JP3535583B2 - Clear lotion - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a transparent lotion, and more particularly to improvement of its transparency.

[0002]

2. Description of the Related Art Conventionally, various cosmetic lotions having a semi-transparent appearance have been developed by blending an oil-based fine emulsion with an aqueous system. For example, in JP-A-63-132813, in a water / alcohol system in which an alcohol / (water + alcohol) weight ratio is 0.01 to 0.4, a lipophilic surfactant having an HLB of 7 or less and an HLB of 10 or more is used. A polyoxyethylene-added nonionic activator and a fine emulsion composed of oil are disclosed. Also, JP-A-59-33
206 is a liquid / paste polyglycerin fatty acid ester of 0.0 in water / alcohol system at room temperature.
A fine emulsion comprising 1-5% by weight is disclosed.

[0003]

However, cosmetics using these fine emulsions are translucent and have a rich usability by blending oily components, but on the other hand, they are strongly sticky due to the above-mentioned blended activator and have a feeling in use. It was desired to further improve. The present invention has been made in view of the above-mentioned problems of the prior art, and an object thereof is to provide a transparent cosmetic having high transparency and an excellent feeling in use despite blending with oil.

[0004]

[Means for Solving the Problems] In order to achieve the above-mentioned object, as a result of intensive studies by the present inventors, when an oil component is dispersed as a fine emulsion in an aqueous phase, a specific amphiphilic agent is used in the composition of the emulsion. It was found that excellent transparency and usability can be obtained by using an organic substance and a surfactant and further adding a polyhydric alcohol in the aqueous phase, and completed the present invention.

That is, the transparent lotion according to the present invention is
Amphiphiles-surfactants-water system
Form a gel and have a gel transition temperature of 67 ° C or higher
Amphiphiles and surfactants selected from among the oils
And water, wherein the amphipathic substance has a carbon chain length of 16
More than higher alcohols and / or higher fatty acids
The surfactant is a cationic surfactant or anion.
A surfactant, which comprises the amphipathic substance and the surfactant.
The oil phase is blended in an amount of ½ or more with respect to the total amount of the sexing agent, and 0.01 to 5% by weight of the fine emulsion formed of the amphipathic substance, the surfactant and the oil is dispersed in water. The water is characterized by containing 1 to 40% by weight of a polyhydric alcohol.

The structure of the present invention will be described in more detail below. Amphiphile and surfactant used in the amphiphile and the surfactant present invention, amphiphile - surfactant - it is necessary to form a specifically gels in aqueous, the amphiphile Is high with a carbon chain length of 16 or more
Consisting of a higher alcohol and / or a higher fatty acid, and having the above interface
Activators are cationic or anionic surfactants.
Become Especially when considering emulsion stability, gel
When it is -type, the stability is good, and the gel transition temperature is preferably 67 ° C or higher.
In addition, the fact that the gel is α-type means that the gel is 2
It can be identified by a strong single peak at 1.4 °.

As described above, as a combination of an amphipathic substance which forms a gel in an aqueous system and at room temperature or higher-a surfactant, behenic acid and / or behenyl alcohol (amphipathic substance)-
Behenic acid / potassium hydroxide fatty acid soap (surfactant),
Alternatively, stearic acid and / or stearyl alcohol (amphiphile) -stearic acid / potassium hydroxide fatty acid soap (surfactant), stearyl alcohol (amphiphile) -sodium cetyl sulfate (surfactant), behenyl alcohol A combination of (amphiphile) -behenyltrimethylammonium chloride (surfactant) and behenyl alcohol (amphiphile) -stearyltrimethylammonium chloride (surfactant) is preferable. In addition,
Emulsion stability can be further improved by using a combination having long carbon chain lengths and different chain lengths such as behenic acid and stearic acid.

[0008] Note that with a surfactant and amphipathic substance, per se are those having no common surfactant as the surfactant strongly hydrophobic, carbon chain length in the present invention
Higher fatty acids and / or higher aliphatic alcohols having a value of 16 or more
It's a call .

