The closer Swet is to 0%, the less shrinkage due to moist heat occurs, indicating superior heat resistance.

[0195] <Thermal shape memory ability> The evaluation of the thermo shape memory ability was performed using the hair bundle immediately after being processed by the above <processing method>. In addition, when the value of the result of "I: Shape imparting (curl)" was 5% or less, subsequent processing and evaluation were not performed, considering it as having no effect. ·I: Shape imparting (curl) 1. After wetting a 22-cm-long hair bundle of 0.5 g of regenerated collagen fiber with tap water at 30°C for 30 seconds, the wet hair bundle was wrapped around a plastic rod with a diameter of 14 mm and fixed with a clip. 2. The hair bundle wrapped around the rod was immersed in a water bath at 60°C (manufacturer: Toyo Seisakusho Co., Ltd. / model number: TBS221FA) and heated for 1 minute. 3. The hair bundle was taken out of the water bath, immersed in water at 25°C for 1 minute, taken out of the water, and returned to room temperature. 4. The hair bundle was removed from the rod, passed through a comb 3 times, and after being taken out of the water, 3 minutes later, a photo was taken horizontally in the suspended state.

[0196] (Evaluation criteria) Taking the length of the untreated hair bundle as L0 (22 cm) and the length of the hair bundle after treatment as L, the curl-up rate = the reduction rate of the hair bundle length (I) (%) obtained according to the following formula was defined as the curling strength. I = [(L0 - L) / L0] × 100

[0197] ·II: Re-shape imparting (straight) 1. For the hair bundle evaluated in I, after removing tangles by passing through a comb, it was slid 6 times at a speed of 5 cm / sec with a flat iron set at 180°C (manufactured by Miki Electric Industry Co., Ltd. / model number: AHI-938). 2. It was rinsed with running tap water at 30°C for 30 seconds, foamed for 60 seconds with an evaluation shampoo, then rinsed with running tap water at 30°C for 30 seconds, and towel-dried. 3. It was suspended and naturally dried at 20°C and 65% RH for 12 hours, passed through a comb, and then visually observed horizontally in the suspended state.

[0198] (Evaluation criteria) The straightening rate (ST) (%), calculated according to the following formula, is defined as the degree of straightening achieved, with the untreated hair bundle length being L0 (22 cm) and the treated hair bundle length being L. When ST = 100%, the hair bundle is completely straightened. ST = [1 - (L0 - L) / L0] × 100

[0199] • III: Reshaping (curling) 1.II The hair bundles evaluated were wet with 30°C tap water for 30 seconds, then the wet hair bundles were wrapped around a 14mm diameter plastic rod and secured with a clip. 2. The hair bundles wrapped around the rod were immersed in a 60°C water bath (manufacturer: Toyo Seisakusho Co., Ltd. / model number: TBS221FA) and heated for 1 minute. 3. Remove the hair bundles from the water bath, immerse them in 25°C water for 1 minute, remove them from the water, and allow them to return to room temperature. 4. Remove the hair bundle from the rod, comb it through three times, and then, three minutes after taking it out of the water, take a picture of it hanging from the side.

[0200] (Evaluation Criteria) Let L0 be the length of the untreated hair bundle (22 cm) and L be the length of the treated hair bundle. The curl-up rate = hair bundle length reduction rate (I) (%), calculated according to the following formula, was defined as the curl strength. I = [(L0 - L) / L0] × 100

[0201] <Good surface texture> The surface texture was evaluated using hair strands immediately after treatment using the <treatment method>. Five expert panelists evaluated the smoothness of the texture when touched by hand according to the following criteria, and the sum of the five evaluations was used as the final result. (Evaluation Criteria) 5: It has an extremely smooth texture compared to untreated fibers (Comparative Example 1). 4: It has a smoother feel compared to untreated fibers (Comparative Example 1). 3: It has a slightly smoother texture compared to the untreated fibers (Comparative Example 1). 2: The texture is the same as the untreated fiber (Comparative Example 1). 1: It is rougher and has a less pleasant feel than untreated fibers (Comparative Example 1).

