Hair cosmetic

JP2024152574A5Pending Publication Date: 2026-04-21PHARMA FOODS INT CO LTD
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Patent Information

Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
PHARMA FOODS INT CO LTD
Filing Date
2023-11-22
Publication Date
2026-04-21

AI Technical Summary

Technical Problem

Eggshell membranes are insoluble in most solvents, including water, making it difficult to form them into a fibrous form for use in hair cosmetics, and their cosmetic effects are not fully realized when used alone or with conventional synthetic resin fibers.

Method used

Incorporating hydrolyzed eggshell membranes into fibers such as cellulose, acetate, hemp, cotton, silk, wool, nylon, polypropylene, polyester, and polylactic acid, specifically using viscose rayon, to enhance the cosmetic properties of hair cosmetics.

Benefits of technology

The hair cosmetic with eggshell membrane fibers exhibits improved flexibility, adherence to hair, and maintains deformation, providing better application and cosmetic benefits compared to conventional products.

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Abstract

To provide a hair cosmetic that easily adheres to hair.SOLUTION: This application provides a hair cosmetic containing fibers containing eggshell membranes. Such a cosmetic can be obtained by a method for producing fibers containing eggshell membranes, the method comprising the steps of: obtaining a solution containing the eggshell membranes; mixing the solution containing the eggshell membranes with dope containing raw fibers so as to obtain eggshell membrane-containing dope; and producing fibers containing the eggshell membranes from the eggshell membrane-containing dope.SELECTED DRAWING: None
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Description

[Technical field]

[0001] The present invention relates to a hair cosmetic composition, and in particular to one comprising fibers containing eggshell membrane. [Background technology]

[0002] Eggshell membrane is a thin membrane found inside the eggshell, and it has long been known that it is effective as a cosmetic or wound dressing, taking advantage of its properties, such as the cell production activity of its amino acids, its adhesion to tissues due to its mesh structure, and its moderate moisture retention and breathability. However, eggshell membrane is insoluble in most solvents, including water, and it is difficult to mold it into a fibrous form. Therefore, eggshell membrane is hydrolyzed to solubilize it, and used as a water-soluble eggshell membrane component. Summary of the Invention [Means for solving the problem]

[0003] The present inventors have found that by blending eggshell membrane, which is discarded and incinerated in quantities of tens of thousands of tons per year, into fibers and using the resulting mixture as a material for hair cosmetics, it is possible to obtain cosmetic effects that are superior to those obtained using fibers alone or conventional synthetic resin fibers. Therefore, the present invention provides a hair cosmetic comprising fibers containing eggshell membrane.

[0004] Therefore, according to a main aspect of the present invention, the following invention is provided. (Item 1) A hair cosmetic comprising fibers containing eggshell membrane. (Item 2) The hair cosmetic preparation according to the above items, wherein the eggshell membrane comprises an eggshell membrane hydrolysate. (Item 3) The hair cosmetic composition according to any one of the preceding items, wherein the fibers comprise one or more types of fibers selected from cellulose, acetate, hemp, cotton, silk, wool, nylon, polypropylene, polyester, and polylactic acid. (Item 4) 3. The hair cosmetic composition according to any one of the preceding claims, wherein the cellulose comprises viscose rayon. (Item 5) The hair cosmetic composition according to any one of the preceding items, wherein the fiber contains about 0.5 parts by mass or more and about 25 parts by mass or less of the eggshell membrane per 100 parts by mass of raw fiber. (Item 6) The hair cosmetic composition according to any one of the preceding items, wherein the fiber has a zeta potential of 0 mV or more. (Item 7) The hair cosmetic composition according to any one of the preceding items, characterized in that the flexibility of the fiber is greater than that of a similar fiber that does not contain the eggshell membrane. (Item 8) The fiber containing eggshell membrane is Obtaining a solution containing the eggshell membrane; A step of mixing a spinning dope containing raw fibers with the solution containing eggshell membrane to obtain an eggshell membrane-containing spinning dope; producing a fiber containing the eggshell membrane from the eggshell membrane-containing spinning dope; 2. The hair cosmetic composition according to any one of the preceding items, which is produced by a method comprising the steps of: (Item 9) The hair cosmetic composition according to any one of the above items, which is for eyelashes. (Item 10) The hair cosmetic composition according to any one of the preceding items, wherein the fibers have a fiber length of about 0.1 mm to about 5.0 mm. (Item 11) The hair cosmetic composition according to any one of the above items, wherein the fiber has a thickness of about 0.001 decitex to about 5.0 decitex. (Item 12) A method for producing fibers containing eggshell membrane for incorporation into a hair cosmetic, comprising the steps of: Obtaining a solution containing the eggshell membrane; A step of mixing a spinning dope containing raw fibers with the solution containing eggshell membrane to obtain an eggshell membrane-containing spinning dope; producing a fiber containing the eggshell membrane from the eggshell membrane-containing spinning dope; A method comprising: (Item 13) The method of any one of the preceding claims, wherein the eggshell membrane comprises an eggshell membrane hydrolysate. (Item 14) The method according to any one of the preceding items, wherein the fiber containing eggshell membrane contains about 0.5 parts by mass or more and about 25 parts by mass or less of the eggshell membrane per about 100 parts by mass of raw fiber. (Item 15) The method according to any one of the preceding items, wherein the zeta potential of the fiber containing eggshell membrane is 0 mV or more. (Item 16) The method according to any one of the preceding claims, characterized in that the flexibility of the fiber containing eggshell membrane is greater than that of the same fiber not containing eggshell membrane. (Item 17) Fibers containing eggshell membrane for incorporation in a hair cosmetic composition, produced by the method described in any one of the above items.

