JP2021054719A - Emulsified composition obtained by effectively dispersing powder - Google Patents

Abstract

To provide a method for producing an emulsified composition used for a skin external preparation and a cosmetic, which has sufficient dispersibility, no stickiness and good sense of use.SOLUTION: There is provided a method for producing an emulsified composition comprising a biosurfactant, water and/or a polyhydric alcohol, an oily component and a powder having an average particle diameter of 1.0 mm or less, which comprises a first step of mixing a biosurfactant, water and/or a polyhydric alcohol, an oily component to obtain a first composition and a second step of mixing a mixture of a biosurfactant, water and/or a polyhydric alcohol and a powder having an average particle diameter of 1.0 mm or less in the first composition. Preferably, the biosurfactant is one or more selected from surfactin, arthrofactin and iturin or a salt thereof and the polyhydric alcohol is one or more selected from glycerol, sorbitol, xylitol, diglycerol or polyethylene glycol.SELECTED DRAWING: None

Description

The present invention is characterized by containing biosurfactant, and relates to a powder-dispersed external preparation for skin and a cosmetic.

Various dosage forms have been developed for cosmetics, and among them, sunscreen cosmetics have long been used to prevent the skin from being exposed to excessive ultraviolet rays and causing inflammation. It is used. In recent years, it has become known that even ultraviolet rays that are exposed to daily life cause stains, freckles, wrinkles due to photoaging, and skin cancer due to genetic damage to skin cells. Experts such as physicians recommend that skin be protected from UV rays on a daily basis. In response to this, many cosmetics such as lotions, milky lotions, creams, and foundations are now provided with an ultraviolet protection function. Substances having an ultraviolet protection function include organic substances that absorb ultraviolet rays and inorganic substances that scatter ultraviolet rays, but inorganic substances that are considered to be highly safe are relatively preferred. Typical ultraviolet scattering agents include powdered titanium oxide and zinc oxide, but there is a problem that they are difficult to disperse in the cosmetic base as they are. Therefore, various methods for improving dispersibility have been studied so far (Patent Document 1).

Special Fair 1-57084 Gazette

As in Patent Document 1, a method for improving dispersibility has been studied, but the dispersibility is still not sufficient in many cases, and when a dispersion aid is used, the dispersion aid has a peculiar stickiness and a large amount. In many cases, it is necessary to mix it with the above, and there is a problem that the usability is deteriorated.

As a result of diligent studies to solve the above-mentioned problems, the present inventors, as a first step, a step of mixing a biosurfactant and an oily component to obtain a mixture, and a second step of obtaining an emulsified composition. , A mixture of a biosurfactant, an aqueous component and a powder having an average particle size of 1.0 mm or less is mixed with the mixture obtained in the first step to obtain a powder having an average particle size of 1.0 mm or less. We have found that it is possible to obtain an emulsified composition having low irritation and high emulsification stability in which the above-mentioned substances are effectively dispersed, and have completed the present invention.

That is, the present invention
(1). A method for producing an emulsified composition containing a biosurfactant, water and / or polyhydric alcohol, an oily component, and a powder having an average particle size of 1.0 mm or less, which comprises the following first and second steps. Method of manufacturing the composition,
First step: A step of mixing biosurfactant with water and / or polyhydric alcohol and an oily component to obtain a first composition. Second step: Biosurfactant and water and / or polyhydric alcohol with an average particle size of 1. Step of mixing a mixture of powders of 0 mm or less with the first composition (2). The method for producing an emulsified composition according to (1), wherein the biosurfactant is one or more selected from the group consisting of surfactin and arslovactin, itulin, or salts thereof.
(3). The method for producing an emulsified composition according to (1) or (2), wherein the polyhydric alcohol is at least one selected from the group consisting of glycerin and sorbitol, xylitol, diglycerin, and polyethylene glycol. ,
(4). The method for producing an emulsified composition according to any one of (1) to (3), wherein the powder is a scattering agent.
(5). A method for producing an external preparation for skin using the method for producing an emulsified composition according to any one of (1) to (4).
(6). A method for producing a cosmetic product using the method for producing an emulsified composition according to any one of (1) to (4).
Regarding.

It is possible to effectively disperse a powder having an average particle size of 1.0 mm or less, and obtain an emulsified composition that is well-adapted to the skin and has a smooth feeling of use, yet is hypoallergenic and has high emulsion stability.

