JP6860297B2 - Oil-in-water emulsified external preparation composition - Google Patents

Description

The present invention relates to an oil-in-water emulsified external preparation composition (for example, an oil-in-water emulsified cosmetic).

The oil-in-water emulsified external preparation composition in which the continuous phase is the aqueous phase is used for various purposes such as cosmetics, pharmaceuticals, and quasi-drugs. In general, an oil-in-water emulsified external preparation composition is intended to improve its emulsification stability by adding a water-soluble polymer to the aqueous phase to increase the viscosity of the external preparation composition.
As the water-soluble polymer used in the oil-in-water emulsified external preparation composition, for example, xanthan gum, carboxyvinyl polymer and the like are known (Patent Document 1). However, since xanthan gum has a peculiar sliminess (spinning property), it is difficult to say that the oil-in-water emulsified external preparation composition using a sufficient amount of xanthan gum that can maintain emulsion stability has a good usability (for example). , Slimy, poor slipperiness during application, increased stickiness, etc.). Further, the oil-in-water emulsified external preparation composition having a high viscosity has a problem that it is difficult to get out of the container.
Compared to xanthan gum, carboxyvinyl polymer has the advantage of being less slimy and sticky, but when a sufficient amount of carboxyvinyl polymer that can maintain emulsion stability is used, it becomes highly viscous and reminds us of a fresh feeling of use. It is difficult to prepare an oil-in-water emulsified external preparation composition in such a form. Further, the carboxyvinyl polymer has a problem that when an electrolyte coexists, the viscosity is significantly lowered and the emulsion stability cannot be maintained.

On the other hand, as a technique for using fermented cellulose or cellulose nanofibers in cosmetics, for example, a method of preventing stickiness of cosmetics by adding fermented cellulose (Patent Document 2), and organic cosmetics containing cellulose nanofibers (Patent Documents). 3) etc. have been reported.

Japanese Unexamined Patent Publication No. 2014-73991 Japanese Unexamined Patent Publication No. 2009-96769 Japanese Unexamined Patent Publication No. 2015-157996

An object of the present invention is to provide an oil-in-water emulsified external preparation composition having a viscosity at 25 ° C. of 1000 mPa · s or less, which is extremely low in viscosity as compared with a conventional oil-in-water emulsified external preparation composition. As a result, we focused on fermented cellulose and cellulose nanofibers. However, when an oil-in-water emulsified external preparation composition having a viscosity at 25 ° C. of 1000 mPa · s or less is prepared using fermented cellulose and / or cellulose nanofibers, water is separated over time and the entire phase becomes uniform. It was found that a suitable composition could not be provided, and that a part of the composition gels when the content is increased.

The present invention has been made in view of the new findings, and although the viscosity at 25 ° C. is as low as 1000 mPa · s or less, the separation of water generated over time is suppressed and the emulsion stability is improved. An object of the present invention is to provide an excellent oil-in-water emulsified external preparation composition. Another object of the present invention is to provide an oil-in-water emulsified external preparation composition having an improved usability.

The present inventor has made various studies on oil-in-water emulsified external preparation compositions containing fermented cellulose and / or cellulose nanofibers and having a viscosity at 25 ° C. of 1000 mPa · s or less. In addition, by using a specific amount of xanthan gum and / or welan gum in combination with these celluloses, the above-mentioned problems are solved, and despite the low viscosity, the emulsion stability is excellent and the usability is also excellent in water. We have found that we can provide an oil-type emulsified external preparation composition, and have arrived at the present invention.

That is, the present invention has the following aspects;
Item 1. Fermented cellulose and / or cellulose nanofibers, and
Contains xanthan gum and / or welan gum and
An oil-in-water emulsified external preparation composition that satisfies the following conditions (A) and (B);
(A) The content of the xanthan gum and / or welan gum is 0.1 to 15 parts by mass with respect to 1 part by mass of the fermented cellulose and / or cellulose nanofiber (however, a complex containing xanthan gum is used as the fermented cellulose. If so, the xanthan gum content contained in the complex is excluded),
(B) The viscosity of the B-type rotational viscometer at 25 ° C. at 30 rpm is 1000 mPa · s or less.
Item 2. Item 2. The oil-in-water emulsified external preparation composition according to Item 1, wherein the external preparation composition is a cosmetic.
Item 3. Item 2. The method for producing an oil-in-water emulsified external preparation composition according to Item 1 or 2, which comprises the following steps;
Fermented cellulose and / or cellulose nanofibers, and
Steps of preparing an aqueous phase containing xanthan gum and / or welan gum,
The process of preparing the oil phase,
A step of mixing and emulsifying the aqueous phase and the oil phase.
Item 4. Item 3. The method for producing an oil-in-water emulsified external preparation composition according to Item 3.
At least before the process of emulsifying the aqueous and oil phases,
A method comprising a step of homogenizing the fermented cellulose in the presence of water.

According to the present invention, although the viscosity at 25 ° C. is as low as 1000 mPa · s or less, the separation of water generated over time is suppressed, and an oil-in-water emulsified external preparation composition having excellent emulsion stability can be obtained. Can be provided. Further, the oil-in-water emulsified external preparation composition of the present invention has an advantage that it is excellent in usability.