[0202] <Suppression of discoloration of fibers> 1. For both the front and back of each hair strand, the color was measured near the root, mid-length, and tip using a colorimeter (Konica Minolta CR-400), and the average of the six points was used as the color value (L, a, b). 2. The degree of coloring was evaluated using ΔE*ab, with untreated hair strands of color no. 30 white (*) (Comparative Example 1) as the baseline. Color measurements were taken on the same day the treatment was performed. (*) Untreated hair bundles of color number 30 white We purchased Kaneka Corporation's regenerated collagen fibers in the form of commercially available hair extension products, cut the fibers from them, and divided them into small bundles for evaluation. For this evaluation, we used extension products that were labeled as using 100% Ultima fiber, with a color count of 30 (white) and a straight shape. ΔE*ab is calculated by taking the measurements of an untreated hair bundle with color number 30 white as (L0, a0, b0) and the measurements of a treated hair bundle as (L1, a1, b1), where (L1-L0) 2 +(a1-a0) 2 +(b1-b0) 2 ] 1 / 2 The color-inhibiting effect was determined according to the following criteria, as defined by [the formula]. 5:ΔE*ab ≤ 5.0 4:5.0 < ΔE*ab ≤ 10.0 3:10.0 < ΔE*ab ≤ 15.0 2:15.0 < ΔE*ab ≤ 20.0 1:20.0< ΔE*ab

[0203] [Table 1]

[0204] [Table 2]

Claims

1. A fiber treatment agent comprising the following components (A) and (B): (A): The hydrogen bond term δH of the Hansen solubility parameter is 18.3MPa 1 / 2 A compound having at least one carboxy group or a salt thereof and no condensed ring, which is (B):Water

2. 2. The fiber treatment agent according to claim 1, wherein the component (A) is one or more compounds selected from the group consisting of the following components (A1) and (A2): (A1) The hydrogen bond term δH of the Hansen solubility parameter is 18.3MPa. 1 / 2 An aromatic compound having at least one carboxy group or a salt thereof and no condensed ring, which is (A2) The hydrogen bond term δH of the Hansen solubility parameter is 11.0MPa. 1 / 2 More than 18.3MPa 1 / 2 A compound (excluding aromatic compounds) having at least one carboxy group or a salt thereof and no condensed ring, which is

3. 3. The fiber treatment agent according to claim 2, wherein the component (A1) is a compound represented by the following general formula (1) or general formula (2) or a salt thereof: 【Chemistry 1】 [wherein =X represents a methylidene group or an oxo group, R 1 represents a hydrogen atom, a hydroxyl group, or an alkyl group, an aryl group, an alkoxy group, an aryloxy group, or an aralkyloxy group which may have a substituent; R 2 represents an o-phenylene group, an m-phenylene group, a p-phenylene group, a benzylidene group, or an alkylene group which may have a substituent. 2 When R does not have an aryl group, 1 is an aryl group, an aryloxy group, or an aralkyloxy group. 【Chemistry 2】 [In the formula, A 1 ~A 5 each independently represents a hydrogen atom, an acetyl group, a halogen atom, or a linear or branched alkyl group, alkenyl group, alkoxy group, or alkenyloxy group having 1 to 6 carbon atoms.

4. The fiber treatment agent according to any one of claims 1 to 3, wherein component (A) comprises benzoic acid or a salt thereof.

5. 5. The fiber treatment agent according to claim 4, wherein the pH of the fiber treatment agent is 2.0 or more and less than 6.5, and the content of benzoic acid or a salt thereof in the fiber treatment agent is 0.8% by mass or more and 40% by mass or less in terms of benzoic acid (acid type).

6. 5. The fiber treatment agent according to claim 4, wherein the pH of the fiber treatment agent is 2.0 or more and less than 6.5, and the content of benzoic acid or a salt thereof in the fiber treatment agent is 5.0% by mass or more and 40% by mass or less in terms of benzoic acid (acid type).

7. 5. The fiber treatment agent according to claim 4, wherein the pH of the fiber treatment agent is 6.5 or more and 11.0 or less, and the content of benzoic acid or a salt thereof in the fiber treatment agent is 0.8% by mass or more and 40% by mass or less in terms of benzoic acid (acid type).

8. 5. The fiber treatment agent according to claim 4, wherein the pH of the fiber treatment agent is 6.5 or more and 11.0 or less, and the content of benzoic acid or a salt thereof in the fiber treatment agent is 5.0 mass % or more and 40 mass % or less as benzoic acid (acid type).

9. The fiber treatment agent according to any one of claims 1 to 3, comprising two or more compounds as component (A).

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