The emulsified composition of the present invention contains biosurfactant. A biosurfactant is a natural compound produced by a microorganism, and is generally highly biodegradable and has low skin irritation to the human body, so that it is extremely stable to the environment and the human body. Biosurfactants used in the present invention include the lipopeptide compounds surfactin, arsofactin, itulin, glycolipids mannosyl erythritol lipid and sophorolipid, trehalose lipid, ramnolipid, fatty acid spicrysporic acid, polymer emalzan, etc. Salt, but is not limited to these.

Among the above, since the effect of stabilizing the emulsified composition can be obtained with a small amount, the lipopeptide compound surfactin, arslovactin, itulin, or a salt thereof is preferable, and surfactin or a salt thereof is particularly preferable.

Here, the salt of surfactin is the general formula (1).

[In the formula, X represents an amino acid residue selected from leucine, isoleucine and valine, R represents a C9-18 alkyl group and M + represents an alkali metal ion or a quaternary ammonium ion].
It is a compound represented by, or a composition containing two or more kinds of this compound.

The amino acid residue as X may be L-form or D-form, but L-form is preferable.

The "C9-18 alkyl group" refers to a linear or branched monovalent saturated hydrocarbon group having 9 or more carbon atoms and 18 or less carbon atoms. For example, n-nonyl group, 6-methyloctyl group, 7-methyloctyl group, n-decyl group, 8-methylnonyl group, n-undecyl group, 9-methyldecyl group, n-dodecyl group, 10-methylundecyl group. , N-Tridecyl group, 11-methyldodecyl group, n-tetradecyl group, n-pentadecyl group, n-hexadecyl group, n-heptadecyl group, n-octadecyl group and the like.

The alkali metal ion is not particularly limited, but represents lithium ion, sodium ion, potassium ion and the like.

Examples of the substituent of the quaternary ammonium ion include an alkyl group such as a methyl group, an ethyl group, an n-propyl group, an isopropyl group, an n-butyl group and a tert-butyl group; a benzyl group, a methylbenzyl group and a phenylethyl group. Aralkyl groups such as groups; organic groups such as aryl groups such as phenyl group, toluyl group and xsilyl group can be mentioned. Examples of the quaternary ammonium ion include tetramethylammonium ion, tetraethylammonium ion, pyridinium ion and the like.

The above surfactin or a salt thereof may be used alone or in combination of two or more.

Surfactin or a salt thereof can be used by culturing a microorganism, for example, a strain belonging to Bacillus subtilis, and separating it from the culture solution according to a known method. You can also do it. Further, those obtained by a chemical synthesis method can also be used in the same manner.

The concentration of the biosurfactant of the present invention is preferably 0.01% by weight to 10% by weight, preferably 0.05% by weight to 6% by weight, and more preferably 0.1% by weight to 4% by weight. If the concentration of biosurfactant is less than 0.01% by weight, the storage stability of the emulsified composition will be insufficient, and if it is more than 10% by weight, excess biosurfactant may adversely affect the usability. ..

The emulsified composition of the present invention contains water and / or a polyhydric alcohol. The polyhydric alcohol is not particularly limited, but it is preferable to use any one or more of glycerin, sorbitol, xylitol, diglycerin, and polyethylene glycol.

The concentration of water and / or polyhydric alcohol of the present invention is preferably 0.1% by weight to 50% by weight, preferably 1.0% by weight to 40% by weight. When water and / or the polyhydric alcohol is in the above concentration range, it is possible to form an emulsified composition having excellent stability.

The emulsified composition of the present invention contains an oily component. The oily component of the present invention is not particularly limited as long as it is not mixed with water in an arbitrary ratio, but is squalane, liquid paraffin, light liquid isoparaffin, ceresin, polyethylene powder, squalane, microcrystallin wax, vaseline, liquid isoparaffin. , Polybutene, hydrocarbons such as mineral oil, waxes such as beeswax, carnauba wax, candelilla wax, jojoba oil, lanolin, whale wax, macadamia nut oil, olive oil, cottonseed oil, soybean oil, avocado oil, rice bran oil, rice oil, Oils and fats such as rice germ oil, palm kernel oil, castor oil, rose hip oil, evening primrose oil, camellia oil, horse oil, grape seed oil, palm oil, meadow home oil, shea butter, corn oil, saflower oil, sesame oil, etc. , Ethylhexyl palmitate, isononyl isononanoate, isopropyl myristate, ethyl oleate, tri (capric acid / capric acid) glyceryl, cetyl 2-ethylhexanoate, glyceryl tri 2-ethylhexanoate, diisopropyl sebacate, cholesteryl hydroxystearate Esters such as, myristic acid, stearic acid, fatty acids such as oleic acid, silicone oils such as methylpolysiloxane, methylphenylpolysiloxane, amino-modified silicone, higher alcohols such as cetanol and oleyl alcohol, bacil alcohol, Kimi It is preferable to use any one or more of alkyl glyceryl ethers such as rualcohol.

