JP6909917B1 - Emulsifying composition, oil-in-water (O / W type) emulsifying composition, and cosmetic composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an emulsified composition having good dispersibility of an emulsion even when various oil-soluble substances are used. An emulsified composition containing an oil-soluble substance, a polyhydric alcohol, biomass nanofibers, and a first aqueous medium, and the content of the oil-soluble substance is 20% by mass or more. Is preferably a D-phase medium oil type (O / D type). [Selection diagram] Fig. 1

Description

The present invention relates to emulsified compositions, oil-in-water (O / W type) emulsified compositions, and cosmetic compositions.

Emulsification compositions (emulsions) are used in many products such as processed foods, favorite foods, health foods, cosmetics, pharmaceuticals, paints, cooking / seasonings, various beverages, and feeds. Products containing these emulsifying compositions are required to have a stable emulsifying ability with respect to oils in order to improve quality stability. Various methods are known as methods for producing an emulsified composition. Among them, a D (Detergent) phase emulsification method for obtaining an emulsified composition of fine oil droplets has attracted attention (see, for example, Patent Documents 1 to 4).

In the D-phase emulsification method, an emulsifying composition is produced by first dissolving an emulsifier in a polyhydric alcohol or an aqueous solution of a polyhydric alcohol, adding an oil phase to the emulsifier, and emulsifying the emulsifier. Next, it is a method of obtaining a fine emulsion by diluting this emulsified composition with an aqueous medium (see, for example, Non-Patent Document 1).

Japanese Unexamined Patent Publication No. 7-59545 Japanese Unexamined Patent Publication No. 2000-10256 Japanese Unexamined Patent Publication No. 2000-83624 Japanese Unexamined Patent Publication No. 2004-290104

Fragrance Journal, 4, 34-41 (1993)

For example, Patent Document 2 describes an aqueous phase medium oil emulsion (O / D type) emulsion obtained by adding eggs, vinegar and oil to a D phase medium oil type (O / D type) emulsifying composition containing an emulsifier having an HLB of 6 to 16 in the D phase. Mayonnaise) is disclosed. It is described that the emulsion is more stable than the oil-in-phase oil-type emulsion (mayonnaise) obtained by simply mixing an emulsifier having an HLB of 6 to 16 with eggs, vinegar and oil. Patent Document 4 describes that the oil droplets of the D-phase medium oil type (O / D type) emulsified composition containing an emulsifier having an HLB of 11 to 16 in the D phase are stable even in an acidic food. Further, in Example 2 of Patent Document 3, a D-phase medium oil type (O / D type) containing monostearic acid diglycerin ester (HLB7.6) and distearic acid decaglycerin ester (HLB11.7) in the D phase. The whole egg solution containing the emulsified composition has been described as being stable even when frozen.

However, these D-phase medium oil type (O / D type) emulsified compositions add stability of oil droplets of an aqueous phase medium oil type (O / W type) emulsion obtained by mixing this with an aqueous medium. It is still far from satisfactory in terms of the stability of oil droplets in warm conditions. Further, in order to cope with the diversification of products in the future, it is preferable from the viewpoint of versatility that an emulsified composition having high dispersibility in various oil-soluble substances can be obtained, but such a highly practical emulsified composition Has not yet been found.
Therefore, an object of the present invention is to provide an emulsified composition having good dispersibility of an emulsion even when various oil-soluble substances are used.

As a result of diligent studies in view of the above circumstances, the present inventors have made a fine oil with high stability by combining a polyhydric alcohol and biomass nanofibers when containing a high concentration of oil-soluble substance. They have found that an emulsified composition that gives drops can be obtained, and have completed the present invention. That is, the present invention is as follows.
[1] An emulsified composition containing a polyhydric alcohol, a first aqueous medium, biomass nanofibers, and an oil-soluble substance, wherein the content of the oil-soluble substance is 20% by mass or more.
[2] The emulsified composition according to [1], which is a D-phase medium oil type (O / D type).
[3] The emulsified composition according to [1] or [2], wherein the biomass nanofibers are silk nanofibers.
[4] The emulsified composition according to any one of [1] to [3], wherein the oil-soluble substance is at least one of a saturated hydrocarbon oil and a silicone oil.
[5] An oil-in-water (O / W type) emulsified composition containing the emulsified composition according to any one of [1] to [4] and a second aqueous medium.
[6] A cosmetic composition containing the emulsified composition according to any one of [1] to [4] or the oil-in-water (O / W type) emulsified composition according to [5].

According to the present invention, it is possible to provide an emulsified composition having good dispersibility of an emulsion even when various oil-soluble substances are used.
In particular, when the emulsified composition of the present invention is a D-phase medium oil type (O / D type) emulsified composition, when further diluted with an aqueous medium, an emulsion having a small particle size of oil droplets and excellent stability is obtained. , Foods, pharmaceuticals, cosmetics, etc. can be suitably used.

It is an image which observed the emulsified state of the emulsified composition in Examples 1-5. It is an image which observed the emulsified state of the emulsified composition in Comparative Examples 1-5. It is an image which observed the emulsified state of the emulsified composition in Examples 9-13. It is an image which observed the emulsified state of the emulsified composition in Examples 17-21. It is an image which observed the emulsified state of the emulsified composition in Examples 22, 25-28. It is an image which observed the emulsified state of the emulsified composition in Examples 29-33. It is an image which observed the emulsified state of the emulsified composition in Examples 34-38.

[Emulsification composition]
The emulsified composition according to the embodiment of the present invention contains a polyhydric alcohol, a first aqueous medium, biomass nanofibers, and an oil-soluble substance, and the content of the oil-soluble substance is 20% by mass or more. ..

