WO2021250742A1

WO2021250742A1 - Cosmetic for eyelashes

Info

Publication number: WO2021250742A1
Application number: PCT/JP2020/022536
Authority: WO
Inventors: 正也野原; 三佳誉岩田; 博章田口; 浩伸蓑輪; 武志小松
Original assignee: 日本電信電話株式会社
Priority date: 2020-06-08
Filing date: 2020-06-08
Publication date: 2021-12-16
Also published as: JPWO2021250742A1; JP7368782B2

Abstract

This cosmetic for eyelashes comprises, as a pigment, a co-continuous fibrous carbon having a three-dimensional network structure in which a carbon is branched off, wherein the co-continuous fibrous carbon is made of cellulose nanofibers.

Description

Eyelash cosmetics

The present invention relates to cosmetics for eyelashes.

Conventionally, eyelash cosmetics have cosmetic effects such as curling the eyelashes upward (curl keeping), making the eyelashes look longer (long rush), and making the eyelashes thicker (volume up) to make the eyes clearer. It has. Eyelash cosmetics contain various components in order to impart adhesiveness and volume, and to adjust the drying speed (see Patent Documents 1 and 2).

Japanese Unexamined Patent Publication No. 2008-37815 Japanese Unexamined Patent Publication No. 2008-44860

In eyelash cosmetics, carbon black, black iron oxide, etc. are used as black pigments in order to have the function of developing a black color. In recent years, keywords such as natural, clean, and sustainable have been attracting attention, and there is a tendency for cosmetics composed only of raw materials with a low environmental load to be preferred. Therefore, eyelash cosmetics containing carbon black synthesized from petroleum may be avoided.

Black iron oxide produced from minerals is said to be a natural material, but because black iron oxide has a large particle size and poor dispersibility, a large amount of black iron oxide is used as a cosmetic for eyelashes in order to develop color. Need to be added to. Therefore, the amount of ingredients other than pigments for obtaining curl-keeping effect, long rush effect, volume-up effect, smooth usability (applying comfort), and adhesiveness (makeup retention) is reduced, and these effects can be obtained. There is a problem that it is difficult.

The present invention has been made in view of the above problems, and an object of the present invention is to provide a cosmetic for eyelashes using a material having a low environmental load and high dispersibility as a pigment.

One aspect of the present invention is a cosmetic for eyelashes, which comprises co-continuous fibrous carbon having a three-dimensional network structure in which carbon is branched as a pigment, and the co-continuous fibrous carbon is produced from cellulose nanofibers. ..

One aspect of the present invention is a cosmetic for eyebrows, which comprises rod-shaped carbon obtained by crushing co-continuous fibrous carbon having a three-dimensional network structure in which carbon is branched, and the co-continuous fibrous carbon is cellulose. Made from nanofibers.

According to the present invention, it is possible to provide a cosmetic for eyelashes using a material having a low environmental load and high dispersibility as a pigment.

It is a flowchart which shows the manufacturing method of the co-continuous fibrous carbon of 1st Embodiment. 3 is an SEM image of the co-continuous fibrous carbon of the first embodiment. It is a flowchart which shows the manufacturing method of the eyelash cosmetics of 1st Embodiment. It is a figure which shows the experimental example and evaluation of the underwater oil type eyelash cosmetics of 1st Embodiment. It is a figure which shows the experimental example and evaluation of the oil-based eyelash cosmetics of 1st Embodiment. It is a figure which shows the experimental example and evaluation of the water-in-oil type eyelash cosmetics of 1st Embodiment. It is a flowchart which shows the manufacturing method of the rod-shaped carbon of 2nd Embodiment. It is an SEM image of the rod-shaped carbon of the second embodiment. It is a flowchart which shows the manufacturing method of the eyelash cosmetics of 2nd Embodiment. It is a figure which shows the experimental example and evaluation of the underwater oil type eyelash cosmetics of 2nd Embodiment. It is a figure which shows the experimental example and evaluation of the oil-based eyelash cosmetics of 2nd Embodiment. It is a figure which shows the experimental example and evaluation of the water-in-oil type eyelash cosmetics of 2nd Embodiment.

Hereinafter, embodiments of the present invention will be described with reference to the drawings.

<First Embodiment>
[Manufacturing method of co-continuous fibrous carbon]
FIG. 1 is a flowchart showing a method for producing co-continuous fibrous carbon according to the first embodiment. The co-continuous fibrous carbon is used as a pigment for the eyelash cosmetics (mascara) of the present embodiment.

The illustrated method for producing co-continuous fibrous carbon includes a dispersion step (step S1), a freezing step (step S2), a drying step (step S3), and a carbonization step (step S4). This production method requires a cellulose nanofiber dispersion.

If it is a cellulose nanofiber, the raw material is not particularly limited. Cellulose nanofibers include, for example, wood-derived, pulp-derived, crustacean-derived, bacterial-derived, food-derived, plant-derived, and other biological-derived. In this embodiment, any one of these cellulose nanofibers may be used, or two or more kinds of these may be selected and mixed with the cellulose nanofibers. In this embodiment, such a material having a low environmental load is used as a pigment.

The form of the cellulose nanofibers in the cellulose nanofiber dispersion liquid is preferably a dispersed form. Therefore, the manufacturing process shown in FIG. 1 includes a dispersion step (step S1), but the dispersion step (step S1) may not be included. That is, when the cellulose nanofiber dispersion liquid in which the cellulose nanofibers are dispersed is used, the step is not necessary.

The dispersion step disperses the cellulose nanofibers contained in the cellulose nanofiber dispersion liquid. The dispersion medium may be an aqueous system such as water (HO), carboxylic acid, methanol (CH ₃ OH), ethanol (C ₂ H ₅ OH), propanol (C ₃ H ₇ OH), n-butanol, isobutanol, n. -At least one selected from the group consisting of organic systems such as butylamine, dodecane, unsaturated fatty acids, ethylene glycol, heptan, hexadecane, isoamyl alcohol, octanol, isopropanol, acetone and glycerin can be used.

For the dispersion of the cellulose nanofibers, for example, a homogenizer, an ultrasonic cleaner, an ultrasonic homogenizer, a magnetic stirrer, a stirrer, a shaker, or the like may be used.

Further, the solid content concentration of the cellulose nanofibers in the cellulose nanofiber dispersion liquid is preferably 0.001 to 80% by mass, more preferably 0.01 to 30% by mass. This is because if the solid content concentration is too low, a network of cellulose nanofibers cannot be formed, and it becomes difficult to form a co-continuous structure of carbon in the carbonization step (step S4) described later. Further, if the solid content concentration is too high, it aggregates in the freezing step (step S2) described later, and further, in the carbonization step (step S4), the sintering of cellulose proceeds to form a fibrous structure. This is because it becomes difficult.

In the freezing step, a dispersion containing cellulose nanofibers is frozen to obtain a frozen product (step S2). In this step, for example, the cellulose nanofiber dispersion liquid is housed in a suitable container such as a test tube, and the surroundings of the test tube are cooled in a cooling material such as liquid nitrogen, so that the cellulose nanofibers housed in the test tube are stored. Is done by freezing.

The method of freezing is not particularly limited as long as the dispersion medium of the dispersion liquid can be cooled below the freezing point, and may be cooled in a freezer or the like. By freezing the cellulose nanofiber dispersion liquid, the dispersion medium loses its fluidity, the cellulose nanofibers which are the dispersoids are fixed, and a three-dimensional network structure is constructed.

In the drying step, the frozen body frozen in the freezing step is dried in a vacuum to obtain a dried body (step S3). This step sublimates the frozen dispersion medium from the solid state. For example, the obtained frozen product is placed in a suitable container such as a flask, and the inside of the container is evacuated. By arranging the frozen body in a vacuum atmosphere, the sublimation point of the dispersion medium is lowered, and it is possible to sublimate even a substance that does not sublimate under normal pressure.