[0005] It is contemplated that one or more of the above features may be provided in combinations other than those specifically described herein.Further embodiments and advantages of the present disclosure will be recognized by those skilled in the art upon reading and understanding the following detailed description, if necessary.

[0006] Furthermore, features and notable actions and effects of the present disclosure other than those described above will become apparent to those skilled in the art by referring to the following description of the preferred embodiments of the present invention and the drawings. Effect of the Invention

[0007] The hair cosmetic composition of the present invention is more flexible than conventional hair cosmetic compositions in that it bends to conform to the shape of the hair, and is more easily attached to the hair due to its positive surface potential. In addition, since it has low bending recovery, it can maintain its deformed state when attached to the hair. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0008] The present disclosure will be described below while showing the best mode. Throughout this specification, the expression of the singular form should be understood to include the concept of the plural form, unless otherwise specified. Therefore, the singular article (for example, in the case of English, "a", "an", "the", etc.) should be understood to include the concept of the plural form, unless otherwise specified. In addition, it should be understood that the terms used in this specification are used in the sense commonly used in the field, unless otherwise specified. Therefore, unless otherwise defined, all technical terms and scientific and technical terms used in this specification have the same meaning as commonly understood by those skilled in the art to which this disclosure belongs. In case of conflict, the present specification (including definitions) will take precedence.

[0009] The following provides definitions of terms particularly used in this specification and / or explains basic technical content as appropriate.

[0010] As used herein, "about" means ±10% of the preceding numerical value.

[0011] As used herein, "hair cosmetics" refers to cosmetics used on human hair, such as hair, eyebrows, eyelashes, and artificial hair, and examples thereof include mascara, eyebrow products, hair mascara, and hair foundation.

[0012] (Preferred embodiment) Preferred embodiments of the present disclosure are described below. The embodiments provided below are provided for a better understanding of the present disclosure, and the scope of the present disclosure should not be limited to the following description. Therefore, it is clear that a person skilled in the art can make appropriate modifications within the scope of the present disclosure in light of the description in this specification. In addition, the following embodiments of the present disclosure can be used alone or in combination.

[0013] In one aspect of the present invention, a hair cosmetic composition is provided that includes fibers containing eggshell membrane. [Eggshell membrane] The origin of the eggshell membrane used as the material of the hair cosmetic of the present invention is not particularly limited. For example, the eggshell membrane may be that of poultry birds such as chicken, quail, turkey, duck, goose, ostrich, guinea fowl, cock-tailed geese, bantam, pigeon, mute swan, emu, or pheasant. In one embodiment of the present invention, chicken is preferred because it is easy to obtain, is a prolific egg-laying species, produces large eggs, and a mass-breeding method has been established.

[0014] Usually, eggshell membranes have eggshell attached, and if they are hydrolyzed as is, the eggshell will remain insoluble, causing clogging of the spinneret during wet spinning and resulting in damage to the spinneret, which is undesirable. To remove the eggshell, the eggshell membrane containing the eggshell may be immersed in an aqueous solution of hydrochloric acid, phosphoric acid, etc., to dissolve the eggshell in water, and then removed in advance by filtration and washing with water, or the eggshell membrane containing the eggshell may be hydrolyzed to make it soluble in a solvent, and then the eggshell that is insoluble in the solvent may be physically removed by filtration, centrifugation, etc.

[0015] [Eggshell membrane crushing] In one embodiment of the present invention, it is preferable to crush the eggshell membrane in advance in order to smoothly hydrolyze the eggshell membrane, and the size after crushing is not particularly limited as long as it is crushed to an extent that allows smooth hydrolysis. In one embodiment, the crushed eggshell membrane has a diameter of preferably about 0.1 μm or more and about 5 mm or less, and more preferably about 1 μm or more and about 1 mm or less. By making the eggshell membrane within this range, it is possible to uniformly hydrolyze the eggshell membrane when hydrolyzing it. It is difficult to produce the eggshell membrane with a diameter of less than about 0.1 μm, and the molecular weight of the hydrolyzed eggshell membrane component becomes too low, which is not preferable.

[0016] [Hydrolysis of eggshell membrane] The eggshell membrane of the present invention can be hydrolyzed and used for fiber production. Regarding the hydrolysis of eggshell membrane, it is known that solubilized eggshell membrane with a relatively large molecular weight can be obtained by hydrolyzing it at high temperature in the presence of an alkali (Patent No. 6288686). In this case, the decomposition reaction is stopped by neutralizing it with an acidic substance.

[0017] In addition, by applying a protease having an optimal pH in the alkaline region, an eggshell membrane hydrolysate with a high cystine content can be obtained (JP Patent Publication No. 2018-177713). In addition, the eggshell membrane can be dissolved in thiopropionic acid or the like and spun by electrospinning to provide a fiber assembly (JP Patent Publication No. 2009-89859, Patent No. 5166953). In another embodiment, the eggshell membrane can be hydrolyzed in the presence of a reducing agent to obtain a solubilized eggshell membrane, which can be processed into a fiber fabric (JP Patent Publication No. 4387806, Patent Publication No. 2004-84154).