Oil Phase In the present invention, the oily component blended in the system is a liquid oil component,
It may be a solid oil, a semi-solid oil or a substance which is poorly soluble in water, for example, avocado oil, camellia oil, turtle oil, macadamia nut oil, corn oil, mink oil, olive oil, rapeseed oil, egg yolk oil, sesame oil, Persic. Oil, wheat germ oil, southern oil, castor oil, linseed oil, safflower oil, cottonseed oil, evening primrose oil, eno oil, soybean oil, peanut oil, teaseed oil, kaya oil, rice bran oil, cinnamon oil, Japanese kiri oil,
Liquid oils and fats such as jojoba oil, germ oil, triglycerin, glyceryl trioctanoate, glyceryl triisopalmitate, cocoa butter, coconut oil, horse fat, hardened coconut oil, palm oil,
Solid fats such as beef tallow, sheep fat, hardened beef tallow, palm kernel oil, lard, beef bone fat, mokuro kernel oil, hardened oil, beef tallow, mokuro, hydrogenated castor oil, beeswax, candelilla wax, cotton wax, carnauba wax, Bayberry wax, ivorot wax, whale wax, montan wax, nuka wax, lanolin, cabox wax, lanolin acetate, liquid lanolin, sugar cane wax, lanolin fatty acid isopropyl, hexyl laurate, reduced lanolin, jojoba wax, hard lanolin, shellac wax, P
Waxes such as OE lanolin alcohol ether, POE lanolin alcohol acetate, lanolin fatty acid polyethylene glycol, POE hydrogenated lanolin alcohol ether, liquid paraffin, ozokerite, squalene,
Hydrocarbons such as pristane, paraffin, ceresin, squalane, petrolatum, microcrystalline wax, isopropyl myristate, cetyl octanoate, octyldodecyl myristate, isopropyl palmitate, butyl stearate, hexyl laurate, myristyl myristate, decyl oleate. Hexyldecyl dimethyloctanoate, cetyl lactate, myristyl lactate, lanolin acetate, isocetyl stearate, isocetyl isostearate, cholesteryl 12-hydroxystearylate,
Ethylene glycol di-2-ethylhexylate, dipentaerythritol fatty acid ester, N-alkyl glycol monoisostearate, neopentyl glycol dicaprate, diisostearyl malate, glycerin di-2-heptylundecanoate, tri-2-ethylhexyl acid Trimethylolpropane, trimethylolpropane triisostearate, pentaerythritol tetra-2-ethylhexylate, glycerin tri-2-ethylhexylate, trimethylolpropane triisostearate, cetyl-2-ethylhexanoate, 2-ethylhexyl palmitate, Glycerin trimyristate, tri-2-heptylundecanoic acid glyceride, castor oil fatty acid methyl ester, oleic acid oil, cetostearyl alcohol, Setoguriseraido, palmitic acid -
2-heptylundecyl, diisopropyl adipate,
N-lauroyl-L-glutamic acid-2-octyldodecyl ester, di-2-heptylundecyl adipate, ethyl laurate, di-2-ethylhexyl separate, 2-hexyldecyl myristate, 2-hexyl palmitate Decyl, 2-hexyl adipate decyl, diisopropyl sebacylate, 2-ethylhexyl succinate, ethyl acetate, butyl acetate, amyl acetate, synthetic esters such as triethyl citrate, lauric acid, myristic acid, palmitic acid, stearic acid, Behenic acid (behenyl) acid, oleic acid, 12-hydroxystearic acid, undecylenic acid, tallic acid, lanolin fatty acid, isostearic acid, linoleic acid, linoleic acid, higher fatty acids such as eicosapentaenoic acid, lauric alcohol, cetyl alcohol, stearic acid Such as ril alcohol, behenyl alcohol, myristyl alcohol, oleyl alcohol, cetostearyl alcohol, monostearyl glycerene ether (batyl alcohol), 2-decyltetradecinol, lanolin alcohol, cholesterol, hexyldecanol, isostearyl alcohol, octyldodecanol, etc. Silicone oils such as linear or branched higher alcohols, dimethylpolysiloxane, methylphenylpolysiloxane, vitamin A and its derivatives, vitamin D and its derivatives, vitamin E and its derivatives, vitamin K and its derivatives, sterols , And natural and synthetic fragrances, and the like, and the melting point of which is lower than room temperature is distinguished from the liquid oil, and the melting point of which is higher than room temperature is distinguished from the solid and semi-solid oils.

Further, as substances which are poorly soluble in water, ubiquinone, vitamins such as vitamin P, chlorhexidine hydrochloride, trichlorocarbanilide, imegassan DP300
Sterilizing agents such as dexamethasone acetate, para-aminobenzoic acid (hereinafter abbreviated as PABA), N, N-dimethyl PAB
Examples thereof include UV absorbers such as A octyl ester and preservatives such as parabens. The amount of oil phase is amphipathic substance-
It is 1/2 times or more, preferably equal to or more than the total amount of the surfactant. When the amount of the oil phase is less than 1/2 of the total amount of the amphipathic substance-surfactant, the temporal stability of the emulsified state tends to deteriorate.