The degree of vacuum in the drying step varies depending on the dispersion medium used, but is not particularly limited as long as the degree of vacuum is such that the dispersion medium sublimates. For example, when water is used as the dispersion medium, it is necessary to set the pressure to a vacuum degree of 0.06 MPa or less, but it takes time to dry because heat is taken away as latent heat of sublimation. Therefore, the degree of vacuum is preferably 1.0 × 10 ^-6 Pa to 1.0 × 10 ^-2 Pa. Further, heat may be applied using a heater or the like at the time of drying.

In the carbonization step, the dried body dried in the drying step is heated and carbonized in an atmosphere that does not burn to obtain co-continuous fibrous carbon (step S4). The cellulose nanofibers may be carbonized by firing at 100 ° C. to 2000 ° C., preferably 150 ° C. to 1300 ° C. in an inert gas atmosphere.

In addition, it is possible to change the color of co-continuous fibrous carbon by adjusting the progress of carbonization, and it turns brown at 150 ° C to 400 ° C and black at temperatures higher than 400 ° C. That is, the co-continuous fibrous carbon has a color according to the progress of carbonization. The degree of carbonization is adjusted by the firing temperature, firing time, and the like. Specifically, in the case of co-continuous fibrous carbon obtained by calcining the dried product at 150 ° C. to 400 ° C., brown eyelash cosmetics are applied to the eyelashes. Further, in the case of co-continuous fibrous carbon obtained by calcining the dried product at a temperature higher than 400 ° C., black eyelash cosmetics are applied to the eyelashes. Depending on the temperature, for example, even if it is brown, the lightness or saturation can be adjusted from light brown to dark brown. In the present embodiment, by using the co-continuous fibrous carbon, the progress of carbonization of the co-continuous fibrous carbon is adjusted without preparing pigments of a plurality of colors, respectively, so that various shades of brown or black can be used. It is possible to realize a cosmetic for eyebrows.

The gas that does not burn cellulose may be, for example, an inert gas such as nitrogen gas or argon gas. Further, the gas on which cellulose does not burn may be a reducing gas such as hydrogen gas or carbon monoxide gas, or may be carbon dioxide gas. Nitrogen gas is more preferable from the viewpoint of cost.

By the manufacturing method described above, co-continuous fibrous carbon having a three-dimensional network structure is obtained.

FIG. 2 is an SEM (Scanning Electron Microscope) image of co-continuous fibrous carbon produced by the manufacturing method of the present embodiment. The magnification is 10000 times. From the image, it can be seen that the three-dimensional network structure is being constructed.

As described above, the co-continuous fibrous carbon of the present embodiment is a naturally derived raw material unlike carbon black, carbon nanotubes, fullerenes, graphene, and graphite synthesized from fossil fuels, and has a low burden on the environment. ..

Further, in the present embodiment, fibrous carbon is branched and has a co-continuous three-dimensional network structure. Therefore, even when this co-continuous fibrous carbon is added to eyelash cosmetics as a black pigment, the branched structure suppresses the formation of bundles (aggregates) of fibers, and the fibrous carbon is made uniform. It becomes possible to disperse to.

If the fiber diameter of the co-continuous fibrous carbon is too small, the branched structure is fragile and aggregates during storage of the eyelash cosmetics. Further, if the fiber diameter is too large, the dispersibility is lowered when the eyelash cosmetic is used, and sufficient color development performance cannot be obtained. Therefore, the fiber diameter is preferably 10 nm to 200 nm.

Similarly, if the fiber length of the co-continuous fibrous carbon is too short, it will aggregate during storage of the eyelash cosmetics. On the other hand, if it is too long, the dispersibility is lowered and sufficient color development performance cannot be obtained when the eyelash cosmetics are used. Therefore, the fiber length is preferably 300 nm to 2 μm. The fiber length described in this embodiment is the average value of the lengths measured by SEM observation of co-continuous fibrous carbon and tracing from one branch to the next (between adjacent branches). Define. The number of measurement points is 500 or more.

In order to produce co-continuous fibrous carbon having a fiber diameter of 10 nm to 200 nm and a fiber length of 300 nm to 2 μm, the cellulose nanofibers used preferably have a fiber diameter of 20 nm to 400 nm and a fiber length of 500 nm to 4 μm. Is.

Normally, cellulose nanofibers are carbonized in the carbonization step (step 4), and the fibers become thinner and shorter than before carbonization due to decomposition, combustion, activation, and the like. However, when cellulose nanofibers having a fiber diameter smaller than 20 nm are used, the fibers aggregate in the freezing step (step S2), and a dried cellulose nanofiber having a large fiber diameter can be obtained in the subsequent drying step (step S3). .. Therefore, when cellulose nanofibers having a fiber diameter smaller than 20 nm are used, the fiber diameter of the obtained co-continuous fibrous carbon becomes larger than 200 nm.

[Manufacturing method of eyelash cosmetics]
Eyelash cosmetics include pigments, waxes, liquid oils, coating agents and thickeners. In this embodiment, the pigment contains co-continuous fibrous carbon having a three-dimensional network structure in which carbon is branched.

FIG. 3 is a flowchart showing a method for manufacturing eyelash cosmetics according to the present embodiment. The illustrated manufacturing method further includes a pulverization step (step S5) and a mixing step (step S6) in the manufacturing method (steps S1-S4) shown in FIG. That is, in the eyelash cosmetics of the present embodiment, the steps of steps S5-S6 are added to the co-continuous fibrous carbon produced in steps S1-S4. Since steps S1 to S4 are the same as the manufacturing method of FIG. 1, description thereof will be omitted here.

In the crushing step, the co-continuous fibrous carbon carbonized in the above-mentioned carbonization step (step S4) is crushed (step S5). The crushing process uses, for example, a mixer, a homogenizer, an ultrasonic homogenizer, a high-speed rotary shear type stirrer, a colloidal mill, a roll mill, a high-pressure injection disperser, a rotary ball mill, a vibration ball mill, a planetary ball mill, an attritor, etc. Make continuous fibrous carbon into powder or slurry.

In this case, the co-continuous fibrous carbon preferably has a secondary particle diameter of 10 nm to 1 mm, more preferably 1 μm to 50 μm. This is because when the secondary particle size is crushed to a size smaller than 10 nm, the co-continuous structure is broken and the eyelash cosmetics are aggregated during storage.

Further, when the secondary particle diameter is larger than 1 mm, the fibrous carbon does not form a bundle, but the co-continuous fibrous carbon that functions as a pigment is not sufficiently dispersed, which causes coating spots. ..

Further, since the co-continuous fibrous carbon has a high porosity and a low density, when the co-continuous fibrous carbon is crushed alone, the powder of the co-continuous fibrous carbon flies during or after crushing, which makes it difficult to handle. be. Therefore, a wet pulverization method in which co-continuous fibrous carbon is impregnated with a solvent and then pulverized is preferable.

The solvent used in the wet state is not particularly limited, but is not particularly limited, for example, 3-methyl-3-methoxybutyl ether, 3-methyl-3--methoxybutanol, n-butanol, n-butylamine, n-methylpyrrolidone, acetone, isoamyl alcohol, iso. Butanol, isopropanol, ethanol, ethyl carbitol, ethylene glycol, ethylene glycol ethyl ether acetate, ethylene glycol butyl ether, octanol, carboxylic acid, diethylene glycol methyl ether, dipropylene glycol isopropyl ethyl ether, dipropylene glycol isopropyl methyl ether, dipropylene glycol ethyl Organic systems such as ether, dipropylene glycol methyl ether, dodecane, tripropylene glycol methyl ether, propanol, propylene glycol ethyl ether acetate, propylene monomethyl ether, hexadecane, heptane, methanol, butyl acetate, butyl lactate, unsaturated fatty acids, glycerin, etc. And at least one selected from the group consisting of water systems such as water. Further, the dispersion medium may consist of at least one selected from the above group.

It is also possible to use the components of the eyelash cosmetics used in step S6 as the solvent used here. In this case, since the eyelash cosmetics do not contain an unnecessary solvent, it is preferable to use the components of the eyelash cosmetics as the solvent used in the pulverization step.

In the mixing step, the material (co-continuous fibrous carbon) crushed in the crushing step (step S5) is mixed with the wax, liquid oil, coating agent, and thickener used for the eyelash cosmetics to prepare the eyelash cosmetics. Obtain (step S6).