(Oil-in-water emulsified external preparation composition)
The oil-in-water emulsified external preparation composition targeted by the present invention is an O / W type emulsified composition in which the continuous phase is the aqueous phase and the dispersed phase is the oil phase. The external preparation composition targeted by the present invention refers to a composition used by applying it to the exodermis (skin), hair, oral mucosa, intranasal mucosa, etc., and the purpose of use is not particularly limited, and it can be used for various purposes. Can be used.
For example, it can be used for pharmaceuticals, quasi-drugs, cosmetics (cosmetics), etc., and a particularly preferable use is cosmetics. The type of composition is also not particularly limited, and the external preparation composition of the present invention is, for example, an external preparation, a spray agent, a cream agent, a mouthwash, an oral moisturizer, a mouth refreshing agent, an antiperspirant, and a dyeing agent. It can be used as a hair agent, a washing pigment, a cleansing agent, a lotion, a milky lotion, a beauty essence, a pack, a sunscreen, a makeup base, a foundation, an eye makeup, a shampoo, a conditioner, a hair mist, and the like.

(Fermented cellulose)
Fermented cellulose is cellulose produced by cellulose-producing bacteria (for example, bacteria belonging to the genus Acetobacter, Pseudomonas, Acrobacterium, etc.). Fermented cellulose has a very fine fiber diameter as compared with the fiber diameter of general plant-derived cellulose fibers. On the other hand, its fiber length is long, and it is significantly different from crystalline cellulose obtained by obtaining only a pure crystalline region.

In the present invention, it is preferable to use a fermented cellulose complex complexed with another polymer substance as the fermented cellulose. The complex is substantially composed of fermented cellulose and other polymer substances, and is preferably a complex in which the other polymer substances are attached to the surface of the fermented cellulose fibers. By adhering other polymer substances to the surface of the fermented cellulose fibers in this way, when the fermented cellulose composite is added to the aqueous phase, the fermented cellulose fibers are easily loosened, so that the composition of the oil-in-water emulsified external preparation The emulsification stability of the product can be further improved.

The method for synthesizing the fermented cellulose is not particularly limited and can be carried out according to a conventional method. For example, a method of mixing a liquid containing fermented cellulose with a solution of another polymer substance, and then obtaining a fermented cellulose complex by alcohol precipitation using isopropyl alcohol or the like, spray drying, or the like, a gel of fermented cellulose. Is immersed in a solution of another polymer substance, or a method disclosed in JP-A-09-121787, specifically, another polymer substance in a medium used in culturing a fermented cellulose-producing microorganism. Fermented cellulose can be compounded by using a method of adding the above. If desired, the fermented cellulose complex can be dried to obtain a dry powder.

The other polymer substance used for such complexing is not particularly limited as long as it is a water-soluble polysaccharide. For example, galactomannan (eg, guar gum, locust bean gum, tara gum, etc.), xanthan gum, carboxymethyl cellulose, sodium carboxymethyl cellulose, carboxymethyl cellulose calcium, tamarind seed gum, pectin, tragant gum, karaya gum, carrageenan, agar, alginic acid, alginate, gellan gum. , Carrageenan, pullulan, psyllium seed gum, glucomannan, chitin, chitosan, dextrin, starch and the like. The preferred polymeric substance is one or more selected from the group consisting of carboxymethyl cellulose, sodium carboxymethyl cellulose, calcium carboxymethyl cellulose, xanthan gum and guar gum.

The dry powder of the fermented cellulose complex is commercially available, for example, "Sun Artist [registered trademark] H-PN" and "Sun Artist [registered trademark] PN" manufactured by San-Ei Gen FFI Co., Ltd. , "Sun Artist [Registered Trademark] H-PG", "Sun Artist [Registered Trademark] PG" and the like.
Among the above-mentioned preparations, "Sun Artist [registered trademark] H-PN" and "Sun Artist [registered trademark] PN" are preparations containing a fermented cellulose complex of fermented cellulose, sodium carboxymethyl cellulose and xanthan gum, and "Sun Artist". [Registered Trademark] H-PG and "Sun Artist [Registered Trademark] PG" are formulations containing a fermented cellulose complex of fermented cellulose, sodium carboxymethyl cellulose and guar gum.

(Cellulose nanofiber)
Cellulose nanofibers are cellulose obtained by refining plant fibers to nano size, and have a fiber width of about 1 to 100 nm and an aspect ratio of about 100 or more. The origin of the plant fiber is not particularly limited, and various raw materials such as wood, straw (for example, wheat, rice, etc.), stem (for example, corn, cotton, etc.), sugar cane, bagasse, reeds, bamboo, etc. can be used.
The method for producing cellulose nanofibers is not particularly limited. For example, a method of treating plant fibers from which lignin and hemicellulose have been removed with a refiner to cut the cell wall several times in the lateral direction and then kneading with a twin-screw kneader to defibrate a strong secondary wall, a high-pressure homogenizer, etc. A method of defibrating with a microfluidizer or the like, by treating the cellulose raw material in the coexistence of TEMPO (2,2,6,6-tetramethyl-1-piperidin-N-oxyradical) and sodium hypochlorite. Various methods can be used, such as a method in which a carboxyl group is introduced into the surface of a cellulose microfibril and then the cellulose raw material into which the carboxyl group is introduced is treated in water with a mixer or the like.