[0018] In one embodiment of the present invention, the hydrolysis treatment of eggshell membrane can be carried out using an acid (hydrochloric acid, sulfuric acid, etc.), an alkali (sodium hydroxide, potassium hydroxide, etc.), a protease (enzyme of microbial origin, enzyme of plant origin, enzyme of animal origin), etc., but is preferably carried out using an alkali, and more preferably in an alkaline aqueous solution. The eggshell membrane hydrolysate used as a material for the hair cosmetic of the present invention may be a hydrolysate using sodium hydroxide, or an aqueous solution of an alkali metal such as lithium hydroxide or potassium hydroxide, or an alkaline earth metal such as calcium hydroxide, etc. can also be used. Since the peptide bond constituting a protein is an extremely stable bond, it can be decomposed non-enzymatically using an alkali by heating at a high pH and high temperature, or when a relatively weakly alkaline alkali is used, it can be treated at high temperature for a long period of time.

[0019] In other embodiments, the eggshell membrane can be hydrolyzed using proteolytic enzymes such as pepsin, trypsin, renin, papain, caspase, chymotrypsin, proteases, peptidases, and acids such as citric acid, hydrochloric acid, and sulfuric acid.

[0020] In one embodiment of the present invention, in the case of hydrolysis with an alkali such as sodium hydroxide, eggshell membrane is prepared as a raw material, and the alkali is added to the eggshell membrane and stirred. The stirring conditions may be any conditions that allow the raw material and the alkali to be sufficiently stirred, and the alkali to hydrolyze the peptide bonds in the raw material to appropriately obtain the hydrolyzed eggshell membrane according to the present invention.

[0021] In one embodiment, the alkali concentration when treating eggshell membranes with alkali is preferably about 0.1 to about 20%, more preferably about 0.5 to about 10%. If it is less than about 0.1%, a sufficient hydrolysate cannot be obtained, and if it is more than about 20%, the hydrolysis rate is too fast, making it difficult to control the degree of hydrolysis, which is not preferred.

[0022] In one embodiment of the present invention, the hydrolysis temperature is preferably about 10 to about 90° C., more preferably about 40 to about 80° C. If the temperature is less than about 10° C., the hydrolysis hardly proceeds, and if the temperature is more than about 90° C., it is difficult to control the degree of hydrolysis, and therefore it is not preferable.

[0023] In one embodiment, the reaction time when treating eggshell membranes with alkali can be appropriately changed depending on the reaction temperature, alkali concentration, target molecular weight, etc., and is not particularly limited as long as the eggshell membranes are appropriately hydrolyzed for that time. For example, in one embodiment, the reaction time can be about 30 minutes to about 6 hours, preferably about 1 hour to about 4 hours.

[0024] In one embodiment of the present invention, the solvent required for hydrolysis is preferably water, but water-soluble organic solvents such as methanol, ethanol, acetone, n-propanol, isopropanol, etc. may be used in combination. From the viewpoint of the working environment and wastewater treatment, hydrolysis in a water solvent is preferred.

[0025] [Stopping the hydrolysis process] The hydrolysis reaction in the present invention is preferably terminated when the weight average molecular weight (Mw) of the obtained hydrolysate is about 10,000 to about 100,000, preferably about 15,000 to about 80,000, and more preferably about 30,000 to about 60,000. The hydrolysis reaction can be achieved by any means known in the art. In a preferred embodiment, there are two methods for terminating the hydrolysis of eggshell membranes, either of which may be used.

[0026] (1) Eggshell membrane is hydrolyzed in the presence of alkali, and then carbon disulfide is added to stop the hydrolysis. After the hydrolysis reaction is completed, the mixture is cooled to about 30°C, and carbon disulfide is added to stop the hydrolysis in the presence of an alkali. After the hydrolysis is completed, the mixture can be cooled quickly to stop the hydrolysis, and a freezing agent such as ice can also be added to the system.

[0027] To completely stop hydrolysis even in the presence of alkali, it is effective to react eggshell membrane with about 0.2 to about 50% of carbon disulfide based on the weight of the charged eggshell membrane to form a complex between amino groups (-NH-) and carbon disulfide (CS2), and more preferably about 1 to about 40%, and particularly preferably about 2 to about 30% of carbon disulfide. At less than about 0.2%, it is insufficient to stop alkaline hydrolysis, and at more than about 50%, excess carbon disulfide is separated and present, which poses a safety problem during production.

[0028] (2) Eggshell membrane is hydrolyzed in the presence of alkali and then neutralized with acid After the hydrolysis reaction, the mixture is cooled quickly to about 50°C, and about 0.5 to about 1.0 equivalents of the acid used in the alkaline hydrolysis are quickly added to stop the hydrolysis. The acid to be added may be either a strong acid or a weak acid, but a weak acid is preferable because strong acids such as hydrochloric acid and sulfuric acid cause the hydrolyzed eggshell membrane to precipitate at the stage of adding about 0.5 equivalents of the acid, and furthermore, a strong sulfur odor is generated and cystine and / or cysteine ​​are dropped off. In one embodiment, the weak acid can be an acid that shows an acid dissociation constant (pKa) of 0 or more in water, preferably about 0.2 or more, more preferably about 1.0 or more, more preferably about 1.5 or more, more preferably about 2.0 or more, and more preferably about 3.0 or more, with no particular upper limit. For example, acetic acid has a pKa of 4.6, carbonic acid has a pKa of 6.4, oxalic acid has a pKa of 1.0, citric acid has a pKa of 3.1, and benzoic acid has a pKa of 4.0.