The wax used in this embodiment is not particularly limited. , Hard lanolin, lanolin, vaseline, hardened castor oil, polyoxyethylene cholesterol ether, polyoxyethylene hydrogenated lanolin alcohol ether, polyoxyethylene lanolin alcohol ether, paraffin wax, bead wax, microcrystallin wax, jojobaroester, polyoxy It contains at least one selected from the group consisting of ethylene lanolin alcohol ether, hexyl laurate, lanolin fatty acid isopropyl, lanolin fatty acid polyethylene glycol, fatty acid glyceride, and alkyl silicone.

The amount of wax added to the eyelash cosmetics is appropriately adjusted, but is preferably 1 to 30% by mass, more preferably 5 to 25% by mass.

If the amount added is less than 1% by mass, it may not always be sufficient in terms of curl keeping effect, long rush effect, volume increasing effect, adhesive strength (makeup retention), etc. On the other hand, if the addition amount exceeds 30% by mass, the makeup lasts poorly. Further, it becomes sticky and has a high viscosity, which makes it difficult to apply.

The liquid oil content used in this embodiment is not particularly limited, and is, for example, hydrocarbon oils such as heavy isoparaffin, squalane, and liquid paraffin, cetyl-2-ethylhexanoate, 2-ethylhexyl palmitate, and 2-octyldodecylmili. Esters such as State, Neopentyl Glycol-2-ethylhexanoate, Isopropyl Millistate, Myristyl Millistate, Olive Oil, Avocado Oil, Johova Oil, Sunflower Oil, Saflower Oil, Camellia Oil, Macademia Nut Oil, Mink Oil, Oils and fats such as liquid lanolin, lanolin acetate, and castor oil, dimethylpolysiloxane, methylphenylpolysiloxane, gum-like dimethylpolysiloxane with high degree of polymerization, polyether-modified silicone, silicone-based oils such as amino-modified silicone, and fluorine-modified dimethyl. It contains at least one selected from the group consisting of fluorine-based oils such as polysiloxane, fluorine-modified methylphenylpolysiloxane, perfluoropolyether, and perfluorocarbon.

The amount of the liquid oil added to the eyelash cosmetics is appropriately adjusted, but is preferably 0.1 to 20% by mass, and more preferably 1 to 10% by mass.

If the addition amount is less than 0.1% by mass, it may not always be sufficient in terms of elongation (coating comfort) during coating. On the other hand, if the addition amount exceeds 20% by mass, the makeup lasts poorly.

The coating agent used in the present embodiment is not particularly limited, and is, for example, cellulose derivatives such as alkyl cellulose, dextrin, and nitrocellulose, latexes such as alkyl polyacrylate, polyvinyl acetate, polyvinyl alcohol, and polyvinylpyrrolidone, and trimethylsiloxy. Silicone resins such as silicic acid, trimethylsiloxysilylpropylcarbamide acid, acrylic silicone copolymer resin, fluorine-modified silicone, fluororesin, aromatic hydrocarbon resin, polymer emulsion resin, terpene resin, polybutene, polyisoprene, alkyd It contains at least one selected from the group consisting of resins, polyvinylpyrrolidone-modified polymers, rosin-modified resins, and polyurethanes.

The amount of the coating agent added to the eyelash cosmetics is appropriately adjusted, but is preferably 1 to 25% by mass, more preferably 2 to 20% by mass. If the amount added is less than 1% by mass, the curl-up effect is reduced and the makeup lasts poorly. On the other hand, if the addition amount exceeds 25% by mass, it becomes difficult to apply.

The thickener used in the present embodiment is not particularly limited, and includes, for example, at least one selected from the group consisting of dextrin fatty acid ester, bentonite, xanthan gum, and cellulose gum.

The amount of the thickener added to the eyelash cosmetics is appropriately adjusted, but is preferably 0.1 to 30% by mass, and more preferably 1 to 20% by mass. If the addition amount is less than 0.1% by mass, it may be difficult to adjust the viscosity to a sufficient level. On the other hand, if the addition amount exceeds 30% by mass, the viscosity becomes too high and it becomes difficult to apply.

Further, an ingredient usually added to eyelash cosmetics may be added as long as the effect of the present embodiment is not impaired. Examples of such components include synthetic fibers, alcohols, polyhydric alcohols, chemicals, surfactants, water-soluble polymers, clay minerals, powders, preservatives, fragrances, antioxidants, ultraviolet absorbers, and moisturizers. Examples thereof include oily components such as agents, water, oils and fats, and hydrocarbon oils.

The mixing step uses, for example, a mixer, a homogenizer, an ultrasonic homogenizer, a high-speed rotary shear type stirrer, a colloid mill, a roll mill, a high-pressure injection disperser, a rotary ball mill, a vibration ball mill, a planetary ball mill, an attritor, a kneader, and the like. be able to.

The manufacturing method of this embodiment does not have to include all the steps shown in FIG. For example, by simultaneously adding wax, liquid oil, a film agent, and a thickener together with co-continuous fibrous carbon during the pulverization step, pulverization and mixing can be performed at the same time. In this case, the mixing step is performed. It does not have to be.

[Evaluation of eyelash cosmetics]
For the purpose of confirming the effects of the present embodiment described above, the eyelash cosmetics produced by the production method of the present embodiment (Experimental Examples 1 to 12) and the eyelash cosmetics produced by a different production method from the present embodiment (Experimental Examples 1 to 12). An experiment was conducted to compare with Comparative Examples 1 to 6).

The evaluation methods for eyelash cosmetics in Experimental Examples 1 to 12 and Comparative Examples 1 to 6 below are as follows.

(1) Curl-keeping effect evaluation panel We asked 10 people to apply eyelash cosmetics to the eyelashes, visually observe whether the eyelashes curled upward, and answered whether they had the curl-keeping effect. received. The number of people who answered that they had a curl-keeping effect was used to evaluate according to the following criteria.
◎: 7 or more people answered that there is a curl-keeping effect 〇: 5-6 people answered that there is a curl-keeping effect △: 3-4 people answered that there is a curl-keeping effect ×: There is a curl-keeping effect 2 or less people answered

(2) Long rush effect evaluation panel We asked 10 people to apply eyelash cosmetics to the eyelashes, visually observe whether the eyelashes became longer, and answer whether they had a long lash effect. .. The number of people who answered that they had a long rush effect was used to evaluate according to the following criteria.
◎: 7 or more people answered that there is a long rush effect 〇: 5-6 people answered that there is a long rush effect △: 3-4 people answered that there is a long rush effect ×: There is a long rush effect 2 or less people answered

(3) Volume-up effect evaluation panel We asked 10 people to apply eyelash cosmetics to the eyelashes, visually observe whether the eyelashes became thicker, and answer whether they had the volume-up effect. .. The number of people who answered that there was a volume-up effect was used to evaluate according to the following criteria.
◎: 7 or more people answered that there is a volume-up effect 〇: 5-6 people answered that there is a volume-up effect △: 3-4 people answered that there is a volume-up effect ×: There is a volume-up effect 2 or less people answered

(4) Applicability evaluation panel We asked 10 people to apply eyelash cosmetics to the eyelashes and answered whether they were comfortable to apply (whether they were smooth to use). The number of people who answered that they were comfortable to apply was used and evaluated according to the following criteria.
◎: 7 or more people answered that it was comfortable to apply 〇: 5 to 6 people answered that it was comfortable to apply △: 3 to 4 people answered that it was comfortable to apply ×: Comfortable to apply 2 or less people answered

(5) Makeup retention evaluation panel We asked 10 people to apply eyelash cosmetics to the eyelashes, and visually observed whether the adhesive strength was maintained even after one day's life, and whether the makeup retention was good. I asked you to answer. The number of people who answered that they had good makeup was evaluated according to the following criteria.
◎: 7 or more people answered that they had good makeup 〇: 5-6 people answered that they had good makeup △: 3-4 people answered that they had good makeup ×: Good makeup 2 or less people answered

(6) Stability over time A glass bottle was filled with eyelash cosmetics, left under the following three conditions, and changes in state after 30 days were observed and evaluated according to the following criteria.
Condition 1: Leave for 30 days at room temperature Condition 2: Leave for 30 days in a constant temperature bath set at 40 ° C Condition 3: Raise the temperature from -5 ° C to 45 ° C in 2 days, then from 45 ° C to -5 ° C 2 Leave for 30 days in a constant temperature bath set to a temperature cycle that lowers the temperature in a day ◎: No change under all conditions 〇: A slight change in hardness etc. was confirmed, but there is no problem in use. Was inside Δ: Solidification or separation was confirmed under at least one condition ×: Solidification or separation was confirmed under all conditions

Below, the oil-in-water type eyelash cosmetics shown in FIG. 4 (Experimental Examples 1-4, Comparative Example 1-2) and the oily eyelash cosmetics shown in FIG. 5 (Experimental Examples 5-8, Comparative Example 3, 4) and the water-in-oil type eyelash cosmetics shown in FIG. 6 (Experimental Examples 9-12 and Comparative Examples 5-6) will be described.