The content of the fermented cellulose and / or cellulose nanofibers in the oil-in-water emulsified external preparation composition of the present invention is not particularly limited as long as the viscosity of the external preparation composition does not exceed 1000 mPa · s, but is preferable. The content is 0.005 to 1% by mass, more preferably 0.01 to 0.75% by mass, still more preferably 0.01 to 0.5% by mass, still more preferably 0.015 to 0.3% by mass. %.

(Xanthan gum)
Xanthan gum is a polysaccharide produced outside the cells of the genus Xanthmonas campestris. Xanthan gum is commercially available, for example, "San Ace [Registered Trademark]", "San Ace [Registered Trademark] C", "San Ace [Registered Trademark] NXG-S", manufactured by Saneigen FFI Co., Ltd. Examples include "San Ace [registered trademark] NXG-C".

(Wellangham)
Welan gum is a polysaccharide obtained from the culture medium of Alcaligenes, for example, a suitable aqueous having a carbon source, a nitrogen source and an inorganic salt source under controlled conditions by inoculation with Alcaligenes organism ATCC31555. It is produced by aerobic formation of a nutrient medium and can be obtained separately from the culture solution. Further, for example, it can be produced according to the method described in Japanese Patent Application Laid-Open No. 05-213650, US Pat. No. 4,342,866, and the like. Welan gum is commercially available, and examples thereof include "Bistop [registered trademark] W" manufactured by Saneigen FFI Co., Ltd.

(Condition A)
The oil-in-water emulsified external preparation composition of the present invention is characterized by containing a specific amount of xanthan gum and / or welan gum with respect to the fermented cellulose and / or cellulose nanofibers. Specifically, the xanthan gum and / or welan gum content is 0.1 to 15 parts by mass, preferably 0.2 to 12 parts by mass, more preferably 0. parts by mass with respect to 1 part by mass of the fermented cellulose and / or cellulose nanofiber. It is 25 to 11 parts by mass, and more preferably 0.3 to 10 parts by mass (however, when a fermented cellulose complex containing xanthan gum is used as the fermented cellulose, the xanthan gum content is excluded).
By using fermented cellulose and / or cellulose nanofibers in combination with xanthan gum and / or welan gum at the blending ratio, an oil-in-water emulsified external preparation composition having extremely excellent emulsion stability despite having a low viscosity is provided. can do. Further, since xanthan gum usually has a spinnability property, the external preparation composition containing xanthan gum may become slimy or sticky. However, according to the present invention, even when xanthan gum is contained in the oil-in-water emulsified external preparation composition, it is possible to provide an oil-in-water emulsified external preparation composition having an excellent usability, which is an unexpected effect.
On the other hand, when the content of xanthan gum and / or welan gum is less than 0.1 parts by mass with respect to 1 part by mass of fermented cellulose and / or cellulose nanofibers, water separation occurs over time, and the composition of an oil-in-water emulsified external preparation It adversely affects the quality of products (for example, the appearance is poor and the commercial value is reduced, the content components are not homogenized, and the active ingredients are not evenly distributed, etc.). Further, when the content of xanthan gum and / or welan gum exceeds 15 parts by mass with respect to 1 part by mass of fermented cellulose and / or cellulose nanofibers, the usability of the oil-in-water emulsified external preparation composition deteriorates.

The content of xanthan gum and / or welan gum in the oil-in-water emulsified external preparation composition of the present invention is not particularly limited as long as it is the above-mentioned compounding ratio, but the preferable content is 0.005 to 0.6% by mass, more preferably. It is 0.025 to 0.45% by mass, more preferably 0.05 to 0.3% by mass.

The oil-in-water emulsified external preparation composition of the present invention has a viscosity at 25 ° C. at 30 rpm of a B-type rotational viscometer of 1000 mPa · s or less, preferably less than 800 mP · s, more preferably 750 mPa · s or less, still more preferably. Is 700 mPa · s or less. The viscosity is determined by adjusting the product temperature of the oil-in-water emulsified external preparation composition to 25 ° C. and then measuring for 1 minute under the condition of a rotation speed of 30 rpm using a B-type rotational viscometer.
Normally, when the viscosity of the oil-in-water emulsified external preparation composition is lower than the above viscosity, it becomes difficult to suppress the separation of water generated over time. However, in the present invention, fermented cellulose and / or cellulose nanofibers and xanthan gum are used. And / or by using welan gum in combination at a specific ratio, it is possible to provide an oil-in-water emulsified external preparation composition having extremely excellent emulsion stability despite having a low viscosity. In addition, the viscosity of the oil-in-water emulsified external preparation composition is within the above range, and by using fermented cellulose and / or cellulose nanofibers in combination with xanthan gum and / or welan gum, the oil-in-water type is excellent in usability. An emulsified external preparation composition can be provided.
The lower limit of the viscosity of the oil-in-water emulsified external preparation composition of the present invention is not particularly limited, and examples thereof include 100 mPa · s or more, preferably 120 mPa · s or more, more preferably 150 mPa · s or more, and further preferably 200 mPa · s or more.・ It is s or more.