Biomass nanofibers are nanofibers derived from biomass, and examples thereof include plant nanofibers and animal nanofibers. All of these have a hydrophilic part and a hydrophobic part in the network. Due to this amphipathic nature, the polyhydric alcohol and the aqueous medium are well retained in the nanofiber network, and the emulsion stability of oil-soluble substances having a high concentration of 20% by mass or more can be improved. It is presumed that it can be done.
Here, the "nanofiber" of the biomass nanofiber means a fiber having an average diameter (average width) of 1 nm to 1000 nm.

The emulsified composition according to the present embodiment can be obtained by adding an oil-soluble substance to a polyhydric alcohol containing biomass nanofibers and an aqueous medium, or an aqueous solution of a polyhydric alcohol containing biomass nanofibers, and stirring the mixture. .. In particular, the inclusion of biomass nanofibers makes it easier for oil-soluble substances to be captured by the polyhydric alcohols in the network. As a result, unlike the conventional emulsifier, it becomes easy to obtain an emulsified composition having good dispersibility of the emulsion not only in the heated state but also at room temperature.

Here, the emulsified composition according to the present embodiment is preferably a D-phase medium oil type (O / D type) from the viewpoint of efficiently supplementing an oil-soluble substance in the network of biomass nanofibers. Hereinafter, each component and the like will be described, but the present invention is not limited thereto.

(Multivalent alcohol)
As the polyhydric alcohol, a water-soluble polyhydric alcohol is preferably used, and among them, those having three or more hydroxyl groups in the molecule are preferable. For example, polyglycerin such as glycerin, diglycerin, triglycerin, tetraglycerin, sugars such as glucose, maltose, martitol, sucrose, fructose, xylitol, inositol, pentaerythritol, sorbitol, maltotriose, starch-degrading sugar and these. Glycerin is preferable, and glycerin is more preferable. These may be used alone or in combination of two or more. Further, the polyhydric alcohol may be used as it is, or may be dissolved in water and used as an aqueous solution of about 50 to 99.9% by mass.

The proportion of the polyhydric alcohol in the emulsified composition (particularly the oil-type (O / D-type) emulsified composition in the D phase) is preferably 7% by mass or more, and more preferably 15% by mass or more. Further, it is preferably 40% by mass or less, and more preferably 20% by mass or less.

(First aqueous medium)
Examples of the first aqueous medium include water, an aqueous solution containing a polar organic solvent and the like, and it is desirable that the concentration of the organic solvent is low, and water is particularly preferable. The ratio of the first aqueous medium to the emulsified composition (particularly the oil-type (O / D-type) emulsified composition in the D phase) is preferably 1.0% by mass or more, preferably 1.5% by mass or more. Is more preferable. Further, it is preferably 8.0% by mass or less, and more preferably 4.0% by mass or less.

(Biomass nanofiber)
Biomass nanofibers are excellent in emulsification performance, and stable emulsification compositions can be produced even when various oil-soluble substances are used.
Examples of biomass nanofibers include plant nanofibers and animal nanofibers, examples of plant nanofibers include cellulose nanofibers, and examples of animal nanofibers include silk nanofibers, chitin nanofibers, and chitosan nanofibers. Can be mentioned.

Here, as the cellulose nanofibers, nanofibers derived from crystalline cellulose and nanofibers derived from powdered cellulose are preferable. These are preferable in terms of chemical stability and thermal stability.
The nanofibers derived from crystalline cellulose refer to those obtained by micronizing known crystalline cellulose into nanofibers. The crystalline cellulose used in the present invention is obtained by partially depolymerizing α-cellulose obtained as pulp from a fibrous plant with an acid and purifying it. As the crystalline cellulose, for example, those described in the Food Additives Official Standard (9th Edition) are known.

Further, the nanofibers derived from powdered cellulose refer to those obtained by finely processing known powdered cellulose into nanofibers. The powdered cellulose used in the present invention is obtained by treating α-cellulose obtained as pulp from a fibrous plant, purifying it while leaving amorphous components such as hemicellulose and lignin, and mechanically pulverizing it. As the powdered cellulose, for example, those described in the Food Additives Official Standard (9th Edition) are known.

Biomass nanofibers have an average diameter of 1 to 1000 nm. If the average diameter is less than 1 nm, the network structure of the nanofibers becomes fragile, the structure cannot be maintained, and the emulsion may become unstable. On the other hand, if it exceeds 1000 nm, the size may become too large and the stability of the emulsion may be impaired. The average diameter of the biomass nanofibers is preferably 10 nm or more, more preferably 20 nm or more. Further, it is preferably 100 nm or less, and more preferably 50 nm or less.

The average length of the biomass nanofibers is preferably 1000 nm or more, more preferably 2000 nm or more. Further, it is preferably 100 μm or less, and more preferably 50 μm or less.
The average diameter and average length of the biomass nanofibers can be obtained as the average value by measuring the fiber diameter (fiber width) and length of the fibers by, for example, observing with a transmission electron microscope.

The aspect ratio (average length / average diameter) of the biomass nanofibers is preferably 20 to 10000, more preferably 40 to 5000, and even more preferably 100 to 1000.

In addition, although any of the biomass nanofibers can be used, silk nanofibers and plant-derived nanofibers are preferable in consideration of the affinity for living organisms for cosmetic purposes.