(Experimental Example 1)
Experimental Example 1 is an oil-in-water type eyelash cosmetic containing co-continuous fibrous carbon as a pigment. The eyelash cosmetics of Experimental Example 1 were produced by the following procedure.

<Manufacturing procedure for co-continuous fibrous carbon>
In Experimental Example 1, cellulose nanofibers (average fiber diameter 40 nm, average fiber length 1 μm) were used, and 1 g of cellulose nanofibers and 10 g of ultrapure water were stirred with a homogenizer (manufactured by SMT) for 12 hours to disperse the cellulose nanofibers. The liquid was adjusted and poured into a test tube.

The cellulose nanofiber dispersion was completely frozen by freezing the above test tube in a freezer at -30 ° C for 2 hours. After completely freezing the cellulose nanofiber dispersion, take out the frozen cellulose nanofiber dispersion on a chalet and dry it in a vacuum of 10 Pa or less with a freeze dryer (manufactured by Tokyo Science Instruments Co., Ltd.) for 24 hours. A dried product of cellulose nanofibers was obtained. After drying in a vacuum, the cellulose nanofibers were carbonized by firing at 600 ° C. for 2 hours in a nitrogen atmosphere, whereby the co-continuous fibrous carbon of Experimental Example 1 was produced. When the co-continuous fibrous carbon produced in this experimental example was observed by SEM, it was confirmed that the average fiber diameter was 20 nm and the average fiber length was 500 nm.

<Manufacturing procedure for eyelash cosmetics>
The components of the eyelash cosmetics having the composition shown in FIG. 4 were adjusted by the following production procedure at the ratio (mass%) of Experimental Example 1 shown in FIG. In Experimental Example 1, the co-continuous fibrous carbon prepared by the above-mentioned production procedure was used for the A phase, and the blending amount of the co-continuous fibrous carbon was 10% by mass.

Here, purified water, 1,3-butylene glycol, xanthan gum, triethanolamine, tetrasodium edetate dihydrate, polyoxyethylene sorbitan monostearate, ethyl paraoxybenzoate, butyl paraoxybenzoate, paraoxybenzoate in phase B. Methyl acid acid and D-pantothenyl alcohol were used. For the C phase, glycerin monostearate, natural vitamin E, beeswax bleached wax, carnauba wax, and candelilla resin (manufactured by Japan Natural Products Co., Ltd.) were used. A (Acrylate / ethylhexyl acrylate) copolymer (manufactured by Daito Kasei Kogyo Co., Ltd.) was used for the D phase, phenoxyethanol was used for the E phase, and nylon fiber (manufactured by Cosmetics Terials) with a length of 2 mm was used for the F phase.

The components of the oil-in-water type eyelash cosmetics having the composition shown in FIG. 4 were adjusted according to the following manufacturing procedure. The B-phase mixture shown in FIG. 4 was heated to 85 ° C., the C-phase mixture was heated to 95 ° C., and the heated B-phase and C-phase and A-phase were stirred with a homogenizer for 2 hours while maintaining 85 ° C. Phase B and C phases were emulsified, and phase A was pulverized and dispersed. The resulting mixture was cooled to 60 ° C. with stirring, the D, E and F phase components were added and mixed in a homogenizer for 2 hours. The homogeneous mixture was cooled to 32 ° C. in the air to obtain an oil-in-water type eyelash cosmetic.

(Comparative Example 1)
Comparative Example 1 is an eyelash cosmetic in which the co-continuous fibrous carbon (pigment) of the eyelash cosmetic of Experimental Example 1 is replaced with the conventionally used black iron oxide (spherical, average particle size 2 μm). In Comparative Example 1, black iron oxide was used for the A phase in the production procedure of Experimental Example 1, and other eyelash cosmetics were prepared in the same manner as in Experimental Example 1.

FIG. 4 shows the evaluation results of Experimental Example 1 evaluated by the above evaluation method. Looking at Experimental Example 1 in FIG. 4, the eyelash cosmetics of Experimental Example 1 were compared in all evaluations of curl-keeping effect, long rush effect, volume-up effect, application comfort, makeup retention, and stability over time. It was superior to Example 1. As can be seen from this result, the eyelash cosmetics using the co-continuous fibrous carbon of the present embodiment as a pigment have a significantly superior curl-keeping effect and long rush as compared with the eyelash cosmetics containing black iron oxide. It can be said that it exerts an effect, a volume-up effect, a feeling of application, a long-lasting makeup, and stability over time.

(Experimental Example 2)
Experimental Example 2 is a cosmetic for eyelashes prepared by the production method of Experimental Example 1 in which the blending amount of the co-continuous fibrous carbon is 5% by mass. The blending amount of the B phase to the F phase is the same as that of Experimental Example 1. Therefore, in Experimental Example 2, the blending amount of purified water was increased by 20% by mass as compared with Experimental Example 1. Using the composition and blending amount shown in FIG. 4, the eyelash cosmetics of this experimental example were prepared by the same production method as in experimental example 1.

FIG. 4 shows the evaluation results of Experimental Example 2 evaluated by the above evaluation method. Looking at Experimental Example 2 in FIG. 4, the eyelash cosmetics of Experimental Example 2 are compared with Comparative Example 1 in all evaluations of curl-keeping effect, long rush effect, volume-up effect, application comfort, makeup retention, and stability over time. Was better. Further, it can be seen that Experimental Example 2 is more comfortable to apply than Experimental Example 1. It is considered that this is because the proportion of co-continuous fibrous carbon contained in the eyelash cosmetics decreased, the viscosity decreased, and the eyelash cosmetics spread better at the time of application.

Therefore, the blending amount of the co-continuous fibrous carbon is preferably 5% by mass or less of the eyelash cosmetics. In the case of eyelash cosmetics in which the blending amount of co-continuous fibrous carbon was less than 0.5% by mass and the same as in Experimental Example 2 except for purified water, sufficient black color could not be obtained, and eyelash makeup. Could not be used as a fee. Sufficient black in this case means that a 5 cm line is overlaid on the back of the hand three times using a brush for eyelash cosmetics, and the black line is not interrupted by 2 cm or more.

(Experimental Example 3)
Experimental Example 3 is an eyelash cosmetic produced from the eyelash cosmetic of Experimental Example 2 without including F-phase nylon fiber. The blending amount of the A phase to the E phase is the same as that of Experimental Example 2. Therefore, in Experimental Example 3, the blending amount of purified water was increased by 2% by mass as compared with Experimental Example 2. Using the composition and blending amount shown in FIG. 4, the eyelash cosmetics of this experimental example were prepared by the same production method as in experimental example 1.

FIG. 4 shows the evaluation results of Experimental Example 3 evaluated by the above evaluation method. From the results of FIG. 4, Experimental Example 3 was superior to Comparative Example 1 in the evaluation of curl-keeping effect, long rush effect, volume-up effect, application comfort, makeup retention, and stability over time. Further, Experimental Example 3 is evaluated as having a curl-keeping effect, a long rush effect, a volume-up effect, a feeling of application, and a long-lasting makeup as compared with Experimental Example 2.