[0029] The organic carboxylic acid used in the present invention is not particularly limited, but is preferably a weak acid such as citric acid, since the hydrolyzed eggshell membrane does not precipitate as an insoluble matter when the amount is up to the equivalent neutralization amount. The amount of organic carboxylic acid used for neutralization is about 0.5 to about 1.0 equivalent of acid relative to the alkaline agent used, and about 0.6 to about 0.8 equivalent is more preferable. If it is less than about 0.5 equivalent, hydrolysis will proceed over time, and if it is more than about 1.0 equivalent, the hydrolyzed eggshell membrane component will precipitate, which is not preferable.

[0030] When neutralized with an organic carboxylic acid, there is no problem in proceeding to the next spinning step with a small amount of alkaline agent remaining, but it is preferable to treat with an alkaline adsorbent (such as Kyoward 700 manufactured by Kyowa Chemical Industry Co., Ltd.) and then remove the adsorbent by filtration. This is preferable because it results in the eggshell membrane hydrolysate being stable over time with almost no alkaline agent remaining.

[0031] In one embodiment, the organic carboxylic acid is not particularly limited as long as it can neutralize hydrolysis, but preferred examples include weak acids such as citric acid, acetic acid, carbonic acid, and oxalic acid. In particular, citric acid is preferred because it is used in applications such as fibers and cosmetics.

[0032] In one embodiment, either one of the above-mentioned terminating the hydrolysis with carbon disulfide or neutralizing the hydrolysis with an organic carboxylic acid such as citric acid may be carried out, or the two may be used in combination to terminate or neutralize the hydrolysis.

[0033] The molecular weight of the eggshell membrane hydrolysate obtained as described above is, in terms of weight average molecular weight (Mw) measured by GPC (gel permeation chromatography), about 10,000 to about 100,000, preferably about 15,000 to about 80,000, and more preferably about 30,000 to about 60,000.

[0034] If the molecular weight is less than about 10,000, the solubility in water increases when spun into rayon fiber, resulting in a low residual rate. On the other hand, if it exceeds about 100,000, the compatibility with viscose is poor, resulting in a low residual rate when spun, which is undesirable.

[0035] In one embodiment of the present invention, the molecular weight of the eggshell membrane hydrolysate of the present invention can be maintained at a value within about 30%, within about 20%, preferably within about 15%, more preferably within about 10%, and even more preferably within about 5% when allowed to stand at room temperature to about 40°C for at least about 3 days, at least about 5 days, or at least about 7 days.

[0036] [fiber] In one embodiment of the present invention, the fibers with which the eggshell membrane or eggshell membrane components are mixed are not particularly limited, and as long as the effects of the present invention are achieved, synthetic fibers, semi-synthetic fibers, man-made fibers, natural fibers, synthetic resin fibers, etc. can be used. The fibers with which the eggshell membrane or eggshell membrane components are mixed can include, for example, one or more types of fibers selected from cellulose, acetate, hemp, cotton, silk, wool, nylon, polypropylene, polyester, polylactic acid, etc., and preferably cellulose, and particularly preferably viscose rayon can be used.

[0037] In the present invention, an eggshell membrane component is kneaded into regenerated cellulose fibers using a manufacturing method that does not require special equipment and can be implemented using current manufacturing processes, and a hair cosmetic composition containing such fibers is provided.

[0038] In one embodiment, the hair cosmetic of the present invention comprises a fiber containing eggshell membrane, preferably a fiber containing an eggshell membrane hydrolysate. The fiber used in the hair cosmetic of the present invention may contain about 0.5 parts by mass or more and about 25 parts by mass or less of the eggshell membrane per 100 parts by mass of the raw fiber.

[0039] In one embodiment, in the hair cosmetic of the present invention, the fiber containing eggshell membrane can be obtained by a method including the steps of obtaining a solution containing eggshell membrane, mixing a spinning dope containing raw fiber with the solution containing eggshell membrane to obtain an eggshell membrane-containing spinning dope, and producing the fiber containing eggshell membrane from the eggshell membrane-containing spinning dope.

[0040] Therefore, in one aspect of the present invention, there is provided a method for producing fibers containing eggshell membrane for incorporation into hair cosmetics, the method comprising the steps of obtaining a solution containing the eggshell membrane, mixing a spinning dope containing raw fibers with the solution containing the eggshell membrane to obtain an eggshell membrane-containing spinning dope, and producing fibers containing the eggshell membrane from the eggshell membrane-containing spinning dope.

[0041] In yet another aspect of the present invention, there is provided a fiber containing eggshell membrane for incorporation into a hair cosmetic composition, produced by the method described elsewhere herein.