The concentration of the oily component of the present invention is preferably 30% by weight to 99% by weight, preferably 40% by weight to 95% by weight. When the oily component is in the above concentration range, a gel-like composition having excellent stability can be obtained.

The emulsified composition of the present invention may contain any component as long as the effects of the present invention are achieved. Optional components include lower alcohols such as ethanol, isopropyl alcohol; anionic surfactants, cationic surfactants, amphoteric surfactants, thickeners, UV absorbers, antioxidants, emollients, etc. Examples thereof include emulsifiers, solubilizers, anti-inflammatory agents, moisturizers, preservatives, bactericides, pigments, fragrances, powders and the like.

The emulsified composition of the present invention can be prepared, for example, by dissolving biosurfactant in water and / or polyhydric alcohol and adding the above oily component little by little with stirring. When water and a polyhydric alcohol are used in combination, water may be added after the oily component is added.

The oily component may be added in predetermined amounts (divided addition) or continuously (continuously added).

In the case of partial addition, 60% by mass or less, preferably 30% by mass or less, more preferably 10% by mass or less of the amount of water and / or polyhydric alcohol already added is added at one time and stirred. To make it uniform. The required amount is added by repeating this.

In the case of continuous addition, the addition rate is 60% by mass or less, preferably 30% by mass or less, and more preferably 10% by mass or less of the amount of water and / or polyhydric alcohol already added. ..

When other components are added, they may be added before the oil component is added, dissolved or dispersed in the oil component, or added after the entire amount of the oil component is added. It does not matter which method is used even if it is added in the middle of adding. Water and / or polyhydric alcohol may be added in full at the beginning, or part of the amount added may be used first and the rest may be added later.

The liquid composition of the present invention contains biosurfactant, a powder having an average particle size of 1.0 mm or less, an aqueous component, and an oily component.

The powder having an average particle diameter of 1.0 mm or less of the present invention is not particularly limited, but is a scattering agent such as fine particle titanium oxide and fine particle zinc oxide, Red No. 104, Red No. 201, Yellow No. 4, Blue No. 1. Pigments such as Black No. 401, Yellow No. 4 Al Lake, Yellow No. 203 Ba Lake and other rake pigments, Nylon powder, Silk powder, Urethane powder, Tetrafluoroethylene powder, Silicone powder, Polymethyl methacrylate powder, Cellulose powder, Silicone Elastomer spherical powder, polyethylene powder, polymers such as acrylic resin, colored pigments such as yellow iron oxide, red iron oxide, black iron oxide, chromium oxide, carbon black, ultramarine blue, dark blue, zinc oxide, titanium oxide, cerium oxide, etc. White pigments, talc, mica, sericite, kaolin, plate-shaped barium sulfate, plate-shaped zinc oxide, extender pigments such as synthetic mica, pearl pigments such as mica titanium, barium sulfate, calcium carbonate, magnesium carbonate, aluminum silicate, silicic acid. It is preferable to use any one or more of a metal salt such as magnesium, an inorganic powder such as silica and alumina, bentonite, smectite, and boron nitride. Shape of these powders (spherical, rod-shaped, needle-shaped, plate-shaped, amorphous, fluffy, spindle-shaped, etc.), size, presence or absence of organic or inorganic surface treatment (for example, aluminum oxide treatment, dioxide There are no particular restrictions on silicon treatment, zirconium oxide treatment, ester treatment, alkyl treatment, fatty acid treatment, etc.).

In the present invention, a laser diffraction measurement method is used as a method for measuring the average particle size of powder. The average particle size of the powder is not particularly limited as long as it is 1.0 mm or less, but is preferably 0.01 μm to 0.5 mm (500 μm), more preferably 0.1 μm to 100 μm, and even more preferably 1 μm to 50 μm. For fine titanium oxide powder, etc., the particle size of each titanium oxide particle (primary particle size) and the particle size of agglomerates in which each particle is agglomerated (secondary particle size) are determined. However, the average particle size of the present invention uses the average particle size of the secondary particle size.