Normally, a make-up for eyebrows that does not contain synthetic fibers (fiber material) such as nylon fiber tends to have a poor curl-keeping effect, a long rush effect, and a volume-up effect. It is considered that the co-continuous fibrous carbon used as a pigment showed the same effect as the synthetic fiber usually added to the eyebrows cosmetics. Further, it can be seen that Experimental Example 3 has higher stability over time than Experimental Example 2. This is due to the fact that the absence of synthetic fibers eliminates the agglutination and separation of synthetic fibers.

(Experimental Example 4)
In Experimental Example 4, the amount of components (phases B to E other than purified water) that affect the curl-keeping effect, long lash effect, volume-up effect, application comfort, makeup retention, and stability over time of Experimental Example 3 is used. Increased eyelash cosmetics.

In this experimental example, a cosmetic for eyelashes was prepared by the same production method as in Experimental Example 1 using the composition and the blending amount shown in FIG. Specifically, in this experimental example, the difference in weight (7% by mass) between the A phase (co-continuous fibrous carbon) and the F phase (nylon fiber) of Experimental Example 1 and Experimental Example 3 is shown in Experimental Example 1. The fibers were allocated to phases B to E other than purified water so as to have the same blending ratio as that of Experimental Example 1, and the total weight other than purified water was adjusted to be the same as that of Experimental Example 1. In FIG. 4, the total of the components other than the purified water of Experimental Example 4 does not match the total of the components other than the purified water of Experimental Example 1, but this is the difference due to rounding off to the third decimal place. Is.

FIG. 4 shows the evaluation results of Experimental Example 4 evaluated by the above evaluation method. From the results shown in FIG. 4, Experimental Example 4 was superior to Comparative Example 1 in the evaluation of curl-keeping effect, long rush effect, volume-up effect, application comfort, makeup retention, and stability over time. In addition, Experimental Example 4 had better makeup retention than Experimental Example 1-3. This is due to the increase in the amount of ingredients (phases B to E other than purified water) that affect the curl-keeping effect, long rush effect, volume-up effect, application comfort, makeup retention, and stability over time. .. In this experimental example, by using co-continuous fibrous carbon having a high dispersibility and a three-dimensional network structure as a pigment, the amount of the A-phase pigment added can be reduced, and instead of adding the F-phase nylon fiber, others can be used. Since the amount of the component added can be increased, such excellent performance can be realized.

(Comparative Example 2)
Comparative Example 2 is a cosmetic for eyelashes in which the co-continuous fibrous carbon of Experimental Example 4 is replaced with conventionally used black iron oxide (spherical, average particle size 2 μm). Specifically, in Comparative Example 2, black iron oxide was used for the A phase of Experimental Example 4, and other eyelash cosmetics were prepared in the same manner as in Experimental Example 4.

In Comparative Example 2, since black iron oxide is used as a pigment, dispersibility is poor, and when the blending amount is 5% by mass or less, sufficient black color cannot be obtained and it cannot be used as a cosmetic for eyelashes. rice field. Sufficient black in this case means that a 5 cm line is overlaid on the back of the hand three times using a brush for eyelash cosmetics, and the black line is not interrupted by 2 cm or more.

(Experimental Examples 5-8, Comparative Examples 3 and 4)
In order to evaluate the effect of this embodiment also in oil-based eyelash cosmetics, in Experimental Examples 5 to 8 and Comparative Examples 3 and 4, the underwater oil-type eyelash makeup of Experimental Examples 1 to 4 and Comparative Examples 1 and 2 are used. Ingredients other than the A phase of the agent were replaced with oily eyelash cosmetics, and the same preparation and evaluation were performed.

The components of the oily eyelash cosmetics having the composition shown in FIG. 5 were adjusted according to the following manufacturing procedure. Here, isododecane, paraffin, microcrystalline wax, sala beeswax, polyethylene wax, propyl paraoxybenzoate, and natural vitamin E were used as the B phase. Dimethyl distearyl ammonium hectorite and propylene carbonate are used for the C phase, trimethylsiloxysilicic acid / isodecane (manufactured by Shin-Etsu Chemical Co., Ltd.) is used for the D phase, and nylon fiber (manufactured by Cosmetics Terials) is used for the E phase. 2 mm was used.

The B-phase mixture shown in FIG. 5 was heated to 90 ° C. and mixed with a homogenizer for 1 hour. The composition of phase A and phase C was added to the mixture of phase B, and the mixture was again disrupted with a homogenizer for 2 hours. Then, the obtained mixture was added with the components of the D phase and the E phase at 50 ° C. and uniformly mixed with a homogenizer for 2 hours to obtain an oily eyelash cosmetic.

Looking at the evaluations of Experimental Examples 5 to 8 and Comparative Examples 3 and 4 in FIG. 5, the eyelash cosmetics of Experimental Examples 5 to 8 had a curl-keeping effect, a long rush effect, a volume-up effect, a feeling of application, and a make-up lasting. It was superior to Comparative Examples 3 and 4 in all of the stability over time. As can be seen from this result, even in the oil-based eyelash cosmetics, the eyelash cosmetics containing the co-continuous fibrous carbon of the present embodiment can produce eyelash cosmetics with a small pigment ratio. Even if it does not contain synthetic fibers, it exhibits remarkably excellent curl-keeping effect, long lash effect, volume-up effect, application comfort, makeup retention, and stability over time.

(Experimental Examples 9 to 12, Comparative Examples 5 and 6)
In order to evaluate the effect of this embodiment also in the water-in-oil type eyelash cosmetics, in Experimental Examples 9 to 12 and Comparative Examples 5 and 6, the underwater oil type of Experimental Examples 1 to 4 and Comparative Examples 1 and 2 were used. Ingredients other than the A phase of the eyelash cosmetics were replaced with water-in-oil type eyelash cosmetics, and the same preparation and evaluation were performed.

The components of the water-in-oil type eyelash cosmetics having the composition shown in FIG. 6 were adjusted according to the following manufacturing procedure. Here, in phase B, isododecane, ester gum, microcrystalline wax, polyethylene wax, carnauba wax, dimethyl distearyl ammonium hectorite, ethanol, polyglyceryl diisostearate, macadamia nut oil fatty acid phytosteryl, and natural vitamin E. And the mica titanium were used. Purified water, polyvinylpyrrolidone, D-pantothenyl alcohol, sodium chloride, and 1,2-pentanediol were used in the C phase.

The B-phase mixture shown in FIG. 6 was heated to 95 ° C., the C-phase mixture was heated to 85 ° C., and the heated B-phase and C-phase and A-phase were stirred with a homogenizer for 2 hours while maintaining 85 ° C. Phases B and C were emulsified and phase A was pulverized and dispersed. The obtained mixture was cooled to 40 ° C. with stirring, the components of D phase, E phase, F phase and G phase were added, and the mixture was mixed with a homogenizer for 2 hours. The homogeneous mixture was cooled to 32 ° C. in the air to obtain a water-in-oil type eyelash cosmetic.

Looking at the evaluations of Experimental Examples 9 to 12 and Comparative Examples 5 and 6 in FIG. 6, the eyelash cosmetics of Experimental Examples 9 to 12 have a curl-keeping effect, a long rush effect, a volume-up effect, a feeling of application, and a make-up lasting. It was superior to Comparative Examples 5 and 6 in all of the stability over time. As can be seen from this result, even in the water-in-oil type eyelash cosmetics, the eyelash cosmetics containing the co-continuous fibrous carbon of the present embodiment can produce eyelash cosmetics with a small pigment ratio. Even if it does not contain synthetic fibers, it exhibits remarkably excellent curl-keeping effect, long lash effect, volume-up effect, application comfort, makeup retention, and stability over time.

The cosmetic for eyelashes of the present embodiment described above contains co-continuous fibrous carbon having a three-dimensional network structure in which carbon is branched as a pigment, and the co-continuous fibrous carbon is produced from cellulose nanofibers.