[0042] In one embodiment, the method for producing the fiber to be blended in the hair cosmetic of the present invention includes, for example, the cuprammonium method in which cellulose is solubilized by converting it into a cuprammonium complex to obtain a spinning solution, the viscose method in which cellulose is converted into alkali cellulose, and then reacted with carbon disulfide to obtain cellulose xanthate to obtain a solubilized spinning solution (viscose), and the solvent spinning method in which cellulose is dissolved in a special solvent to obtain a spinning solution, and the like. Among these, viscose rayon fiber obtained by the viscose method is particularly useful.

[0043] In one embodiment, a process for producing fibers containing eggshell membrane can include a step of hydrolyzing eggshell membrane in the presence of an alkali, a step of stopping the hydrolysis to obtain a solution containing an eggshell membrane hydrolysate, a step of mixing a spinning dope containing raw fibers with the solution containing the eggshell membrane hydrolysate to prepare an eggshell membrane-containing spinning dope, and a step of producing fibers containing the eggshell membrane from the eggshell membrane-containing spinning dope.

[0044] In one embodiment, eggshell membrane component-containing viscose rayon fiber produced by the viscose process can be obtained through the following steps. (1) A process in which eggshell membrane is hydrolyzed in the presence of an alkali and then carbon disulfide is added to stop the hydrolysis. (2) A step of hydrolyzing the eggshell membrane in the presence of an alkali and then terminating the hydrolysis by neutralizing the hydrolysis with an organic carboxylic acid. (3) A process for blending the eggshell membrane hydrolyzate obtained through the process (1) or (2) with a spinning solution of viscose and obtaining viscose rayon fiber by a wet spinning method. (4) A process for processing the viscose rayon fiber obtained through the process (3) into staple fibers.

[0045] In one embodiment of the present invention, the fiber used in the hair cosmetic of the present invention has functionality, and since eggshell membrane is a natural material, it is preferable that the material is a fiber derived from a natural product, and in particular, viscose rayon fiber, which is a regenerated cellulose fiber, is preferable. In one embodiment, the viscose rayon fiber is produced by the steps of converting wood or non-wood-derived natural cellulose into alkali cellulose, reacting it with carbon disulfide to obtain cellulose xanthate, obtaining viscose, which is a spinning stock solution made by dissolving the cellulose xanthate in an aqueous solution, and spinning the viscose to obtain regenerated cellulose fiber.

[0046] [Combination of eggshell membrane ingredients and viscose] In one embodiment of the present invention, eggshell membrane components can be blended with viscose. In one embodiment, the eggshell membrane hydrolyzate whose hydrolysis has been stopped with carbon disulfide can be blended with viscose, which is an aqueous solution of cellulose xanthate obtained by reacting alkali cellulose with carbon disulfide, at any ratio at room temperature. In another embodiment, the eggshell membrane hydrolyzate neutralized with an organic carboxylic acid can also be blended with viscose at any ratio at room temperature, and when mixed with viscose, the hydrolysis is stopped by the carbon disulfide present in the viscose, so that it can be stabilized even in the presence of an alkaline agent.

[0047] [Eggshell membrane component kneaded into spinning] In one embodiment, when the eggshell membrane component and viscose are blended, the viscose to which the hydrolyzed eggshell membrane component has been added can be spun under known conditions using a normal viscose rayon spinning facility. In one embodiment, the raw viscose may contain, for example, about 7% by mass to about 10% by mass of cellulose, about 5% by mass to about 8% by mass of sodium hydroxide, and about 2% by mass to about 3.5% by mass of carbon disulfide. In one embodiment, the temperature of the raw viscose is preferably maintained at about 18°C ​​to about 23°C.

[0048] In one embodiment, when eggshell membrane components are blended with viscose, the amount of eggshell membrane component added to viscose in the eggshell membrane hydrolysate is preferably from about 0.5% by mass to about 25% by mass of the eggshell membrane component relative to approximately 100% by mass of cellulose in the raw viscose, more preferably from about 1.0% by mass to about 20% by mass, and even more preferably from about 2.0% by mass to about 15% by mass.

[0049] By spinning the viscose containing eggshell membrane components prepared under the above-mentioned conditions, it is possible to obtain viscose rayon fibers containing eggshell membrane components in which the eggshell membrane components are effectively contained inside the fibers without compromising fiber strength.

[0050] In one embodiment, the eggshell membrane component-containing viscose rayon fiber of the present invention can be spun, for example, using a normal circular nozzle. As the spinning nozzle, it is preferable to use a circular nozzle having a diameter of 0.05 mm to 0.12 mm and a number of holes of 1000 to 20000, depending on the target production amount. Using the spinning nozzle, the viscose liquid for spinning is extruded into a spinning bath, spun, and coagulated and regenerated. The spinning speed is preferably in the range of 30 m / min to 80 m / min. The stretch ratio is preferably 39% to 55%. Here, the stretch ratio indicates how much the sliver speed after stretching is increased when the sliver speed before stretching is set to 100. In terms of magnification, it is 1 before stretching and 1.39 times to 1.55 times after stretching.

[0051] As the spinning bath (Muller bath), it is preferable to use a strong acid bath containing, for example, about 95 g / L to about 130 g / L of sulfuric acid, about 10 g / L to about 17 g / L of zinc sulfate, and about 290 g / L to about 370 g / L of sodium sulfate (mirabilite). A more preferable sulfuric acid concentration is about 95 g / L to about 120 g / L.