(Water phase)
The aqueous phase of the oil-in-water emulsified external preparation composition of the present invention is not particularly limited as long as it contains water. It may also contain water-soluble alcohols and / or polyhydric alcohols. Examples of the water-soluble alcohol include lower alcohols, and preferable carbon atoms of the lower alcohols are 5 or less, more preferably 4 or less, and further preferably 3 or less. Examples of such lower alcohols include ethanol, isopropanol and the like. Examples of the water-soluble polyhydric alcohol include glycerin, diglycerin, and glycol (for example, ethylene glycol, diethylene glycol, diethylene glycol monoalkyl ether, triethylene glycol, propylene glycol, dipropylene glycol, 1,3-butylene glycol, and hexylene. Glycerol, isoprene glycol, polyethylene glycol, etc.), sugar alcohols (for example, sorbitol, martitol, mannitol, xylitol, erythritol, etc.) and the like can be mentioned.
The oil-in-water emulsified external preparation composition of the present invention has a viewpoint that fermented cellulose and / or cellulose nanofibers and xanthan gum and / or welan gum are sufficiently dispersed or dissolved in a solvent to exert a function of stabilizing emulsification. Therefore, it is preferable that 40% by mass or more of the solvent in the aqueous phase is water, and more preferably 50% by mass or more of the solvent is water.

(Oil phase)
The oil phase of the oil-in-water emulsified external preparation composition of the present invention is not particularly limited, and various materials that can be used for the external preparation composition such as cosmetics can be used.
For example, fats and oils, higher alcohols, higher fatty acids, esters, hydrocarbons, lipophilic surfactants and the like can be mentioned.
Examples of fats and oils include rice bran oil, olive oil, soybean oil, rice germ oil, wheat germ oil, jojoba oil, sunflower oil, red flower oil, sunflower oil, olive oil, macadamia nut oil, avocado oil, flaxseed oil, almond oil, and palm oil. , Mink oil and the like.
Examples of the higher alcohol include those having 6 or more carbon atoms, and specifically, lauryl alcohol, cetanol (cetyl alcohol), cetearyl alcohol, stearyl alcohol, oleyl alcohol, behenyl alcohol, lanolin alcohol, and hexyldecanol (hexadecyl alcohol). ), Octyldodecanol, isostearyl alcohol and the like.
Examples of higher fatty acids include those having 12 or more carbon atoms, and specific examples thereof include lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, hydroxystearic acid, isostearic acid, oleic acid, undecylene acid, and d. Examples thereof include icosapentaenoic acid and docosahexaenoic acid.
Examples of the esters include isooctyl palmitate, isopropyl myristate, isopropyl palmitate, octyldodecyl myristate, glyceryl trioctanoate, diglyceryl diisostearate, diglyceryl triisostearate, glyceryl tribehenate, pentaerythrite rosinate, Examples thereof include neopentyl glycol dioctanoate, cholesterol fatty acid ester, di-lauroyl-L-glutamate (cholesteryl behenyl octyldodecyl) and the like.
Examples of hydrocarbons include liquid paraffin, petrolatum, squalane, polyisobutylene, polybuden, paraffin wax, selecin wax, microcrystalline wax, mokurou, and montan wax.
Examples of the lipophilic surfactant include glycerin fatty acid ester, polyglycerin fatty acid ester, propylene glycol fatty acid ester, sorbitan fatty acid ester, and sorbitol fatty acid ester, and alkylene glycol adducts, polyalkylene glycol fatty acid ester, and sucrose. Fatty acid ester, polysorbate 20, polysorbate 60, polysorbate 80, polyoxyalkylene alkyl ether, polyoxyethylene alkylphenyl ether, polyoxyethylene hydrogenated castor oil, PEG-40 hydrogenated castor oil, lanolin alkylene glycol adduct, fatty acid soaps (For example, those formed by fatty acids such as stearic acid, lauric acid, myristic acid, behenic acid, isostearic acid, oleic acid, 12-hydroxystearic acid and alkaline substances such as sodium, potassium and triethanolamine), acyl Glycerates, alkyl phosphates, polyoxyalkylene-added alkyl phosphates, alkylamine salts, alkyl quaternary ammonium salts, N, N-dimethyl-N-alkyl-N-carboxymethylammonium betaine, N, N-diaquil Aminoalkylene carboxylic acid, N, N, N-trialkyl-N-sorboalkylene ammonium betaine, N, N-diaquil-N, N-bis (polyoxyethylene sulfate) ammonium betaine, 2-alkyl-1-hydroxyethyl -1-carboxymethyl imidazolinium betanin, lecithin, phospholipid and the like can be mentioned.
In addition, oil-soluble vitamins (eg, vitamin A, vitamin E, etc.), fluorine-based oils (eg, perfluoropolyether, perfluorodecane, perfluorooctane, etc.), sterols (eg, cholesterol, phytosterol, etc.), wax Classes (eg, honeybee, mokuro, carnauba wax, etc.), lanolin derivatives (eg, lanolin, lanolin acetate, lanolin fatty acid isopropyl, lanolin alcohols, etc.), silicones (eg, low degree of polymerization dimethylpolysiloxane, high degree of polymerization dimethylpoly). Siloxane, methylphenylpolysiloxane, decamethylcyclopentasiloxane, octamethylcyclotetrasiloxane, polyether-modified silicone, crosslinked organopolysiloxane, fluorine-modified silicone, etc.), oil-soluble UV absorbers, oil-soluble fragrances, oil-soluble pigments, etc. Can be mentioned.