The eyelash cosmetics of the present embodiment use co-continuous fibrous carbon having a three-dimensional network structure as the pigment, so that the fibrous carbons are uniformly dispersed in the eyelash cosmetics without forming a bundle. Further, in the present embodiment, the fibrous carbon is uniformly dispersed in the dispersion medium, so that the blending ratio of the pigment can be lowered, and even when the synthetic fiber is not contained, the curl-keeping effect, the long lash effect, and the effect can be reduced. It is possible to provide eyelash cosmetics that have a volume-increasing effect, elongation during application (applying comfort), and adhesive strength (makeup retention).

Further, in the present embodiment, by using carbon of cellulose nanofiber derived from a natural product, it becomes possible to produce a cosmetic for eyelashes composed of raw materials having a low environmental load.

Further, in this embodiment, synthetic fibers normally added to eyelash cosmetics are not included. Synthetic fibers used in eyelash cosmetics are a type of microplastic, which has a large impact on marine pollution, and consumers who are highly environmentally conscious tend to avoid purchasing them. Since the eyelash cosmetics of the present embodiment do not contain such synthetic fibers, it is possible to produce environmentally friendly eyelash cosmetics.

<Second embodiment>
The eyelash cosmetics according to the second embodiment of the present invention will be described. The eyelash cosmetics of the present embodiment are eyelash cosmetics containing rod-shaped carbon obtained by crushing co-continuous fibrous carbon having a three-dimensional network structure in which carbon is branched.

Since the method for producing co-continuous fibrous carbon of the present embodiment is the same as the method for producing co-continuous fibrous carbon of the first embodiment (see FIG. 1), the description thereof is omitted here. As shown in FIG. 2, the co-continuous fibrous carbon of the present embodiment has a three-dimensional network structure in which carbon is branched.

As described in the first embodiment, the rod-shaped carbon has a color according to the progress of carbonization of the co-continuous fibrous carbon. That is, it is possible to change the color of the co-continuous fibrous carbon by adjusting the progress of carbonization. Therefore, by using the rod-shaped carbon of the present embodiment obtained by crushing the co-continuous fibrous carbon, the progress of carbonization of the co-continuous fibrous carbon can be adjusted without preparing pigments of a plurality of colors. It is possible to realize a brown or black eyebrows cosmetic having a different color.

[Manufacturing method of rod-shaped carbon]
Rod-shaped carbon is produced from the obtained co-continuous fibrous carbon. Rod-shaped carbon is a rod-shaped nanocarbon material that is not hollow. Here, the rod is not hollow and refers to a fiber having an aspect ratio (rod length / rod width) of 2 to 200.

FIG. 7 is a flowchart showing a method for manufacturing rod-shaped carbon. The production method shown in FIG. 7 further includes a pulverization step (step S5) in the production method of co-continuous fibrous carbon. That is, the method for producing rod-shaped carbon of the present embodiment includes a crushing step of crushing the co-continuous fibrous carbon obtained by the manufacturing method of FIG. 1 to obtain rod-shaped carbon. Since steps S1 to S4 are the same as the manufacturing method of FIG. 1, description thereof will be omitted here.

In the crushing step, the dried body (co-continuous fibrous carbon) carbonized in the above-mentioned carbonization step (step S4) is crushed (step S5). The crushing process uses, for example, a mixer, a homogenizer, an ultrasonic homogenizer, a high-speed rotary shear type stirrer, a colloidal mill, a roll mill, a high-pressure injection disperser, a rotary ball mill, a vibration ball mill, a planetary ball mill, an attritor, etc. Make continuous fibrous carbon into powder or slurry. The pulverization method includes a wet method and a dry method, but a wet method capable of more uniform and fine pulverization is preferable.

The dispersion medium used in the wet state is not particularly limited, but is, for example, an aqueous _{system such as water (H 2} O), carboxylic acid, methanol (CH ₃ OH), ethanol (C ₂ H ₅ OH), propanol (C ₃ H). ₇ OH), n-butanol, isobutanol, n-butylamine, dodecane, unsaturated fatty acids, ethylene glycol, heptan, hexadecane, isoamyl alcohol, octanol, isopropanol, acetone, glycerin and at least selected from the group consisting of organic systems. Includes one. Further, the dispersion medium may consist of at least one selected from the above group.

It is also possible to use the components of the eyelash cosmetics used in the mixing step (FIG. 9: step S6) described later as the dispersion medium used here. In this case, since the eyelash cosmetics do not contain an unnecessary dispersion medium, it is preferable to use the components of the eyelash cosmetics as the dispersion medium used in the pulverization step.

FIG. 8 is an SEM image of rod-shaped carbon produced by the manufacturing method of the present embodiment. The magnification in FIG. 8 is 100,000 times. From FIG. 8, it can be seen that rod-shaped carbon is formed.

In the present embodiment, by using the co-continuous fibrous carbon obtained by the manufacturing method of FIG. 1, it is possible to provide a rod-shaped carbon manufacturing method that is easy to mass-produce at low cost.

As described above, unlike carbon black, carbon nanotubes, fullerenes, graphene, graphite, etc., which are synthesized from fossil fuels, the rod-shaped carbon of the present embodiment is a naturally derived raw material and has a low burden on the environment.

Further, the rod-shaped carbon of the present embodiment has a rod-shaped structure (shape). Therefore, even when this rod-shaped carbon is added to eyelash cosmetics as a black pigment, the rod structure is oriented along the eyelash direction at the time of application, resulting in excellent curl-keeping effect, long rush effect, volume-up effect, and application. It is possible to achieve time extension (feeling of application) and adhesive strength (makeup lasting). That is, the rod-shaped carbons are oriented and arranged in the longitudinal direction in parallel with the eyelashes (application direction).

If the rod diameter of the rod-shaped carbon is too small, there is a concern about deposition in the living body and effects on the living body. Further, if the rod diameter is too large, the dispersibility is lowered when added to the eyelash cosmetics, and sufficient color development performance cannot be obtained. Therefore, the rod diameter is preferably 10 nm to 200 nm.

Similarly, the rod length of the rod-shaped carbon is preferably 20 nm to 400 nm, more preferably 50 nm to 200 nm. This is because when the rod length is crushed to be smaller than 20 nm, the aspect ratio (rod length / rod width) of the rod-shaped carbon becomes small, and the specificity due to the shape of the nanorod is lost. Further, when it exceeds 400 nm, the branched structure of the co-continuous fibrous carbon remains, which makes it difficult to manufacture the rod-shaped carbon. Specifically, the rod-shaped carbon is a cylinder, but if there is a branch portion, the rod-shaped carbon does not have the shape of a cylinder. That is, if the branched portion remains, it becomes difficult to manufacture rod-shaped carbon in the shape of a cylinder.

For example, when rod-shaped carbon having a rod diameter of 10 nm to 200 nm and a rod length of 20 nm to 400 nm is used for eyelash cosmetics, the rod-shaped carbon is oriented along the eyelash direction at the time of application to maintain excellent curl. It is possible to realize the effect, long lash effect, volume up effect, elongation at the time of application (applyance comfort), and adhesive force (makeup retention).

The rod length described in this embodiment is defined as the average value of the lengths measured by observing the rod-shaped carbon by SEM and tracing the rod. The number of measurement points is 500 or more.

In order to produce rod-shaped carbon having a rod diameter of 10 nm to 200 nm and a rod length of 20 nm to 400 nm, it is preferable that the cellulose nanofibers used have a fiber diameter of 20 nm to 400 nm and a fiber length of 500 nm to 4 μm. ..

[Manufacturing method of eyelash cosmetics]
Eyelash cosmetics include pigments, waxes, liquid oils, coating agents, thickeners and the like. In the present embodiment, the pigment includes rod-shaped carbon made from co-continuous fibrous carbon having a three-dimensional network structure in which carbon is branched.

FIG. 9 is a flowchart showing a method for manufacturing eyelash cosmetics according to the present embodiment. The illustrated manufacturing method further includes a mixing step (step S6) in the manufacturing method (steps S1-S5) shown in FIG. That is, in the eyelash cosmetics of the present embodiment, the mixing step of step S6 is added to the rod-shaped carbon produced in steps S1-S5 of FIG. 7.

In the mixing step, the material (rod-shaped carbon) crushed in the crushing step (step S5) is mixed with the wax, liquid oil, film agent, and thickener used for the eyelash cosmetics to obtain the eyelash cosmetics (step S5). Step S6).