[0052] [Scouring of fiber containing eggshell membrane components] In one embodiment, the eggshell membrane component-containing fiber obtained as described above can be cut to a predetermined length and subjected to a conventional refining process. The refining process can be carried out in the usual order of hot water treatment, hydrosulfurization, bleaching, and pickling. Bleaching can be carried out under the same conditions as for normal fibers, and sodium hypochlorite or hydrogen peroxide may be used. In one embodiment, bleaching is preferably carried out with sodium hypochlorite (sodium hypochlorite).

[0053] In one embodiment, the fiber containing eggshell membrane components in the hair cosmetic of the present invention contains eggshell membrane components in an amount of about 0.5 parts by mass or more and about 25 parts by mass or less per 100 parts by mass of raw fiber. Preferably, the eggshell membrane component is contained in an amount of about 1.0 parts by mass or more and about 20 parts by mass or less, more preferably about 2.0 parts by mass or more and about 15 parts by mass or less. If the content of the eggshell membrane component is less than about 0.5 parts by mass, the properties of the eggshell membrane cannot be fully exhibited, and if it exceeds about 25 parts by mass, the fiber strength will decrease significantly.

[0054] In the fiber containing an eggshell membrane component in the hair cosmetic of the present invention, the molecular weight of the eggshell membrane hydrolyzate, as measured by GPC, is about 10,000 to about 100,000, preferably about 15,000 to 80,000, and more preferably about 30,000 to about 60,000. If the molecular weight is less than about 10,000, the solubility in water increases, resulting in a low residual rate when spun into fibers, whereas if the molecular weight exceeds about 100,000, spinnability tends to decrease, which is undesirable.

[0055] The fiber containing eggshell membrane components in the hair cosmetic of the present invention can have a zeta potential of 0 mV or more. Without being bound by theory, the surface of human hair is negatively charged due to dissociation of protein end groups, but by mixing eggshell membrane components with fibers such as rayon, the surface potential becomes positive, making it easier for the components to adhere to hair. Zeta potential is the potential formed by the charge generated on the fiber surface in a solution, and zeta potential varies greatly depending on the material that constitutes the fiber layer.

[0056] Examples of methods for measuring the zeta potential include electrophoretic light scattering, electrokinetic sonic amplitude (ESA) method in which an alternating electric field is applied to a dispersion liquid to measure a sound field, and colloid vibration current method. The zeta potential of the present invention is preferably measured by electrophoretic light scattering.

[0057] In the electrophoretic light scattering method, the particles (filler) are moved (electrophoresed) by applying an electric field to the particles, and the moving particles are irradiated with a laser to calculate the electrophoretic velocity from the change in frequency of the irradiated light and the scattered light, thereby calculating the zeta potential. Examples of various instruments known to those skilled in the art include the ELSZ series (ELSZneo, ELSZneoSE, ELSZ-2000ZS) of Otsuka Electronics Co., Ltd. and the ZetaPlus or ZetaPALS series of Brookhaven Instrument. When measuring a very small potential or when measuring in a non-polar medium or at a high salt concentration, the so-called phase analysis light scattering (PALS) technique can also be applied. In the present invention, the zeta potential of the fiber containing eggshell membrane is 0 mV or more, typically more than 0 mV (i.e., the zeta potential is positive), and specifically, it can be 0 mV to about 1.5 mV. Preferably, the zeta potential of the fiber containing eggshell membrane is about 0.05mv or more, about 0.06mv or more, about 0.07mv or more, about 0.08mv or more, about 0.09mv or more, or about 0.1mv or more, and more preferably about 0.5mV or more, about 0.6mV or more, about 0.7mV or more, about 0.8mV or more, about 0.9mV or more, or about 1.0mV or more. In the present invention, the zeta potential of the fiber containing eggshell membrane may be a value measured by electrophoretic light scattering. Typically, the zeta potential of the fiber of the present invention may be measured by an ELSZ series (such as ELSZ-2000ZS or ELSZneo) manufactured by Otsuka Electronics Co., Ltd., which can determine the zeta potential by electrophoretic light scattering by actually measuring the electroosmotic flow in a cell.

[0058] The eggshell membrane component-containing fiber in the hair cosmetic of the present invention is characterized by its higher flexibility than the same type of fiber that does not contain eggshell membrane. By blending eggshell membrane into the fiber, the flexibility is improved, and it becomes easier to bend flexibly to fit the shape of the hair.

[0059] The hair cosmetic of the present invention may also contain a plurality of types of eggshell membrane component-containing fibers with different lengths. In one embodiment, the fibers to be blended in the hair cosmetic of the present invention have, for example, a fiber length of about 0.1 mm to about 5.0 mm, preferably about 0.5 to about 4.0 mm, and more preferably about 1.0 to about 3.0 mm. In one embodiment, the fiber length of the fibers to be blended in the hair cosmetic of the present invention can be appropriately set according to the application, and can be, for example, about 0.1 mm, about 0.5 mm, about 1.0 mm, about 1.5 mm, about 2.0 mm, about 2.5 mm, about 3.0 mm, about 3.5 mm, about 4.0 mm, about 4.5 mm, about 5.0 mm, etc. If the fiber length exceeds about 5.0 mm, the fiber is too long, so there is a problem that it gets entangled with the brush and does not move, and if it is less than about 0.1 mm, the fiber length is short, so the connection between the fibers is weak. Depending on the application, the fibers may be used as long fiber bundles without being cut after scouring.