The content of the oil phase in the oil-in-water emulsified external preparation composition of the present invention is not particularly limited, but is preferably 0.1 to 30% by mass, more preferably 0.1 to 25% by mass, still more preferably 1 to 20% by mass. , 1 to 16% by mass is even more preferable.

In addition, the oil-in-water emulsified external preparation composition of the present invention includes powders such as inorganic powders, organic powders, pigment powders, and composite powders, pH adjusters, preservatives, chelating agents, and neutralizing agents. , Various materials such as medicinal ingredients can be contained.

The oil-in-water emulsified external preparation composition of the present invention may or may not contain an electrolyte (for example, salts, etc.), but the oil-in-water emulsified external preparation composition of the present invention may contain an electrolyte. Also has the feature of being excellent in emulsion stability. For example, the carboxyvinyl polymer conventionally used in the oil-in-water emulsification external preparation composition has a problem that the viscosity is significantly reduced in the coexistence of an electrolyte (for example, salts) and the emulsification stability cannot be maintained. .. However, when the oil-in-water emulsified external preparation composition of the present invention contains an electrolyte, the content of the electrolyte in the external preparation composition is 0.5% by mass or more, further 1% by mass or more, particularly 1.5. Even when it is as high as% by mass or more, it has an advantage of being excellent in emulsion stability. The upper limit of the content of the electrolyte in the oil-in-water emulsified external preparation composition of the present invention is not particularly limited, and examples thereof include 5% by mass or less, preferably 4% by mass or less.

The electrolyte is a substance that ionizes into cations and anions when dissolved in a solvent, and examples thereof include acids, bases, and salts.
As the acid, a water-soluble organic acid, an inorganic acid or the like that can be blended in the external preparation composition can be used. Similarly, as the base, a water-soluble base that can be blended in the external preparation composition can be used.
Examples of the salts include water-soluble salts that can be blended in the external preparation composition (for example, sodium salt, potassium salt, calcium salt, magnesium salt, ammonium salt, lithium salt, phosphate, organic amine salt, etc.). .. For example, salts of monocarboxylic acids such as sorbic acid and benzoic acid; salts of dicarboxylic acids such as oxalic acid, malonic acid and succinic acid; salts of hydroxy acids such as malic acid, citric acid, tartaric acid, salicylic acid and ferulic acid; ascorbin Salts of acids, erythorbic acid, etc .; salts of amino acids such as glycine, alanine, threonine, leucine, isoleucine, cysteine, pyrrolidone carboxylic acid, serine, aspartic acid, glutamic acid, oxyglutamic acid; sodium chloride, potassium chloride, potassium sulfate, sodium sulfite , Sodium carbonate, sodium hydrogencarbonate, sodium phosphate, sodium hydrogenphosphate, potassium phosphate, potassium hydrogenphosphate, sodium polyphosphate, sodium metaphosphate, sodium silicate and other inorganic salts; sodium pyrrolidone carboxylate and the like. ..

(Manufacturing method of oil-in-water emulsified external preparation composition)
The method for producing the oil-in-water emulsified external preparation composition of the present invention is not particularly limited, and it can be carried out by preparing each of the aqueous phase and the oil phase according to a conventional method, and then mixing and emulsifying both phases. At this time, the aqueous phase and the oil phase can be heated as necessary to dissolve the material contained in each phase.
For example, the oil-in-water emulsified external preparation composition of the present invention can be produced according to the following steps;
Fermented cellulose and / or cellulose nanofibers, and
Steps of preparing an aqueous phase containing xanthan gum and / or welan gum,
The process of preparing the oil phase,
A step of mixing and emulsifying the aqueous phase and the oil phase.

The emulsification treatment is not particularly limited and can be carried out according to a conventional method. For example, a mechanical emulsification method, a D-phase emulsification method, a phase inversion emulsification method, a liquid crystal emulsification method, an amino acid gel emulsification method and the like can be mentioned. Examples of the method used in the mechanical emulsification method include an emulsification method using a high-pressure homogenizer, a colloid mill, a nanomizer, a microfluitizer, a stirrer with a propeller, a homomixer, a homodisper, or the like. The conditions of the emulsification treatment are not particularly limited, but as an example, when a high-pressure homogenizer, nanomizer, microfluitizer or the like is used, the preferable pressure condition (pressure) is 5 MPa or more, more preferably 10 MPa or more, still more preferably 15 MPa or more. is there. The upper limit of the pressure is not particularly limited, but is, for example, 200 MPa.
Further, when a stirrer with a propeller, a homomixer, a homodisper or the like is used, the preferable rotation condition (rotation speed) is 500 rpm or more, more preferably 800 rpm or more, still more preferably 2000 rpm or more, still more preferably 5000 rpm or more. .. The upper limit of the rotation speed is not particularly limited, but is, for example, 12000 rpm.