The concentration of the powder of the present invention is preferably 0.1% by weight to 50% by weight, preferably 1.0% by weight to 40% by weight. When the powder is in the above concentration range, it is possible to form a liquid composition having excellent stability and usability.

First Step The first step of the present invention is a step of mixing biosurfactant with water and / or a polyhydric alcohol and an oily component to obtain a first composition. The order of mixing is not particularly limited, but it can be prepared, for example, by dissolving biosurfactant in an aqueous component and adding the oily component little by little while stirring. The biosurfactant may be added little by little or all at once, and the addition time is preferably 0.1 seconds to 10 minutes because the addition does not take too much time. The oily component may be added little by little or all at once. The addition time is preferably 0.1 seconds to 10 minutes because the addition does not take too much time. After adding the entire amount of the oily component, it is preferable to further stir for about 1 to 30 minutes in order to stabilize the emulsified state.

The temperature at the time of mixing in the first step is not particularly limited, and is preferably 5 to 80 ° C, more preferably 10 to 50 ° C, still more preferably 15 to 40 ° C, and most preferably 20 to 30 ° C. When the mixing temperature is 80 ° C. or lower, deterioration of surfactin and oily components is small, which is preferable. The mixed atmosphere of the first step is not particularly limited, and examples thereof include an air atmosphere, a nitrogen atmosphere, and an argon atmosphere, but the air atmosphere is preferable because it is economical.

Second Step The second step of the present invention is a step of mixing a mixture of biosurfactant, water and / or polyhydric alcohol, and a powder having an average particle size of 1.0 mm or less into the first composition.

The mixing order of the biosurfactant, water and / or polyhydric alcohol, and powder is not particularly limited. For example, the biosurfactant is dissolved in water and / or polyhydric alcohol, and the powder is mixed with stirring. preferable. The biosurfactant may be added little by little or all at once, and the addition time is preferably 0.1 seconds to 10 minutes because the addition does not take too much time. The powder may be added little by little or all at once. The addition time is preferably 0.1 seconds to 10 minutes because the addition does not take too much time. After adding the entire amount of the powder, it is preferable to further stir for about 1 to 30 minutes in order to stabilize the emulsified state. The temperature at the time of mixing is not particularly limited, and is preferably 5 to 80 ° C, more preferably 10 to 50 ° C, still more preferably 15 to 40 ° C, and most preferably 20 to 30 ° C. When the mixing temperature is 80 ° C. or lower, deterioration of surfactin and oily components is small, which is preferable. The atmosphere at the time of mixing is not particularly limited, and examples thereof include an air atmosphere, a nitrogen atmosphere, and an argon atmosphere, but the air atmosphere is preferable because it is economical.

The method for mixing the biosurfactant with a mixture of water and / or polyhydric alcohol and powder into the first composition is not particularly limited, but the method containing the powder or the like while stirring the first composition is described above. It is preferable to mix the mixture. The mixture containing powder or the like may be added little by little or all at once, and the addition time is preferably 0.1 seconds to 10 minutes because the addition does not take too much time. After adding the entire amount of the mixture containing powder or the like, it is preferable to further stir for about 1 to 30 minutes in order to stabilize the emulsified state. The temperature at the time of mixing is not particularly limited, and is preferably 5 to 80 ° C, more preferably 10 to 50 ° C, still more preferably 15 to 40 ° C, and most preferably 20 to 30 ° C. When the mixing temperature is 80 ° C. or lower, deterioration of surfactin and oily components is small, which is preferable. The atmosphere at the time of mixing is not particularly limited, and examples thereof include an air atmosphere, a nitrogen atmosphere, and an argon atmosphere, but the air atmosphere is preferable because it is economical.

When other components are added, they may be added before the oil component is added, dissolved or dispersed in the oil component, or added after the entire amount of the oil component is added. It does not matter which method is used even if it is added in the middle of adding. The total amount of the aqueous component may be added first, or a part of the added amount may be used first and the rest may be added later.

The emulsified composition of the present invention is prepared, for example, as follows, but the present invention is not limited thereto.

(Example 1)
(A) Sodium surfactin 0.8% by weight
(B) Glycerin 20% by weight
(C) Squalane 20% by weight
(D) Purified water 1% by weight
Glycerin was added to sodium surfactin and dissolved by stirring to obtain a surfactin solution. Squalane was gradually added to the surfactin solution with stirring, and then purified water was gradually added with stirring to obtain a gel-like composition (E).
(F) Sodium surfactin 0.2% by weight
(G) Purified water 43% by weight
(H) Titanium oxide 15% by weight
Purified water was added to sodium surfactin and dissolved by stirring to obtain a surfactin solution. Titanium oxide (manufactured by Titan Kogyo Co., Ltd., ST-455WS) was gradually added to the surfactin solution with stirring to obtain a liquid composition (I).