[0060] In one embodiment, the eggshell membrane component-containing fiber blended in the hair cosmetic of the present invention is not particularly limited by its fineness. For example, the fineness of the eggshell membrane component-containing fiber blended in the hair cosmetic of the present invention is about 0.001 to about 5.0 decitex (dtex), preferably about 0.005 to about 4.0 dtex, more preferably about 0.01 to about 3.0 dtex. In one embodiment, the fineness of the fiber blended in the hair cosmetic of the present invention can be appropriately set depending on the application, and can be, for example, about 0.001 dtex, about 0.005 dtex, about 0.01 dtex, about 0.05 dtex, about 0.1 dtex, about 0.5 dtex, about 1.0 dtex, about 1.2 dtex, about 1.5 dtex, about 1.7 dtex, about 2.0 dtex, about 3.0 dtex, about 4.0 dtex, about 5.0 dtex, etc. If the thickness (fineness) is less than about 0.001 decitex, the fibers are too thin and can get tangled in the brush and not move, while if it exceeds about 5.0 decitex, the fibers are too thick, making them heavy and making it difficult to achieve long eyelashes.

[0061] In one embodiment of the present invention, the eggshell membrane component-containing fiber incorporated in the hair cosmetic composition of the present invention is soft and has excellent adhesion to human hair because it contains eggshell membrane components derived from natural ingredients, and there are no restrictions on the shape or area of ​​the fiber aggregate.

[0062] In one embodiment of the present invention, the fiber containing eggshell membrane components incorporated in the hair cosmetic composition of the present invention can have almost the same properties as natural eggshell membranes, since the fiber or fiber assembly itself contains eggshell membrane components. Specifically, since the eggshell membrane components themselves contribute to fiber formation, the properties inherent to eggshell membranes are strongly exhibited, unlike when eggshell membrane components are simply made into a film or when eggshell membrane components are simply attached to the surface of synthetic or natural fibers.

[0063] In one embodiment of the present invention, the hair cosmetic composition of the present invention can be for eyelashes or for hair.

[0064] In this specification, "or" is used when "at least one or more" of the items listed in the sentence can be employed. The same applies to "alternative." In this specification, when "within the range of" two values ​​is specified, the range includes the two values ​​themselves. All references cited herein, including scientific literature, patents, patent applications, and the like, are hereby incorporated by reference in their entirety to the same extent as if each was specifically set forth.

[0065] The present disclosure has been described above by showing preferred embodiments for ease of understanding. The present disclosure will be described below based on examples, but the above description and the following examples are provided for illustrative purposes only and are not provided for the purpose of limiting the present disclosure. Therefore, the scope of the present disclosure is not limited to the embodiments or examples specifically described in this specification, but is limited only by the scope of the claims. EXAMPLES

[0066] In the following examples, the blend amounts are expressed in mass % unless otherwise specified. In the following examples, the eggshell membrane component-containing fiber blended in the mascara cosmetic was produced as follows.

[0067] <Preparation of eggshell membrane solution> Washed chicken eggshell membranes (500 g) were placed in a 5% aqueous solution of caustic soda (3,500 g) and hydrolyzed by stirring at 55-65°C for 3 hours. The mixture was then cooled to 30°C, and 120 g of carbon disulfide was added and reacted for 1 hour. The mixture was then filtered through a filter cloth to obtain an eggshell membrane hydrolyzate (4,000 g).

[0068] <Production of Viscose Rayon Fiber> [Preparation of spinning solution] The prepared hydrolyzed eggshell membrane liquid was added to the raw viscose so that the eggshell membrane component was 10 parts by mass per 100 parts by mass of cellulose, and the mixture was stirred and mixed.

[0069] The raw viscose used contained 8.5% by mass of cellulose, 5.7% by mass of sodium hydroxide, and 2.7% by mass of carbon disulfide. The temperature was kept at 20°C.

[0070] [Spinning conditions] The obtained spinning solution was spun by a two-bath tension spinning method at a spinning speed of 50 m / min and a draw ratio of 43% to obtain a fiber with a fineness of 1.7 dtex. The composition of the first bath (spinning bath) was a Mueller bath (50°C) containing 100 g / L of sulfuric acid, 15 g / L of zinc sulfate, and 350 g / L of sodium sulfate. In addition, a nozzle with 4,000 holes with a diameter of 0.06 mm was used as the spinneret for ejecting the spinning solution.

[0071] [Scouring and bleaching treatment] The viscose rayon yarn obtained above was cut to a fiber length of 38 mm and subjected to a refining process. The refining process consisted of a hot water treatment followed by water rinsing, followed by hydrosulfurization, bleaching (sodium hypochlorite), and pickling, in that order. After applying an oil agent, excess water and oil agent were removed using a compression roller, and then a drying process (60°C, 7 hours) was performed to obtain rayon fiber.

[0072] (Example 1: Production of mascara containing eggshell membrane component-containing fiber) A mascara cosmetic was prepared having the composition shown in the following Table 1. In the table, "eggshell membrane hybrid rayon" refers to the rayon produced as described above. [Table 1]

[0073] The raw materials for phase A were heated and dissolved at 80-85°C, and the raw materials for phase B were heated and dissolved at 80-85°C. Phase C was added to the dissolved B layer and mixed with stirring, and then phase A was added to this mixture and emulsified using a homomixer. After cooling, phase D was added at 40°C and mixed with stirring, and then cooled further to 30°C, and layer E was added and dispersed uniformly.