In the present invention, it is preferable to have a step of homogenizing the fermented cellulose in the presence of water, at least prior to the step of emulsifying the aqueous phase and the oil phase. For example, before the step of preparing an aqueous phase using a fermented cellulose-containing liquid obtained by homogenizing fermented cellulose in the presence of water, or the step of emulsifying the aqueous phase and the oil phase, the aqueous phase containing fermented cellulose is homogenized. It is preferable to take a step of chemical treatment. More preferably, it is the former step.

The homogenization treatment can be carried out according to a conventional method using, for example, a high-pressure homogenizer, a colloid mill, a nanomizer, a microfluitizer, a stirrer with a propeller, a homomixer, a homodisper, or the like. The conditions for the homogenization treatment are not particularly limited, but for example, when a high-pressure homogenizer, nanomizer, microfluitizer or the like is used, the preferable pressure condition (pressure) is 1 MPa or more, more preferably 5 MPa or more, still more preferably 10 MPa or more. is there. The upper limit of the pressure is not particularly limited, but is, for example, 300 MPa.
Further, when a stirrer with a propeller, a homomixer, a homodisper or the like is used, the preferable rotation condition (rotational speed) is 3000 rpm or more, more preferably 5000 rpm or more, further preferably 6000 rpm or more, still more preferably 9000 rpm or more. .. The upper limit of the rotation speed is not particularly limited, but is, for example, 50,000 rpm.

Hereinafter, the present invention will be described in more detail with reference to Examples. However, these examples do not limit the present invention.

The tests and analyzes in the examples were carried out by the following methods.
<Measurement of viscosity>
After injecting the oil-in-water emulsified external preparation composition into a screw bottle and adjusting the product temperature of the oil-in-water emulsified external preparation composition to 25 ° C, a B-type rotational viscometer (Toki Sangyo Co., Ltd. viscometer TVB-10) The mold) was used to measure for 1 minute under the condition of a rotation speed of 30 rpm.

<Emulsification stability>
The neck of the wide-mouthed glass bottle (No. 7) (height 55 mm from the bottom of the bottle) was filled with the oil-in-water emulsified external preparation composition, and left to stand in a constant temperature bath at 50 ° C. for a certain period of time with the lid closed. .. After standing, the presence or absence of water separation was confirmed, and those without water separation were evaluated as "○" and those with water separation were evaluated as "x".

<Stability test over time>
The neck of the wide-mouthed glass bottle (No. 7) (height 55 mm from the bottom of the bottle) was filled with the oil-in-water emulsified external preparation composition, and left to stand in a constant temperature bath at 50 ° C. for a certain period of time with the lid closed. .. After standing, the distance from the bottom of the bottle to the separation boundary was measured for the generated water separation.

Test Example 1 Preliminary test (1)
As a prior art, an oil-in-water emulsified external preparation composition containing a carboxyvinyl polymer and xanthan gum was prepared, and a viscosity measurement and a stability test over time were carried out.
(Preparation of oil-in-water emulsified external preparation composition)
An oil-in-water emulsified external preparation composition (cosmetics: emulsion) was prepared according to Table 1.
The raw materials of the oil phase and the aqueous phase were mixed for each phase, heated to 80 ° C., and stirred. An oil phase was added to the aqueous phase, and the mixture was emulsified at 7000 rpm for 1 minute using a homomixer while maintaining a temperature of 75 to 80 ° C. The composition was cooled to room temperature and defoamed to prepare an oil-in-water emulsified external preparation composition. The electrolyte content in the obtained oil-in-water emulsified external preparation composition was 0.1% by mass.

(Viscosity measurement and stability test over time)
The viscosity of the prepared oil-in-water emulsified external preparation composition was measured. In addition, the prepared oil-in-water emulsified external preparation composition was allowed to stand at 50 ° C. for 1 week to evaluate its stability over time. The results are shown in Table 2.

The oil-in-water emulsified external preparation composition containing a carboxyvinyl polymer and having a viscosity of 1934 mPa · s did not show water separation at 50 ° C. for 1 week, but was emulsified in oil-in-water having a viscosity of 1283 mPa · s. In the external preparation composition, water separation (2 mm) was confirmed after 1 week at 50 ° C., and water separation after 1 month was 8 mm. Further, the oil-in-water emulsified external preparation composition containing a carboxyvinyl polymer and having a viscosity of 358 mPa · s separated a large amount of water with a water separation of 44 mm at 50 ° C. for 1 week.
The water separation of the oil-in-water emulsified external preparation composition containing xanthan gum and having a viscosity of 704 mPa · s was 17 mm at 50 ° C. for 1 week and 36 mm after 1 month at 50 ° C.
From the above, it was confirmed that in the prior art, water separation occurs as the viscosity of the oil-in-water emulsified external preparation composition decreases.

Experimental Example 1 Preparation of oil-in-water emulsification external preparation composition (cosmetics: emulsion) Oil-in-water emulsification in the same manner as in Test Example 1 except that the polysaccharide or water-soluble polymer is changed to that shown in Table 3. An external preparation composition (cosmetics: emulsion) was prepared.