An emulsified composition was prepared by adding the liquid composition (I) to the gel composition (E) and stirring the mixture.

(Example 2)
(A) Sodium surfactin 0.2% by weight
(B) Glycerin 20% by weight
(C) Squalane 5% by weight
(D) Purified water 1% by weight
Glycerin was added to sodium surfactin and dissolved by stirring to obtain a surfactin solution. Squalane was gradually added to the surfactin solution with stirring, and then purified water was gradually added with stirring to obtain a gel-like composition (E).
(F) Sodium surfactin 0.1% by weight
(G) Purified water 63.7% by weight
(H) Titanium oxide 10% by weight
Purified water was added to sodium surfactin and dissolved by stirring to obtain a surfactin solution. Titanium oxide was gradually added to the surfactin solution with stirring to obtain a liquid composition (I).

An emulsified composition was prepared by adding the liquid composition (I) to the gel composition (E) and stirring the mixture.

(Comparative Example 1)
In Example 1, the component (C) was gradually added to a mixture other than the component (C) with stirring to prepare an emulsified composition.

(Comparative Example 2)
(A) Sodium surfactin 1% by weight
(B) Glycerin 20% by weight
(C) Squalane 20% by weight
(D) Purified water 1% by weight
Glycerin was added to sodium surfactin and dissolved by stirring to obtain a surfactin solution. Squalane was gradually added to the surfactin solution with stirring, and then purified water was gradually added with stirring to obtain a gel-like composition (E).
(F) Purified water 43% by weight
(G) Titanium oxide 15% by weight
Titanium oxide was gradually added to purified water with stirring to obtain a liquid composition (H).
An emulsified composition was prepared by adding the liquid composition (H) to the gel composition (E) and stirring the mixture.

<Usage evaluation>
On the day when the emulsified composition was prepared for the above Examples and Comparative Examples, the five sensory evaluation panels gave the following points for smoothness, non-greasiness, and non-stickiness, and the total was used as the evaluation point. .. It was judged by the following criteria.

<Smoothness score>
2 points: Smooth after application 1 point: Slightly smooth after application 0 points: Not smooth after application <No roughness>
2 points: No roughness after application 1 point: No roughness after application 0 points: Roughness after application <No stickiness score>
2 points: Not sticky after application
1 point: Not slightly sticky after application 0 point: Sticky after application <Usage evaluation criteria>
○: Total 10 to 8 points ・ ・ ・ Good △: Total 7 to 5 points ・ ・ ・ Slightly good ×: Total 4 points or less ・ ・ ・ Bad <Stability evaluation>
The appearance of the above-mentioned Examples and Comparative Examples after being allowed to stand at 50 ° C. for 4 weeks was evaluated. The results are shown in Tables 1-3. In the examples, the oil was not separated and was stable, but in the comparative example, oil separation was observed.

<Stability evaluation criteria>
〇: No separation (maintaining the emulsified composition)
Δ: Slightly separated (slight oil exudation or suspected)
×: Separation (oil is recommended)

Claims (6)

A method for producing an emulsified composition containing a biosurfactant, water and / or polyhydric alcohol, an oily component, and a powder having an average particle size of 1.0 mm or less, which comprises the following first and second steps. Method for producing the composition.
First step: A step of mixing biosurfactant with water and / or a polyhydric alcohol and an oily component to obtain a first composition.
Second step: A step of mixing a mixture of biosurfactant, water and / or polyhydric alcohol, and a powder having an average particle size of 1.0 mm or less into the first composition. The method for producing an emulsified composition according to claim 1, wherein the biosurfactant is one or more selected from the group consisting of surfactin and arslovactin, itulin, or salts thereof. The method for producing an emulsified composition according to claim 1 or 2, wherein the polyhydric alcohol is at least one selected from the group consisting of glycerin and sorbitol, xylitol, diglycerin, and polyethylene glycol. The method for producing an emulsified composition according to any one of claims 1 to 3, wherein the powder is a scattering agent. A method for producing an external preparation for skin using the method for producing an emulsified composition according to any one of claims 1 to 4. A method for producing a cosmetic using the method for producing an emulsified composition according to any one of claims 1 to 4.