The wax, liquid oil, film agent, and thickener used in this embodiment are the same as the wax, liquid oil, film agent, and thickener described in the first embodiment. Therefore, the description thereof is omitted here.

The manufacturing method of this embodiment does not have to include all the steps. For example, by simultaneously adding wax, liquid oil, a film agent, and a thickener during the pulverization step, pulverization and mixing can be performed at the same time, and in this case, the mixing step does not have to be performed.

The evaluation method of the eyelash cosmetics in Experimental Examples 1 to 12 and Comparative Examples 1 to 6 below is the same as that of the first embodiment.

Below, the oil-in-water type eyelash cosmetics shown in FIG. 10 (Experimental Examples 1-4, Comparative Example 1-2) and the oily eyelash cosmetics shown in FIG. 11 (Experimental Examples 5-8, Comparative Example 3, 4) and the water-in-oil type eyelash cosmetics shown in FIG. 12 (Experimental Examples 9-12 and Comparative Examples 5-6) will be described.

(Experimental Example 1)
Experimental Example 1 is an oil-in-water type eyelash cosmetic containing rod-shaped carbon made from co-continuous fibrous carbon. The eyelash cosmetics of Experimental Example 1 were produced by the following procedure.

<Manufacturing procedure for rod-shaped carbon>
In Experimental Example 1, cellulose nanofibers (average fiber diameter 60 nm, average fiber length 1 μm) were used, and 1 g of cellulose nanofibers and 10 g of ultrapure water were stirred with a homogenizer (manufactured by SMT) for 12 hours to disperse the cellulose nanofibers. The liquid was adjusted and poured into a test tube.

The cellulose nanofiber dispersion was completely frozen by freezing the above test tube in a freezer at -30 ° C for 2 hours. After completely freezing the cellulose nanofiber dispersion, take out the frozen cellulose nanofiber dispersion on a chalet and dry it in a vacuum of 10 Pa or less with a freeze dryer (manufactured by Tokyo Science Instruments Co., Ltd.) for 24 hours. A dried product of cellulose nanofibers was obtained. After drying in a vacuum, the cellulose nanofibers were carbonized by firing at 600 ° C. for 2 hours in a nitrogen atmosphere, whereby the co-continuous fibrous carbon of Experimental Example 1 was produced. When the co-continuous fibrous carbon produced in this experimental example was observed by SEM, it was confirmed that the average fiber diameter was 30 nm and the average fiber length was 500 nm.

After impregnating the prepared co-continuous fibrous carbon with water, a zirconia ball having a diameter of 0.8 mm to 1.0 mm is used in a ball mill (manufactured by Nippon Densan Sympo), and the zirconia balls are crushed at a rotation speed of 60 r / min for 72 hours. Therefore, the crushing step was performed. Then, using a hot plate, it was dried at 80 ° C. for 12 hours to evaporate water as a dispersion medium to prepare rod-shaped carbon.

When the rod-shaped carbon produced in this experimental example was observed by SEM, it was confirmed that the average rod diameter was 30 nm and the rod length was 200 nm.

<Manufacturing procedure for eyelash cosmetics>
The components of the oil-in-water type eyelash cosmetics having the composition of Experimental Example 1 shown in FIG. 10 were adjusted by the following production procedure at the ratio (mass%) of Experimental Example 1 shown in FIG. In Experimental Example 1, rod-shaped carbon made from the co-continuous fibrous carbon prepared in the above preparation procedure was used for the A phase. In Experimental Example 1, the blending amount of the rod-shaped carbon was 10% by mass.

The composition and blending amount of the B phase to F phase of the eyelash cosmetics (Experimental Example 1-4, Comparative Example 1-2) shown in FIG. 10 are the same as those in FIG. 4 of the first embodiment.

The B-phase mixture is heated to 85 ° C., the C-phase mixture is heated to 95 ° C., and the heated B-phase and C-phase and A-phase are stirred with a homogenizer for 30 minutes to emulsify the B-phase and C-phase, and A. The phase was ground and dispersed. The resulting mixture was cooled to 60 ° C. with stirring, the D, E and F phase components were added and mixed with a homogenizer for 30 minutes. The homogeneous mixture was cooled to 32 ° C. in the air to obtain the eyelash cosmetic of Experimental Example 1.

(Comparative Example 1)
Comparative Example 1 is an eyelash cosmetic in which the rod-shaped carbon of the eyelash cosmetic of Experimental Example 1 is replaced with the conventionally used black iron oxide (spherical, average particle size 2 μm).

Looking at Experimental Example 1 and Comparative Example 1 of FIG. 10, the eyelash cosmetics of Experimental Example 1 are compared in the evaluation of curl-keeping effect, long rush effect, volume-up effect, application comfort, makeup retention, and stability over time. It was superior to Example 1. As can be seen from this result, the eyelash cosmetics containing rod-shaped carbon made from the co-continuous fibrous carbon of the present embodiment have significantly superior curls as compared with the eyelash cosmetics containing black iron oxide. It has a keep effect, a long lash effect, a volume-up effect, a feeling of application, long-lasting makeup, and stability over time.

(Experimental Example 2)
Experimental Example 2 is an eyelash cosmetic containing 5% by mass of rod-shaped carbon in the eyelash cosmetic of Experimental Example 1. Therefore, in Experimental Example 2, the blending amount of purified water was increased by 5% by mass as compared with Experimental Example 1. Using the composition and blending amount shown in FIG. 10, the eyelash cosmetics of this experimental example were prepared by the same production method as in experimental example 1.

FIG. 10 shows the evaluation results of Experimental Example 2 evaluated by the above evaluation method. From the evaluation results of FIG. 10, Experimental Example 2 was superior to Comparative Example 1 in the evaluation of curl keeping effect, long rush effect, volume up effect, application comfort, makeup retention, and stability over time. In addition, it can be seen that the coating comfort is superior to that of Experimental Example 1. It is considered that this is because the amount of rod-shaped carbon contained in the eyelash cosmetics decreased, the viscosity decreased, and the eyelash cosmetics spread better at the time of application.

Therefore, the blending amount of rod-shaped carbon is preferably 5% by mass or less of the eyelash cosmetics. In the case of eyelash cosmetics in which the amount of rod-shaped carbon was less than 0.5% by mass and the same as in Experimental Example 2 except for purified water, sufficient black color could not be obtained, and as eyelash cosmetics. Could not be used. Sufficient black in this case means that a 5 cm line is overlaid on the back of the hand three times using a brush for eyelash cosmetics, and the black line is not interrupted by 2 cm or more.

(Experimental Example 3)
Experimental Example 3 is an eyelash cosmetic produced from the eyelash cosmetic of Experimental Example 2 without including F-phase nylon fiber. The blending amount of the A phase to the E phase excluding purified water is the same as that of Experimental Example 2. Therefore, in Experimental Example 3, the blending amount of purified water was increased by 2% by mass as compared with Experimental Example 2. Using the composition and blending amount shown in FIG. 10, the eyelash cosmetics of this experimental example were prepared by the same production method as in experimental example 1.

FIG. 10 shows the evaluation results of Experimental Example 3 evaluated by the above evaluation method. From the results of FIG. 10, Experimental Example 3 was superior to Comparative Example 1 in the evaluation of curl-keeping effect, long rush effect, volume-up effect, application comfort, makeup retention, and stability over time. Further, Experimental Example 3 is evaluated as having a curl-keeping effect, a long rush effect, a volume-up effect, a feeling of application, and a long-lasting makeup as compared with Experimental Example 2.

Normally, eyelash cosmetics that do not contain synthetic fibers (fiber materials) such as nylon fibers tend to have poor curl-keeping effect, long rush effect, and volume-up effect. It is considered that the rod-shaped carbon used as a pigment showed the same effect as the synthetic fiber usually added to eyelash cosmetics. Further, it can be seen that Experimental Example 3 has higher stability over time than Experimental Example 2. This is due to the fact that the absence of synthetic fibers eliminates the agglutination and separation of synthetic fibers.