Formation of Fine Emulsion In the present invention, the particle size of the fine emulsion is 0.15.
It is preferably not more than μm, particularly preferably not more than 0.10 μm. If the particle size exceeds 0.15 μm, creaming may occur at low viscosity. The average particle size of the emulsion used here is measured by a dynamic light scattering method, and specifically, NICOMP-270 (HIAC / RO).
It is measured by YCO).

The transparent lotion of the present invention is an emulsifier capable of applying a stronger shearing force to a mixed dispersion containing the above-mentioned essential components than a homomixer, such as manton gourin, French press, colloid mill, microfluidizer, By processing with a strong shearing force such as an sonic emulsifier, its transparency and stability can be improved. Also, when using a high-pressure homogenizer such as Manton gourin, French press, microfluidizer, etc., 1000
The emulsification is preferably performed under a pressure of psi or more, more preferably 3000 psi or more.

The emulsification treatment according to the present invention may be carried out with the whole amount of the system or, in some cases, a part thereof may be treated and then diluted with water or another compound such as polyhydric alcohol. The temperature at the time of emulsification is preferably higher than the transition temperature of the gel formed by the surfactant and the amphipathic substance in the system together with water. In the present invention, the mechanism of emergence of a fine emulsion having a stable and unique usability is considered as follows.

That is, in the present invention, (1) an amphipathic substance-surfactant-an amphipathic substance and a surfactant selected from those capable of forming a gel in a water system at room temperature or higher; ) Oil and (3) water at least, and it is preferable that substantially all of the amphipathic substance and the surfactant are present at the oil droplet interface. Here, in an oil-in-water emulsion composition, it is generally considered that an amphipathic substance and a surfactant form a gel in an aqueous phase to solidify the base (Barry, B.W., JC
olloid Interface Sci. , 28,
82-91 (1968)). The state of gel formation in this oil-in-water emulsion composition is described as follows (Shoji Fukushima, Physical Chemistry of Cetyl Alcohol, Fragrance Journal, 1992, p112-116). In FIG. 1, an oil phase 12 is dispersed in a water phase 10, and a surfactant 14 and an amphipathic substance 16 are present at the boundary surface between the water phase 10 and the oil phase 12, The stabilization of the dispersed state of the oil phase 12 is attempted.

Further, a surfactant 14 and an amphipathic substance 16 are further present in the aqueous phase 10, and a part of the surfactant 14 and the amphipathic substance 16 has a lamella structure 18 in the aqueous phase. And a gel structure is built up. Such an oil-in-water emulsion composition is treated with an emulsifier having a strong shearing force to destroy the gel structure which is solidifying the base,
For example, as shown in FIG. 2, by forming a dispersion system (vesicle) 20 having a fine lamella structure, a low-viscosity liquid base material can be obtained (Yamaguchi Michihiro, Noda Akira, Nikka, 26-
32 (1989)). However, a system in which the lamella structure is finely dispersed has problems of destabilization such as generation of seeds due to aggregation and increase in viscosity due to restructuring of gel structure.

Therefore, the present inventors have proposed that the amphipathic substance 16
-Surfactant 14-Water 10-Oil 12 The emulsion particles of the oil-in-water emulsion composition are finely divided, and the amphipathic substance 16 and the surfactant 1 which form a gel in the aqueous phase.
4 to the emulsion particle interface to reduce the amount of gel in the aqueous phase, and a combination of an amphipathic substance and a surfactant that forms a stable gel, destroys the gel structure, and then hardly forms the gel structure again By selecting, it is possible to guarantee stability at the product level. That is, FIG.
As shown in (4), the amphipathic substance 16 and the surfactant 14 are almost entirely transferred to the interface of the oil droplet 12, so that the amphiphilic substance 16 and the surfactant 14 are stably retained at the emulsion particle interface. In addition, since there is no finely dispersed lamellar structure or the like in the aqueous phase 10, neither agglomeration nor restructuring of the gel structure can occur due to the aggregation. Therefore, the oil-in-water emulsion composition according to the present invention has an extremely low viscosity in the storage state, and has excellent production suitability and usability when taken out from the container.

In order to form the emulsion as described above, in the present invention, it is preferable that the amount of the amphipathic substance and the surfactant existing on the boundary surface is 90% or more in terms of area ratio by DSC. Further, it is preferable that the amphipathic substance and the surfactant are selected from those in which the transition temperature of the gel formed in the amphiphilic substance-surfactant-water system is 67 ° C or higher.