As the silk nanofibers, it is preferable to use a dilute alkaline chemical and perform a high-pressure injection treatment of 100 to 245 MPa to obtain silk nanofibers. Although such silk nanofibers use alkaline chemicals, they are chemicals commonly used in cosmetic raw materials and food additives, the solvent is water, and the silk raw materials collide with each other. Since it is defibrated into the shape of nanofibers, impurities are less likely to be generated during the production of nanofibers, which is more preferable for nanofibers that are defibrated through a medium such as a mill or a grindstone.
Therefore, the silk nanofibers are preferably obtained through high-pressure injection treatment. Specifically, the crystallinity of the silk nanofibers is preferably 3% or more, more preferably 10 to 90%.
The crystallinity can be determined by placing the sample on a glass cell and measuring it using an X-ray diffraction measuring device. Specifically, the diffraction intensity of the crystalline portion and the amorphous portion (amorphous) can be calculated by measuring the region of 2θ = 5 ° to 60 ° in the X-ray diffraction diagram.

For bio-nanomas fibers other than silk nanofibers, for example, nanofibers derived from crystalline cellulose, nanofibers derived from powdered cellulose, chitin nanofibers, chitosan nanofibers, etc., for example, an injection nozzle having a diameter of 0.1 to 0.8 mm. It is preferable to use a fluid obtained by colliding the biomass dispersion fluid with the collision hard body or injecting and colliding with each other to refine the biomass by a high-pressure injection treatment of 100 to 245 MPa. This method involves not only a shearing force that allows the dispersed fluid to pass through a narrow flow path at high pressure and low speed to homogenize it at the time of release, as in a commercially available high-pressure homogenizer, but also to cause the dispersed fluid to collide with a hard body for collision. Continuous processing at high pressure using collision force and cavitation is possible.

The proportion of biomass nanofibers in the emulsified composition (particularly the D-phase medium oil type (O / D type) emulsified composition) is oil droplets when diluted with an aqueous medium to form an oil-in-water (O / W type) emulsion. From the viewpoint of reducing the particle size of the emulsion, it is 0.05% by mass or more, preferably 0.1% by mass or more, and from the viewpoint of the stability of the emulsion and the flavor when used in foods and beverages. It is 10% by mass or less, preferably 5% by mass or less.

Further, in the emulsified composition (particularly the D-phase medium oil type (O / D type) emulsified composition), the mass ratio of the biomass nanofibers to the oil-soluble substance (oil-soluble substance / biomass nanofibers) is the dispersibility of the emulsion. From the viewpoint of its stability, it is preferably 50 to 1000.
In particular, when the biomass nanofibers are silk nanofibers, the mass ratio is more preferably 100 to 900.
When the biomass nanofibers are chitin nanofibers or chitosan nanofibers, the mass ratio is more preferably 100 to 450, and even more preferably 100 to 350.
Further, when the biomass nanofiber is a nanofiber derived from crystalline cellulose, the mass ratio is more preferably 100 to 450, and further preferably 100 to 350.
When the biomass nanofibers are nanofibers derived from powdered cellulose, the mass ratio is more preferably 100 to 450, and even more preferably 100 to 350.

(Oil-soluble substance)
As the oil-soluble substance, any oil-soluble substance used in fields such as food, feed, cosmetics, pharmaceuticals and industry can be used, and for example, fatty acids, fats and oils, waxes, hydrocarbons, silicone-based oils, higher alcohols, etc. Examples include terpen, essential oils, fat-soluble vitamins, oil-soluble drugs, oil-soluble pigments and the like.

Fatty acids include, for example, myristic acid, palmitic acid, isopalmitic acid, stearic acid, oleic acid, linolenic acid, linolenic acid, ricinoleic acid, 12-hydroxystearic acid, 10-hydroxystearic acid, behenic acid, hexadecatrine acid, Examples thereof include octadecatrienoic acid, eicosatetraenoic acid, docosapentaenoic acid, eicosapentaenoic acid, docosapentaenoic acid, docosapentaenoic acid, tetrahexaenoic acid, and geometric isomers thereof. Examples of the fatty acid ester include the above-mentioned fatty acid esters such as ethyl myristate.

The fat and oil is a glycerin ester of a fatty acid, and is a glycerin ester of the above-mentioned fatty acid mixture. For example, animal fats and oils such as fish oil, beef fat, pork fat, milk fat, horse oil, snake oil, egg oil, egg yolk oil, turtle oil, mink oil; soybean oil, corn oil, cottonseed oil, rapeseed oil, sesame oil, perilla oil, Rice germ oil, sunflower oil, peanut oil, olive oil, palm oil, palm kernel oil, rice germ oil, wheat germ oil, brown rice germ oil, honeybee oil, garlic oil, macadamian nut oil, avocado oil, evening primrose oil, flower oil, Vegetable oils and fats such as brim oil, coconut oil, castor oil, linseed oil, and cacao oil: and hydrogenated or ester-exchanged ones; medium chain fatty acid triglyceride and the like.

Wax is an ester of fatty acid and higher monohydric or divalent alcohol. For example, jojoba oil, rice wax, propolis, beeswax, bleached beeswax, candelilla wax, carnauba wax, wood wax, whale wax and the like can be mentioned.

Examples of hydrocarbons include liquid paraffins such as light liquid paraffin, heavy liquid paraffin, liquid isoparaffin, and light liquid isoparaffin, paraffin, petrolatum, microcrystalline wax, selecin, squalane, and squalene. Among them, saturated hydrocarbons. Squalene oil is preferable.

Silicone-based oils modify, for example, dimethylpolysiloxane, methylphenylpolysiloxane, cyclic silicone, and aminosilicone, fatty acid silicone, alcohol silicone, polyether silicone, epoxy silicone, fluorosilicone, glycoside silicone and / or alkylsilicone. Examples thereof include silicone compounds.

Examples of higher alcohols include saturated or unsaturated alcohols having 8 to 44 carbon atoms such as lauryl alcohol, myristyl alcohol, cetanol, stearyl alcohol, oleyl alcohol, laurin alcohol, isostearyl alcohol and 2-octyldodecanol octacosanol. ..
Examples of terpenes include eugenol, geraniol, menthol, citral, citronellal, borneol and the like.