[0074] (Example 2: Surface potential of fiber containing eggshell membrane component (zeta potential measurement)) The zeta potential of the surface of the fiber sample containing eggshell membrane components was measured by electrophoretic light scattering. The measurement device used was a zeta potential measurement system (Otsuka Electronics Co., Ltd., ELSZ-2000ZS). The zeta potential of the fiber substrate surface was measured using a cell unit for flat plate samples. The tracer particles used were flat plate monitor particles with model number "EL-9001" diluted 300 times with ion-exchanged water. The solvent conditions were a refractive index of 1.3328, a viscosity of 0.8878 cP, a dielectric constant of 78.3, and a measurement temperature of 25°C. The samples were measured in a state where they were closely attached to the sample mounting surface of the flat plate measurement cell by attaching double-sided tape to the sample mounting surface, laying them side by side without overlapping or gaps.

[0075] The results are shown in the table below. In the table, "eggshell membrane rayon" refers to fiber (rayon) containing the eggshell membrane hydrolysate of the present invention, and "soaked rayon" refers to rayon that was soaked for 2 hours in the treatment liquid (10% aqueous solution of eggshell membrane hydrolysate) used in the production of fiber containing the eggshell membrane hydrolysate of the present invention, and then lightly washed with water. [Table 2]

[0076] The surface of human hair is negatively charged due to dissociation of the protein end groups. As described above, it is found that the surface potential of the fiber containing the eggshell membrane hydrolysate of the present invention is changed to a positive one, which makes it easier for the fiber to adhere to hair. In addition, since the surface potential of the soaked rayon is not changed to a positive one, the surface potential does not change to a positive one simply by immersing the fiber in the treatment solution, and the surface potential can be made positive only by using the fiber mixed with the eggshell membrane hydrolysate.

[0077] (Example 3: Flexibility test) The flexibility (the property of an object being flexible and able to be bent) of the fiber samples containing eggshell membrane components was measured using a Handle-O-Meter (Model No. 226, manufactured by Yasuda Seiki Seisakusho).

[0078] A 200 mm wide test piece was prepared and set on a 10 mm wide slit at a right angle to the slit, and a blade was used to lower the test piece 67 mm from the side (1 / 3 of the test piece width) by 8 mm over 15 seconds with a load (full scale) of 981 mN, and the resistance value at this time was evaluated as bending resistance, with an average value of N=3. The smaller the measured value, the better the flexibility.

[0079] The results are shown in the table below. [Table 3]

[0080] It was found that by blending eggshell membrane hydrolysate with rayon, flexibility was improved, making it easier for the material to flex flexibly to conform to the shape of the hair.

[0081] (Example 4: Bending recovery test) The bending recovery (bending hysteresis) of the fiber samples containing eggshell membrane components was measured using a pure bending tester (model KES-FB2-A, manufactured by Kato Tech Co., Ltd.) with the maximum curvature control method.

[0082] The sample was 200 mm long and 200 mm wide. The sample was held in a chuck spaced 1 cm apart and was then rotated 0.50 cm -1 , B is curvature 0.5~1.5cm -1 , 2HB is 1cm -1 A pure bending test was performed within the range of 2HB to determine the hysteresis (2HB). The larger the measured value, the worse the recovery from deformation (the more the deformed state is maintained) (measurement temperature 20°C, humidity 65%).

[0083] The results are shown in the table below. [Table 4]

[0084] It was found that the ability to maintain the deformation state was improved by blending eggshell membrane hydrolysate with rayon.

[0085] Example 5: Sensory Evaluation The mascara cosmetic prepared in Example 1 was evaluated according to the following criteria. The prepared mascara cosmetic was used by five test subjects, who were then rated in the following categories: (1) Resistant to clumping, (2) Clean application to the tips, (3) Feels like one with the eyelashes, (4) Appearance that the length has increased, and (5) Overall evaluation (beauty of the finish). Each was rated on a five-point scale, with higher numbers indicating higher evaluations. The results below show the average of the five test subjects. [Table 5]

[0086] The prepared mascara cosmetic was applied to false eyelashes, and the appearance was blindly evaluated by 10 monitors, with the results shown in the table below. [Table 6]

[0087] As shown in the table above, the mascara containing the fiber containing the eggshell membrane hydrolyzate of the present invention was evaluated as being less likely to clump, adhering neatly to the tips, having a sense of unity with the eyelashes, and making them appear longer than conventional mascaras. The overall evaluation (beauty of the finish) was also higher than that of conventional mascaras.

[0088] (Note) Although the present disclosure has been illustrated using the preferred embodiments thereof, it is understood that the present disclosure should be interpreted in scope only by the claims. It is understood that the patents, patent applications, and other documents cited in this specification are incorporated by reference into this specification in the same manner as if the contents themselves were specifically set forth herein. [Industrial Applicability]

[0089] The hair cosmetic composition of the present invention contains an eggshell membrane component, which allows it to adhere to hair more easily than conventional hair cosmetic compositions, making it applicable in the field of cosmetics.

Claims

[Claim 1] The invention described herein.