(Preparation of fermented cellulose-containing liquid)
For the oil-in-water emulsified external preparation composition containing fermented cellulose as a polysaccharide, a fermented cellulose-containing liquid was prepared in advance, and the fermented cellulose-containing liquid was added to prepare an aqueous phase. For the fermented cellulose-containing liquid, water was added to 1% by mass while stirring with a homodisper (3000 rpm), and then homogenization treatment (9000 rpm, 30 minutes) was performed using a homomixer. Prepared by

(Evaluation of oil-in-water emulsified external preparation composition)
The viscosity of the prepared oil-in-water emulsified external preparation composition was measured. In addition, the prepared oil-in-water emulsified external preparation composition was allowed to stand at 50 ° C. for 1 week to evaluate the emulsification stability. The results are shown in Table 3.

The fermented cellulose complex A used in Experimental Example 1 is a preparation "Sun Artist [registered trademark] H-PN" containing 50% by mass of fermented cellulose, 17% by mass of sodium carboxymethyl cellulose, and 33% by mass of xanthan gum. is there. Table 3 shows the fermented cellulose content, xanthan gum content, and welan gum content in the oil-in-water emulsified external preparation composition. Further, in Table 3, XG indicates xanthan gum, WG indicates welan gum, and CMC-Na indicates sodium carboxymethyl cellulose. The xanthan gum content in the table shows the value excluding the xanthan gum content contained in the fermented cellulose complex (the same applies in the table below).

Sample No. which contains fermented cellulose and xanthan gum and / or welan gum, and has a xanthan gum and / or welan gum content of 2 parts by mass with respect to 1 part by mass of fermented cellulose. In the oil-in-water emulsified external preparation compositions 1 and 2, the water was not separated after 1 week at 50 ° C. Furthermore, when the stability over time of Samples 1 and 2 was continuously confirmed, the water separation after 1 month at 50 ° C. was as small as 0.5 mm (Sample No. 1) or 1 mm (Sample No. 2) from the bottom. there were.
In addition, sample No. The oil-in-water emulsified external preparation compositions 1 and 2 both had an extremely low viscosity of 620 mPa · s, and the tactile sensation was not sticky or sticky, and the feeling of use was refreshing. In addition, the slipperiness at the time of application was also good.

Sample No. Reference numeral 3 denotes an example in which the fermented cellulose complex A is used alone as the polysaccharide. Sample No. In No. 3, the fermented cellulose content was sample No. Although the amount was twice that of 1 and 2, the water was separated after 1 week. Further, when an oil-in-water emulsified external preparation composition containing 0.3% by mass of the fermented cellulose complex A (fermented cellulose content was 0.15% by mass) was prepared, a part of the composition was gelled.
Sample No. 4 to 11 are examples in which the fermented cellulose complex A is used in combination with a polysaccharide or a water-soluble polymer other than xanthan gum or welan gum. In this case as well, the sample No. Similar to No. 3, the water was separated after 1 week.

Experimental Example 2 Preparation of oil-in-water emulsified external preparation composition (cosmetics: milky lotion) The oil-in-water emulsified external preparation composition (cosmetics: milky lotion) was prepared in the same manner as in Experimental Example 1 except that the polysaccharide was changed to that shown in Table 4. Cosmetics: emulsion) was prepared. The viscosity of the prepared oil-in-water emulsified external preparation composition was measured. In addition, the prepared oil-in-water emulsified external preparation composition was allowed to stand at 50 ° C. for 1 month, and the emulsification stability after 1 week and the time stability after 1 month were evaluated. The results are shown in Table 4.

No. 1 containing 0.67 to 10 parts by mass of xanthan gum with respect to 1 part by mass of fermented cellulose. In the samples 12 to 15, no water separation was confirmed after 1 week, and the water separation after 1 month was as small as 1.5 mm or less.
In addition, sample No. The oil-in-water emulsified external preparation compositions of 12 to 15 had an extremely low viscosity of 794 mPa · s or less, and the tactile sensation was not sticky or sticky, and the feeling of use was refreshing. In addition, the slipperiness at the time of application was also good.

Experimental Example 3 Preparation of oil-in-water emulsified external preparation composition (cosmetics: emulsion) (preparation of oil-in-water emulsified external preparation composition)
An oil-in-water emulsified external preparation composition (cosmetics: emulsion) was prepared according to the formulations shown in Tables 5-6.
(Preparation of D-phase gel)
(1) and (2) in Table 5 were each dissolved at 50 ° C. Next, (2) was added slowly while stirring (1). (3) was added to the mixture, and the mixture was stirred at about 50 ° C. using a homodisper at 6000 rpm for 30 minutes and then cooled to room temperature to prepare a D-phase gel.
(Oil-in-water emulsified external preparation composition: preparation of emulsion)
Emulsion was prepared according to the formulation in Table 6. First, the gels other than the D-phase gel were stirred and dissolved at room temperature. A phase D gel was added thereto, and a milky lotion was prepared by stirring at room temperature at 7000 rpm for 1 minute using a homomixer (emulsification treatment).
In the formulation of Table 6, fermented cellulose was added as a fermented cellulose-containing liquid. The fermented cellulose-containing liquid was prepared according to the method described in Experimental Example 1. Similarly, in the formulation shown in Table 7, as the cellulose nanofiber, a 2% cellulose-containing solution (“Leocrysta [registered trademark]” manufactured by Dai-ichi Kogyo Seiyaku Co., Ltd.) mixed with water in advance was used.
The electrolyte content in the obtained oil-in-water emulsified external preparation composition was 0.1% by mass.