Essential oils include, for example, ambrette seed oil, mustard oil, saffron oil, citronella oil, vetiver oil, valerian oil, yomogi oil, chamomile oil, sardine oil, sassafras oil, peppermint oil, rosewood oil, clary sage oil, thyme oil. , Basil oil, carnation oil, cedar wood oil, hinoki oil, hiba oil, clove oil, terepine oil, pine oil, orange oil, lemongrass oil, taragon oil, laurel leaf oil, cassia oil, cinnamon oil, pepper oil, columnar oil , Sage oil, peppermint oil, peppermint oil, spare mint oil, patchuri oil, rosemary oil, lavandine oil, lavender oil, curcuma oil, cardamon oil, ginger oil, angelica oil, anis oil, uikyo oil, parsley oil, celery oil , Carbanum oil, Cumin oil, Coriander oil, Jill oil, Carrot oil, Kiraway oil, Winter green oil, Natsumeg oil, Rose oil, Sipress oil, Byakudan oil, All spice oil, Grapefruit oil, Neroli oil, Lemon oil, Lime oil , Bergamot oil, mandarin oil, onion oil, garlic oil, bitter almond oil, geranium oil, mimosa oil, jasmine oil, kinmokusei oil, staranis oil, cananga oil, ylang ylang oil, eucalyptus oil and other essential oils; Examples thereof include oleoledin or resinoid such as ginger, parsley, coriander, himeuikyo, pimenta, vanilla, celery, chowji, nikuzuku, publica, iris resinoid, and milk scented tree.

Fat-soluble vitamins include, for example, vitamins A, D, E, K and derivatives thereof.
Examples of the oil-soluble drug include coenzyme Q10, α-lipoic acid, rutin, lutein and the like.
Examples of the oil-soluble pigment include annatto pigment, paprika pigment, β-carotene, chlorophyll, red yeast pigment, turmeric pigment and the like. These may be used alone or in combination of two or more.

The oil-soluble substance is preferably at least one of a saturated hydrocarbon-based oil and a silicone-based oil from the viewpoint of good catching property in the network of nanofibers.

When the oil-soluble substance is solid at a temperature at which a D-phase medium oil type (O / D type) emulsified composition is produced, it may be dissolved in a liquid oil-soluble substance at that temperature before use.

The ratio of the oil-soluble substance in the emulsified composition (particularly the oil-type (O / D type) emulsified composition in the D phase) is 20% by mass or more, preferably 30% by mass or more, more preferably 40% by mass or more. More preferably, it is 60% by mass or more. If it is less than 20% by mass, the concentration of the oil-soluble substance is relatively lowered when diluted with an aqueous medium in a later step, and the versatility is also lowered. The proportion of the oil-soluble substance is preferably 90% by mass or less, and more preferably 80% by mass or less.

The D-phase medium oil type (O / D type) emulsifying composition is obtained by using an aqueous solution of a polyhydric alcohol in which biomass nanofibers are dispersed at a temperature of 10 to 80 ° C. at 500 to 20,000 rpm, preferably 1,000 to 10, The mixture is stirred at 000 rpm, and an oil-soluble substance in which a lipophilic emulsifier is dissolved is added little by little, and then the temperature is maintained at 500 to 20,000 rpm, preferably 1,000 to 10,000 rpm for 1 to 60. It can be obtained by further stirring for minutes, preferably 5 to 30 minutes.

(emulsifier)
The emulsified composition according to this embodiment may contain an emulsifier. Examples of the emulsifiers that can be used include polyglycerin having a degree of polymerization of glycerin of 4 or more, preferably 4 to 12, such as decaglycerin monomyristate, decaglycerin monopalmitate, decaglycerin monostearate, and decaglycerin monooleate. Fatty acid ester; sucrose fatty acid ester such as sucrose monomyristic acid ester, sucrose monopalmitic acid ester, sucrose monostearic acid ester, sucrose monooleic acid ester; sucrose partial hydrolyzate, water-soluble phospholipid such as lysolecithin Examples thereof include emulsifiers having an HLB of 10 or more, such as glycolipids; saponins; proteins such as soybean protein and sodium caseinate and modified products thereof. These may be used alone or in combination of two or more.

The emulsified composition according to the present embodiment (particularly, D-phase medium oil type (O / D type) emulsified composition) includes cosmetics, paints, pharmaceuticals and the like, retort foods, instant foods, instant noodles, drifts, processed milk and the like. Foods such as processed foods, favorite foods, supplements, functional foods, special purpose foods, sick foods, elderly foods, childcare powdered milk, health foods such as specified health foods, self-emulsifying fats and oils, ketchup, mayonnaise , Tartar sauce, Worcester sauce, ra oil, spices, herbs, fats and oils, cooking / seasoning such as salad dressing, and beverages such as sake, coffee and tea.

[Oil-in-water type (O / W type) emulsified composition]
The oil-in-water (O / W type) emulsified composition of the present invention contains the above-mentioned emulsified composition of the present invention and a second aqueous medium. As the second aqueous medium, the same as the first aqueous medium can be exemplified, and the first aqueous medium and the second aqueous medium may be the same or different.

The D-phase medium oil type (O / D type) emulsified composition according to the present invention contains 0.01 to 50% by mass, preferably 0.1 to 20% by mass, of the D-phase medium oil type (O / D type) emulsified composition. By mixing with a second aqueous medium so as to be, an oil-in-phase (O / W type) emulsified composition is obtained.
The D-phase medium oil type (O / D type) emulsified composition according to the present invention is diluted with a water-soluble active ingredient or additive and used as a cosmetic composition such as a lotion or a beauty essence. be able to. Further, the oil-in-water (O / W type) emulsified composition of the present invention obtained from the D-phase medium oil type (O / D type) emulsified composition according to the present invention has good stability at a high temperature (60 ° C.). Therefore, it is suitably used for heating foods such as instant soup, and warming beverages such as hot milk coffee and hot milk tea.