In this experimental example, a cosmetic for eyelashes was prepared by the same production method as in Experimental Example 1 using the composition and the blending amount shown in FIG. Specifically, in this experimental example, the difference in weight (7% by mass) between the A phase (rod-shaped carbon) and the F phase (nylon fiber) of Experimental Example 1 and Experimental Example 3 is mixed with Experimental Example 1. Allocated to phases B to E other than purified water so as to be the same as the ratio, and prepared so that the total weight other than purified water was equivalent to that of Experimental Example 1. In FIG. 10, the total of the components other than the purified water of Experimental Example 4 does not match the total of the components other than the purified water of Experimental Example 1, but this is a difference due to rounding off to the third decimal place. Is.

FIG. 10 shows the evaluation results of Experimental Example 4 evaluated by the above evaluation method. From the results of FIG. 10, Experimental Example 4 was superior to Comparative Example 1 in the evaluation of curl-keeping effect, long rush effect, volume-up effect, application comfort, makeup retention, and stability over time. In addition, Experimental Example 4 had better makeup retention than Experimental Example 1-3. This is due to the increase in the amount of ingredients (phases B to E other than purified water) that affect the curl-keeping effect, long rush effect, volume-up effect, application comfort, makeup retention, and stability over time. .. In this experimental example, by using co-continuous fibrous carbon having a high dispersibility and a three-dimensional network structure as a pigment, the amount of the A-phase pigment added can be reduced, and instead of adding the F-phase nylon fiber, others can be used. Since the amount of the component added can be increased, such excellent performance can be realized.

(Comparative Example 2)
Comparative Example 2 is a cosmetic for eyelashes in which the rod-shaped carbon of Experimental Example 4 is replaced with the conventionally used black iron oxide (spherical, average particle size 2 μm). Specifically, in Comparative Example 2, black iron oxide was used for the A phase of Experimental Example 4, and other eyelash cosmetics were prepared in the same manner as in Experimental Example 4.

(Experimental Examples 5-8, Comparative Examples 3 and 4)
In order to evaluate the effect of this embodiment also in oil-based eyelash cosmetics, in Experimental Examples 5 to 8 and Comparative Examples 3 and 4, the underwater oil-type eyelash makeup of Experimental Examples 1 to 4 and Comparative Examples 1 and 2 are used. Ingredients other than the A phase of the agent were replaced with oily eyelash cosmetics, and the same preparation was performed, and the performance was evaluated according to the above evaluation method.

The components of the oily eyelash cosmetics having the composition shown in FIG. 11 were adjusted according to the following manufacturing procedure. The composition and blending amount of the B phase to E phase of the eyelash cosmetics shown in FIG. 11 (Experimental Examples 5 to 8, Comparative Examples 3 and 4) are the same as those of FIG. 5 of the first embodiment.

The B-phase mixture shown in FIG. 11 was heated to 90 ° C. and mixed with a homogenizer for 30 minutes. The composition of phase A and phase C was added to the mixture of phase B, and the mixture was again mixed with a homogenizer for 30 minutes. Then, the obtained mixture was added with the components of the D phase and the E phase at 50 ° C. and uniformly mixed with a homogenizer for 30 minutes to obtain an oily eyelash cosmetic.

Looking at the evaluations of Experimental Examples 5 to 8 and Comparative Examples 3 and 4 in FIG. 11, the eyelash cosmetics of Experimental Examples 5 to 8 had a curl-keeping effect, a long rush effect, a volume-up effect, a feeling of application, and a make-up lasting. It was superior to Comparative Examples 3 and 4 in all of the stability over time. As can be seen from this result, even in the oil-based eyelash cosmetics, the eyelash cosmetics containing rod-shaped carbon of the present embodiment can produce eyelash cosmetics with a small pigment ratio, and synthetic fibers can be produced. Even if it does not contain, it exhibits remarkably excellent curl keeping effect, long lash effect, volume up effect, application comfort, makeup retention, and stability over time.

The components of the water-in-oil type eyelash cosmetics having the composition shown in FIG. 12 were adjusted according to the following manufacturing procedure. The composition and blending amount of the B-phase to G-phase of the eyelash cosmetics shown in FIG. 12 (Experimental Examples 5 to 8, Comparative Examples 3 and 4) are the same as those in FIG. 6 of the first embodiment.

The B-phase mixture shown in FIG. 12 is heated to 95 ° C., the C-phase mixture is heated to 85 ° C., and the heated B-phase and C-phase and the A-phase are stirred with a homogenizer for 30 minutes to obtain the B-phase and C-phase. It was emulsified and the A phase was ground and dispersed. The obtained mixture was cooled to 40 ° C. with stirring, the components of D phase, E phase, F phase and G phase were added, and the mixture was mixed with a homogenizer for 30 minutes. The homogeneous mixture was cooled to 32 ° C. in the air to obtain a water-in-oil type eyelash cosmetic.

Looking at the evaluations of Experimental Examples 9 to 12 and Comparative Examples 5 and 6 in FIG. 12, the eyelash cosmetics of Experimental Examples 9 to 12 have a curl-keeping effect, a long rush effect, a volume-up effect, a feeling of application, and a make-up lasting. It was superior to Comparative Examples 5 and 6 in all of the stability over time. As can be seen from this result, even in the water-in-oil type eyelash cosmetics, the eyelash cosmetics containing rod-shaped carbon of the present embodiment can produce eyelash cosmetics with a small pigment ratio. Even if it does not contain synthetic fibers, it exhibits remarkably excellent curl-keeping effect, long lash effect, volume-up effect, application comfort, makeup retention, and stability over time.

The cosmetic for eyebrows of the present embodiment described above contains rod-shaped carbon obtained by crushing co-continuous fibrous carbon having a three-dimensional network structure in which carbon is branched, and the co-continuous fibrous carbon is cellulose nanofibers. Made from.

The eyelash cosmetic of the present embodiment uses rod-shaped carbon as a pigment, and the rod-shaped carbon is oriented in the direction of the eyelashes, resulting in excellent curl-keeping effect, long rush effect, volume-up effect, and application. Elongation (feeling of application) and adhesive strength (makeup lasting) can be obtained.

Further, in the present embodiment, the rod-shaped carbon is uniformly dispersed in the eyelash cosmetics without forming a bundle. That is, in the present embodiment, the rod-shaped carbon is uniformly dispersed in the dispersion medium, so that the blending ratio of the pigment can be lowered, and even when synthetic fibers are not contained, the curl-keeping effect, the long lash effect, and the effect can be reduced. It is possible to provide eyelash cosmetics that have a volume-increasing effect, elongation during application (applying comfort), and adhesive strength (makeup retention).

Further, in the present embodiment, by using rod-shaped carbon obtained by crushing co-continuous fibrous carbon produced from cellulose nanofibers derived from natural products, cosmetics for eyelashes composed of raw materials having a low environmental load are manufactured. It becomes possible to do.

The present invention is not limited to the above embodiment, and various modifications and combinations are possible within the technical idea of the present invention.

S1: Dispersion process S2: Freezing process S3: Drying process S4: Carbonization process S5: Grinding process S6: Mixing process

Claims

It ’s a makeup for eyelashes.
As a pigment, it contains co-continuous fibrous carbon having a three-dimensional network structure in which carbon is branched.
The co-continuous fibrous carbon is a cosmetic for eyelashes made from cellulose nanofibers.
The eyelash cosmetic according to claim 1, wherein the blending amount of the co-continuous fibrous carbon is 5% by mass or less of the eyelash cosmetic.
It ’s a makeup for eyelashes.
The pigment contains rod-shaped carbon obtained by crushing co-continuous fibrous carbon having a three-dimensional network structure in which carbon is branched.
The co-continuous fibrous carbon is a cosmetic for eyelashes made from cellulose nanofibers.
The eyelash cosmetic according to claim 3, wherein the amount of the rod-shaped carbon compounded is 5% by mass or less of the eyelash cosmetic.
The cosmetic for eyelashes according to any one of claims 1 to 4, which does not contain synthetic fibers.
The cosmetic for eyelashes according to any one of claims 1 to 5, wherein the co-continuous fibrous carbon has a color according to the progress of carbonization.