The viscosity of the prepared oil-in-water emulsified external preparation composition was measured. Moreover, the prepared oil-in-water type external preparation composition was allowed to stand at 50 ° C. for 1 week, and the stability over time was evaluated. The results are shown in Table 7.

In all the samples (oil-in-water emulsified external preparation composition), the water separation after 1 week at 50 ° C. was as small as 3 mm or less from the bottom. In addition, all the samples had an extremely low viscosity of 216 mPa · s or less, and the tactile sensation was not sticky or sticky, and the feeling of use was refreshing. In addition, the slipperiness at the time of application was also good.

Experimental Example 4 Preparation of oil-in-water emulsified external preparation composition (cosmetics: emulsion) (preparation of oil-in-water emulsified external preparation composition)
An oil-in-water emulsified external preparation composition (cosmetics: emulsion) was prepared according to the formulation shown in Table 8.
The raw materials of the oil phase and the aqueous phase were mixed for each phase, heated to 80 ° C., and stirred. An oil phase was added to the aqueous phase, and the mixture was emulsified at 7000 rpm for 1 minute using a homomixer while maintaining a temperature of 75 to 80 ° C. The composition was cooled to room temperature and defoamed to prepare an oil-in-water emulsified external preparation composition.
The electrolyte content in the obtained oil-in-water emulsified external preparation composition was 2.1% by mass.

(Viscosity measurement and emulsion stability test)
The viscosity of the prepared oil-in-water emulsified external preparation composition was measured. In addition, the prepared oil-in-water emulsified composition was allowed to stand at 50 ° C. for 1 week to evaluate the emulsification stability. The results are shown in Table 9.

This formulation has a high electrolyte content of about 2.1% by mass. However, Sample No. containing fermented cellulose and xanthan gum. In each of the oil-in-water emulsified external preparation compositions of 20 to 22, no separation of water was confirmed even after 1 week at 50 ° C., indicating high stability. In addition, all the samples had a low viscosity of 941 mPa · s or less, and the tactile sensation was not sticky or sticky, and the feeling of use was refreshing. In addition, the slipperiness at the time of application was also good.
On the other hand, Sample No. using a carboxyvinyl polymer as the polysaccharide. Since the oil-in-water emulsified external preparation compositions of Nos. 23 and 24 contained an electrolyte, almost no thickening action was exhibited, and after 1 day, water separation occurred and the stability was low.

Experimental Example 5 Preparation of oil-in-water emulsified external preparation composition (cosmetics: emulsion) (preparation of oil-in-water emulsified external preparation composition)
As the fermented cellulose, except that the fermented cellulose complex B (preparation "Sun Artist [registered trademark] H-PG" containing 60% by mass of fermented cellulose, 20% by mass of sodium carboxymethyl cellulose, and 20% by mass of guar gum) is used. , An oil-in-water emulsified external preparation composition was prepared according to the formulation of Experimental Example 1.

(Viscosity measurement and stability test over time)
The viscosity of the prepared oil-in-water emulsified external preparation composition was measured. In addition, the prepared oil-in-water emulsified external preparation composition was allowed to stand at 50 ° C. for 1 week to evaluate the stability test over time. The results are shown in Table 10.

Similarly, when the fermented cellulose complex B was used instead of the fermented cellulose complex A, an oil-in-water emulsified external preparation composition having excellent emulsion stability could be prepared by using xanthan gum in combination. Specifically, No. 1 containing 0.56 to 1.7 parts by mass of xanthan gum with respect to 1 part by mass of fermented cellulose. The water separation of the 25 to 26 samples was very small, 1 mm or less, after being allowed to stand at 50 ° C. for 1 week. Further, the viscosity was as low as 597 mPa · s or less, and the tactile sensation was not sticky or sticky, and the feeling of use was refreshing. In addition, the slipperiness at the time of application was also good.

Claims (4)

And containing a fermentation cellulose Graphics and Weranga-time, and,
An oil-in-water emulsified external preparation composition that satisfies the following conditions (A) and (B);
(A) relative to said fermentation cellulose scan 1 part by weight, the content of pre Kiu Erangamu is 0.1 to 15 parts by weight,
( B) The viscosity of the B-type rotational viscometer at 25 ° C. at 30 rpm is 1000 mPa · s or less. The oil-in-water emulsified external preparation composition according to claim 1, wherein the external preparation composition is a cosmetic. The method for producing an oil-in-water emulsified external preparation composition according to claim 1 or 2, which comprises the following steps;
Preparing an aqueous phase containing the fermented cellulose及beauty c Erangamu,
The process of preparing the oil phase,
A step of mixing and emulsifying the aqueous phase and the oil phase. The method for producing an oil-in-water emulsified external preparation composition according to claim 3.
At least before the process of emulsifying the aqueous and oil phases,
A method comprising a step of homogenizing the fermented cellulose in the presence of water.