[Cosmetic composition]
The cosmetic composition of the present invention includes the emulsified composition of the present invention or the oil-in-water (O / W type) emulsified composition of the present invention. Then, a product to which a water-soluble active ingredient or additive is added can be appropriately diluted and used as a cosmetic composition such as a lotion or a beauty essence.

Additives include, for example, water-soluble vitamins such as ascorbic acid, nicotinic acid amide, and nicotinic acid; Animal and plant extracts such as placenta extract, seaweed extract, marronnier extract, yuzu extract, eucalyptus extract, asunaro extract; salts such as potassium hydroxide, sodium hydroxide, triethanolamine, sodium carbonate; citrate, tartrate, PH adjusters such as lactate, phosphate, succinate, adipate; thickening of carboxyvinyl polymer, sodium alginate, carrageenan, carboxymethyl cellulose, hydroxyethyl cellulose, guar gum, xanthan gum, carboxymethyl chitosan, sodium hyaluronate, etc. Agents and the like can be mentioned.

Hereinafter, the present invention will be described in more detail with reference to Examples. However, these examples do not limit or limit the present invention in any way.
The dispersity in each example was evaluated as follows.

<Dispersion stability>
The dispersion stability (dispersity) was evaluated by allowing the mixture to stand at room temperature after the final stirring and observing the appearance of the emulsified composition after 72 hours. "Those with clear separation between water layer and oil layer" are marked with x, "state where the boundary surface is unclear" is △, and "things that seem to have some separation but can be said to be in an emulsified state" are marked with △ 〇. "Those with almost no clear separation, that is, those in an emulsified state" were marked with 〇, and those with no clear separation, that is, those in a very good emulsified state, were marked with ◎.

<Example 1>
Using 120 g of silicone oil as an oil-soluble substance, an emulsified composition (D phase medium oil type (O / D type) emulsified composition) was prepared by the following procedure.

(1) 24 g of glycerin (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd., the same applies to the following examples), silk nanofiber aqueous dispersion (manufactured by Sugino Machine Co., Ltd., high-pressure injection processed product, silk nanofiber concentration 5 wt%, average 3 g of each of silk nanofibers having a diameter of 100 nm or less (the same applies to the following silk nanofiber examples) and ion-exchanged water were added, and the mixture was stirred for 10 minutes to prepare a uniform mixture.
(2) Silicone oil (manufactured by Shin-Etsu Chemical Co., Ltd., product name KF-96A-100CS, the same applies to the following examples) is added to the mixture prepared in (1) at a rate of 5 ml / min using a three-one motor stirrer. did.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a D-phase medium oil type (O / D type) emulsified composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 1 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Example 2>
D-phase medium oil type (O / D type) in the same manner as in Example 1 except that 120 g of silicone oil was used as an oil-soluble substance for liquid paraffin (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd., the same applies to the following examples). ) An emulsified composition was prepared and the dispersion stability was evaluated. The results are shown in Table 1.

<Example 3>
D-phase medium oil type (O / D type) emulsified composition in the same manner as in Example 1 except that 120 g of silicone oil was used as an oil-soluble substance in Squalane (manufactured by Junsei Chemical Co., Inc., the same applies to the following examples). Was prepared and the dispersion stability was evaluated. The results are shown in Table 1.

<Example 4>
D-phase medium oil type (O / D type) in the same manner as in Example 1 except that 120 g of silicone oil was used as an oil-soluble substance as olive oil (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd., the same applies to the following examples). An emulsified composition was prepared and the dispersion stability was evaluated. The results are shown in Table 1.

<Example 5>
D-phase medium oil type (O / D type) in the same manner as in Example 1 except that 120 g of silicone oil was used as an oil-soluble substance in jojoba oil (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd., the same applies to the following examples). ) An emulsified composition was prepared and the dispersion stability was evaluated. The results are shown in Table 1.

<Example 6>
Using 120 g of the same silicone oil as in Example 1 as the oil-soluble substance, an emulsified composition (D phase medium oil type (O / D type) emulsified composition) was prepared by the following procedure.
(1) 6 g of the silk nanofiber aqueous dispersion used in Example 1 was added to 24 g of glycerin, and the mixture was stirred for 10 minutes to prepare a uniform mixture.
(2) Silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min with a three-one motor stirrer.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a self-emulsifying fat and oil composed of a D-phase medium oil type (O / D type) emulsifying composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 1 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Example 7>
(1) To 24 g of glycerin, 3 g of an aqueous dispersion of silk nanofibers and 78 g of ion-exchanged water were added, and the mixture was stirred for 10 minutes to prepare a uniform mixture.
(2) With a three-one motor stirrer, 45 g of silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a D-phase medium oil type (O / D type) emulsified composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 1 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Example 8>
(1) To 24 g of glycerin (manufactured by Wako Pure Chemical Industries, Ltd.), 3 g of an aqueous dispersion of silk nanofibers and 48 g of ion-exchanged water were added, and the mixture was stirred for 10 minutes to prepare a uniform mixture.
(2) With a three-one motor stirrer, 75 g of silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a D-phase medium oil type (O / D type) emulsified composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 1 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Comparative example 1>
As Comparative Example 1, an emulsified composition (D phase medium oil type (O / D type) emulsified composition) was prepared by using 120 g of silicone oil as an oil-soluble substance by the following procedure.
(1) To 24 g of glycerin, 3 g of silk particles (average particle size 10 to 40 μm) and 3 g of ion-exchanged water were added, and the mixture was stirred for 10 minutes to prepare a uniform mixture.
(2) Silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min with a three-one motor stirrer.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a self-emulsifying fat and oil composed of a D-phase medium oil type (O / D type) emulsifying composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 1 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Comparative example 2>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 1 except that 120 g of silicone oil was used as the oil-soluble substance and 120 g of squalane was used. The results are shown in Table 1.

<Comparative example 3>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 1 except that 120 g of silicone oil was used as the oil-soluble substance and 120 g of liquid paraffin was used. The results are shown in Table 1.

<Comparative example 4>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 1 except that 120 g of silicone oil was used as the oil-soluble substance and 120 g of olive oil. The results are shown in Table 1.

<Comparative example 5>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 1 except that 120 g of silicone oil was used as the oil-soluble substance and 120 g of jojoba oil was used. The results are shown in Table 1.

FIG. 1 is an image of observing the emulsified composition obtained by stirring silk nanofibers and each of silicone oil, squalane, liquid paraffin, olive oil, and jojoba oil, which are Examples 1 to 5, for 72 hours. It is an image of the later emulsified composition.

FIG. 2 is an image of observing the emulsified composition obtained by stirring the silk particles and each of silicone oil, squalane, liquid paraffin, olive oil, and jojoba oil, which are Comparative Examples 1 to 5, after 72 hours. It is an image of the emulsified composition of.

The following was found from FIGS. 1 and 2. In this example, the emulsified composition to which silk nanofibers and polyhydric alcohol were added to which an oil agent was added maintained an emulsified state and did not separate even after 72 hours. After that, the patient was followed up, but the emulsified state was maintained as well. In silk particles not defibrated into nanofibers, the oil layer and the aqueous layer were almost completely separated.

Further, when the viscosity (25 ° C.) at a silk nanofiber concentration of 0.1% (Example 1) and 0.2% (Example 6) was measured (after 72 hours with a rheometer), 13000 mPa · s, respectively. , 30,000 mPa · s, and from the comparison of these viscosities, the viscosity of the emulsified composition could be controlled by the concentration of nanofibers.

According to this example, the emulsion to which silk nanofibers and polyhydric alcohol are added is heated at 60 ° C. for 30 minutes and then allowed to cool, and the emulsion maintains excellent emulsification performance for a long period of time with almost no discoloration. It can be said that it can be done.

<Example 9>
Using 80 g of silicone oil as an oil-soluble substance, an emulsified composition (D phase medium oil type (O / D type) emulsified composition) was prepared by the following procedure.

(1) Examples of the following chitin nanofibers in 16 g of glycerin, chitin nanofiber aqueous dispersion (BiNFi-s (SFO-40010) manufactured by Sugino Machine Co., Ltd., chitin nanofiber concentration 10 wt%, average diameter 20 to 50 nm). The same applies to the above) and 2 g of ion-exchanged water were added, and the mixture was stirred for 10 minutes to prepare a uniform mixture.
(2) Silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min with a three-one motor stirrer.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a D-phase medium oil type (O / D type) emulsified composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 2 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Example 10>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Example 9 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of liquid paraffin was used. The results are shown in Table 2.

<Example 11>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Example 9 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of squalane was used. The results are shown in Table 2.

<Example 12>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Example 9 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of olive oil. The results are shown in Table 2.

<Example 13>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Example 9 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of jojoba oil was used. The results are shown in Table 2.

<Example 14>
Using 80 g of the same silicone oil as in Example 1 as the oil-soluble substance, an emulsified composition (D phase medium oil type (O / D type) emulsified composition) was prepared by the following procedure.
(1) 4 g of the chitin nanofiber aqueous dispersion used in Example 9 was added to 16 g of glycerin, and the mixture was stirred for 10 minutes to prepare a uniform mixture.
(2) Silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min with a three-one motor stirrer.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a self-emulsifying fat and oil composed of a D-phase medium oil type (O / D type) emulsifying composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 2 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Example 15>
(1) To 16 g of glycerin, 2 g of an aqueous dispersion of chitin nanofibers and 52 g of ion-exchanged water were added, and the mixture was stirred for 10 minutes to prepare a uniform mixture.
(2) With a three-one motor stirrer, 30 g of silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a D-phase medium oil type (O / D type) emulsified composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 2 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Example 16>
(1) To 16 g of glycerin (manufactured by Wako Pure Chemical Industries, Ltd.), 2 g of an aqueous dispersion of chitin nanofibers and 32 g of ion-exchanged water were added, and the mixture was stirred for 10 minutes to prepare a uniform mixture.
(2) 50 g of silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min with a three-one motor stirrer.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a D-phase medium oil type (O / D type) emulsified composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 2 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Comparative Example 6>
As Comparative Example 6, an emulsified composition (D phase medium oil type (O / D type) emulsified composition) was prepared by using 80 g of silicone oil as an oil-soluble substance by the following procedure.
(1) Add 0.2 g of chitin particles (average particle size 1 to 300 μm, aspect ratio (major axis / minor axis) less than 10) and 3.8 g of ion-exchanged water to 16 g of glycerin (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.). , Stirring was performed for 10 minutes to prepare a uniform mixture.
(2) Silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min with a three-one motor stirrer.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a self-emulsifying fat and oil composed of a D-phase medium oil type (O / D type) emulsifying composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 2 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Comparative Example 7>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 6 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of liquid paraffin was used. The results are shown in Table 2.

<Comparative Example 8>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 6 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of squalane was used. The results are shown in Table 2.

<Comparative Example 9>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 6 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of olive oil. The results are shown in Table 2.

<Comparative Example 10>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 6 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of jojoba oil was used. The results are shown in Table 1.

FIG. 2 is an image of observing the emulsified composition obtained by stirring chitin nanofibers and silicone oil, liquid paraffin, squalane, olive oil, and jojoba oil, which are Examples 9 to 13, for 72 hours. It is an image of the later emulsified composition.

<Example 17>
Using 80 g of silicone oil as an oil-soluble substance, an emulsified composition (D phase medium oil type (O / D type) emulsified composition) was prepared by the following procedure.

(1) 16 g of glycerin, an aqueous dispersion of nanofibers derived from crystalline cellulose (BiNFi-s (AFO-10010) manufactured by Sugino Machine Co., Ltd., nanofiber concentration derived from crystalline cellulose 10 wt%, average diameter 20 to 50 nm , The same applies to the following examples of nanofibers derived from crystalline cellulose) and 2 g of ion-exchanged water were added, and the mixture was stirred for 10 minutes to prepare a uniform mixture.
(2) Silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min with a three-one motor stirrer.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a D-phase medium oil type (O / D type) emulsified composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 3 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Example 18>
A D-phase medium oil type (O / D type) emulsified composition was prepared in the same manner as in Example 17 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of liquid paraffin was used, and the dispersion stability was evaluated. The results are shown in Table 3.

<Example 19>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Example 17 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of squalane was used. The results are shown in Table 3.

<Example 20>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Example 17 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of olive oil. The results are shown in Table 3.

<Example 21>
A D-phase medium oil type (O / D type) emulsified composition was prepared in the same manner as in Example 17 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of jojoba oil was used, and the dispersion stability was evaluated. The results are shown in Table 3.

<Comparative Example 11>
As Comparative Example 11, using 80 g of silicone oil as an oil-soluble substance, an emulsified composition (D phase medium oil type (O / D type) emulsified composition) was prepared by the following procedure.
(1) 16 g of glycerin (manufactured by Wako Pure Chemical Industries, Ltd.), 0.2 g of crystalline cellulose particles (average particle size 10 to 250 μm, aspect ratio (major axis / minor axis) less than 10) and 3.8 g of ion-exchanged water. Addition and stirring were carried out for 10 minutes to prepare a uniform mixture.
(2) Silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min with a three-one motor stirrer.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a self-emulsifying fat and oil composed of a D-phase medium oil type (O / D type) emulsifying composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 3 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Comparative Example 12>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 11 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of liquid paraffin was used. The results are shown in Table 3.

<Comparative Example 13>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 11 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of squalane was used. The results are shown in Table 3.

<Comparative Example 14>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 11 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of olive oil. The results are shown in Table 3.

<Comparative Example 15>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 11 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of jojoba oil was used. The results are shown in Table 3.

<Example 22>
Using 80 g of the same silicone oil as in Example 17 as the oil-soluble substance, an emulsified composition (D phase medium oil type (O / D type) emulsified composition) was prepared by the following procedure.
(1) To 16 g of glycerin, 3 g of the crystalline cellulose-derived nanofiber aqueous dispersion used in Example 17 and 1 g of ion-exchanged water were added, and the mixture was stirred for 10 minutes to prepare a uniform mixture.
(2) Silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min with a three-one motor stirrer.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a self-emulsifying fat and oil composed of a D-phase medium oil type (O / D type) emulsifying composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 3 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Example 23>
(1) To 16 g of glycerin, 2 g of an aqueous dispersion of nanofibers derived from crystalline cellulose and 52 g of ion-exchanged water were added, and the mixture was stirred for 10 minutes to prepare a uniform mixture.
(2) With a three-one motor stirrer, 30 g of silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a D-phase medium oil type (O / D type) emulsified composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 3 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Example 24>
(1) To 16 g of glycerin (manufactured by Wako Pure Chemical Industries, Ltd.), 2 g of an aqueous dispersion of nanofibers derived from crystalline cellulose and 32 g of ion-exchanged water were added, and the mixture was stirred for 10 minutes to prepare a uniform mixture. did.
(2) 50 g of silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min with a three-one motor stirrer.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a D-phase medium oil type (O / D type) emulsified composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 3 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Example 25>
Using 80 g of the same liquid paraffin as in Example 18 as the oil-soluble substance, an emulsified composition (D phase medium oil type (O / D type) emulsified composition) was prepared by the following procedure.
(1) To 16 g of glycerin, 3 g of the crystalline cellulose-derived nanofiber aqueous dispersion used in Example 17 and 1 g of ion-exchanged water were added, and stirring was performed for 10 minutes to prepare a uniform mixture.
(2) Liquid paraffin was added to the mixture prepared in (1) at a rate of 5 ml / min with a three-one motor stirrer.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a self-emulsifying fat and oil composed of a D-phase medium oil type (O / D type) emulsifying composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 3 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Example 26>
A D-phase medium oil type (O / D type) emulsified composition was prepared in the same manner as in Example 25 except that 80 g of liquid paraffin was used as the oil-soluble substance and 80 g of squalane was used, and the dispersion stability was evaluated. The results are shown in Table 3.

<Example 27>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Example 25 except that 80 g of liquid paraffin was used as an oil-soluble substance and 80 g of olive oil. The results are shown in Table 3.

<Example 28>
A D-phase medium oil type (O / D type) emulsified composition was prepared in the same manner as in Example 25 except that 80 g of liquid paraffin was used as the oil-soluble substance and 80 g of jojoba oil was used, and the dispersion stability was evaluated. The results are shown in Table 3.

FIG. 4 is an image of observing the emulsified composition obtained by stirring the nanofibers derived from crystalline cellulose and each of silicone oil, liquid paraffin, squalane, olive oil, and jojoba oil, which are Examples 17 to 21. Yes, it is an image of the emulsified composition after 72 hours.
FIG. 5 observed the emulsified composition obtained by stirring the nanofibers derived from crystalline cellulose and each of silicone oil, liquid paraffin, squalane, olive oil, and jojoba oil, which are Examples 22 and 25 to 28. It is an image, and is an image of an emulsified composition after 72 hours.

<Example 29>
Using 80 g of silicone oil as an oil-soluble substance, an emulsified composition (D phase medium oil type (O / D type) emulsified composition) was prepared by the following procedure.

(1) 16 g of glycerin (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd., the same applies to the following examples), nanofiber aqueous dispersion derived from powdered cellulose (BiNFi-s (WFO-10010) manufactured by Sugino Machine Co., Ltd.), Add 2 g each of nanofibers derived from powdered cellulose (nanofiber concentration 10 wt%, average diameter 20-50 nm, the same applies to the following examples of nanofibers derived from powdered cellulose) and ion-exchanged water, and stir for 10 minutes to obtain a uniform mixture. Was produced.
(2) Silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min with a three-one motor stirrer.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a D-phase medium oil type (O / D type) emulsified composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 4 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Example 30>
A D-phase medium oil type (O / D type) emulsified composition was prepared in the same manner as in Example 29 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of liquid paraffin was used, and the dispersion stability was evaluated. The results are shown in Table 4.

<Example 31>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Example 29 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of squalane was used. The results are shown in Table 4.

<Example 32>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Example 29 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of olive oil. The results are shown in Table 4.

<Example 33>
A D-phase medium oil type (O / D type) emulsified composition was prepared in the same manner as in Example 29 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of jojoba oil was used, and the dispersion stability was evaluated. The results are shown in Table 4.

<Comparative Example 16>
As Comparative Example 16, using 80 g of silicone oil as an oil-soluble substance, an emulsified composition (D phase medium oil type (O / D type) emulsified composition) was prepared by the following procedure.
(1) Add 0.2 g of powdered cellulose particles (average particle size 10 to 250 μm, aspect ratio (major axis / minor axis) less than 10) and 3.8 g of ion-exchanged water to 16 g of glycerin (manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.). Then, stirring was carried out for 10 minutes to prepare a uniform mixture.
(2) Silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min with a three-one motor stirrer.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a self-emulsifying fat and oil composed of a D-phase medium oil type (O / D type) emulsifying composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 4 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Comparative example 17>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 16 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of liquid paraffin was used. The results are shown in Table 4.

<Comparative Example 18>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 16 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of squalane was used. The results are shown in Table 4.

<Comparative Example 19>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 16 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of olive oil. The results are shown in Table 4.

<Comparative Example 20>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Comparative Example 16 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of jojoba oil was used. The results are shown in Table 4.

<Example 34>
Using 80 g of the same silicone oil as in Example 29 as the oil-soluble substance, an emulsified composition (D phase medium oil type (O / D type) emulsified composition) was prepared by the following procedure.
(1) 4 g of the nanofiber aqueous dispersion derived from powdered cellulose used in Example 29 was added to 16 g of glycerin, and the mixture was stirred for 10 minutes to prepare a uniform mixture.
(2) Silicone oil was added to the mixture prepared in (1) at a rate of 5 ml / min with a three-one motor stirrer.
(3) After completion of the addition, the mixture was stirred at 300 rpm for 15 minutes to obtain a self-emulsifying fat and oil composed of a D-phase medium oil type (O / D type) emulsifying composition. The dispersion stability of the prepared emulsified composition was evaluated. Table 4 shows the evaluation results together with the ratio (mass%) of each component in the emulsified composition.

<Example 35>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Example 34 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of liquid paraffin was used. The results are shown in Table 4.

<Example 36>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Example 34 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of squalane was used. The results are shown in Table 4.

<Example 37>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Example 34 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of olive oil. The results are shown in Table 4.

<Example 38>
A D-phase medium oil type (O / D type) emulsified composition was prepared and the dispersion stability was evaluated in the same manner as in Example 34 except that 80 g of silicone oil was used as the oil-soluble substance and 80 g of jojoba oil was used. The results are shown in Table 4.

FIG. 6 is an image of observing the emulsified composition obtained by stirring nanofibers derived from powdered cellulose and each of silicone oil, liquid paraffin, squalane, olive oil, and jojoba oil, which are Examples 29 to 33. , 72 hours later, is an image of the emulsified composition.
FIG. 7 is an image of observing the emulsified composition obtained by stirring nanofibers derived from powdered cellulose and each of silicone oil, liquid paraffin, squalane, olive oil, and jojoba oil, which are Examples 34 to 38. , 72 hours later, is an image of the emulsified composition.

From the above examples and the like, the emulsified composition of the present invention can be easily applied to retort foods, medical chemicals and cosmetics that require heat treatment, and, for example, when applied to cosmetics, it affects heat treatment. It is possible to incorporate the raw material to be received into the formulation, widen the range of the temperature control range, and obtain the effect of facilitating the temperature control.

Claims (5)

Polyhydric alcohols, the first aqueous medium, the biomass nanofibers, and contain an oil-soluble substance state, and are content above 20 wt% of the oil-soluble substance, D phase in-oil type (O / D type) der Emulsified composition. The emulsified composition according to claim 1, wherein the biomass nanofibers are silk nanofibers. The emulsified composition according to claim 1 or 2 , wherein the oil-soluble substance is at least one of a saturated hydrocarbon oil and a silicone oil. An oil-in-water (O / W type) emulsified composition containing the emulsified composition according to any one of claims 1 to 3 and a second aqueous medium. A cosmetic composition comprising the emulsified composition according to any one of claims 1 to 3 or the oil-in-water (O / W type) emulsified composition according to claim 4.

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