The fine emulsion particle size is 0.15 μm.
It is preferably m or less. Further, it is preferable that the oil phase is added in an amount of ½ or more of the total amount of the amphipathic substance and the surfactant. Further, the total amount of the amphipathic substance and the surfactant is preferably 0.2% by weight or more based on the aqueous phase. The amphipathic substance is preferably composed of a higher alcohol and / or a higher fatty acid having a carbon chain length of 16 or more. It is also preferable that the surfactant comprises a cationic surfactant or an anionic surfactant.

Polyhydric Alcohol In the present invention, the polyhydric alcohol is added in order to enhance the transparency of the lotion in which the unique fine emulsion is dispersed. As the polyhydric alcohol, ethylene glycol, propylene glycol, 1,3-butylene glycol, dipropylene glycol, glycerin, triglycerin, tetraglycerin and the like are preferable. The blending amount thereof depends on the concentration of the fine emulsion composed of the amphipathic substance-surfactant-oil content, and is preferably 1 to 40% by weight in the lotion. If it is blended at 40% by weight or more, stickiness may occur. Further, in relation to the fine emulsion, it is preferably 7 times or more the amount of the fine emulsion. If it is 7 times or less, improvement in transparency may be insufficient.

The same moisturizers as polyhydric alcohols, such as glucose, maltose, maltitol, fructose, sorbitol, are added to lotions.
Examples thereof include starch, decomposing sugar, starch decomposing sugar reducing alcohol and the like, but these have poor stability in the coexistence with a fine emulsion and easily deteriorate.

In the present invention, the aqueous phase contains, for example, vitamin B group, vitamin C and its derivatives, pantothenic acid and its derivatives, water-soluble active substances such as vitamins such as biotin, sodium glutamate, arginine, aspartic acid, Buffering agents such as citric acid, tartaric acid, lactic acid, E
In addition to a chelating agent such as DTA, an ultraviolet absorber and one or more kinds of various dyes can be blended.

[0022]

EXAMPLES The present invention will be described in more detail with reference to specific examples. The present invention is not limited to the examples below. Abundance of amphiphile and surfactant at the oil droplet interface As described above, the abundance of surfactant and amphiphile at the oil droplet interface and the residual amount in the aqueous phase of the present invention are It has a very serious effect on the physical properties of the aqueous solution. Then, the present inventors first of all, the following emulsion 1,
2, 3, and 4 were manufactured, and physical properties at the time of completion and changes with time were examined. That is, the amount of the amphipathic substance and the surfactant present at the oil droplet interface can be estimated by the change in the peak area of gel transition. Therefore, the measurement of transition temperature is suggested by scanning calorimeter (DSC), specifically DS
C120 (manufactured by Seiko Denshi Kogyo Co., Ltd.) was used, and the temperature at the apex of the endothermic peak observed in the obtained DSC heating curve was taken as the transition temperature.

[0023]

[Table 1] ────────────────────────────────────                                         Emulsion                               1 2 3 4 ──────────────────────────────────── 1) Behenyl alcohol 1.0 1.0 1.0 1.0 1.0 2) Stearyl alcohol 0.5 0.5 0.5 0.5 0.5 3) Behenic acid 0.5 0.5 0.5 0.5 0.5 4) Stearic acid 0.5 0.5 0.5 0.5 0.5 5) Liquid paraffin-5.0 5.0 5.0 6) KOH 0.15 0.15 0.15 0.15 7) 1,3-butylene glycol 10.0 10.0 10.0 10.0 10.0 8) Ion-exchanged water 15.0 15.0 15.0 15.0 9) Deionized water Remaining amount Remaining amount Remaining amount Remaining amount ────────────────────────────────────

(Production Method) Emulsion 1: (1) to (4) are stirred and mixed at 80 ° C. This is mixed with a mixed solution of (6) to (9) heated and dissolved at 70 ° C. with stirring, and treated with a homomixer at 80 ° C. Emulsions 2 to 4: (1) to (5) are mixed with stirring at 80 ° C. This is mixed with a mixture of (6) to (8) heated and dissolved at 70 ° C. with stirring, and at 80 ° C.,
Emulsion 2 was emulsified with a homomixer and then (9) was stirred and mixed. Emulsion 3 was emulsified with a high pressure homogenizer at a pressure of 500 psi and then (9) was stirred and mixed. Emulsion 4 was mixed with a high pressure homogenizer at a pressure of 7,000 psi. After emulsification, (9) was mixed with stirring to obtain samples having different fine emulsion particle sizes.

FIG. 4 shows the DS with the miniaturization of the emulsion.
The change in the C temperature rise curve is shown. In the figure, although emulsion 1 is a system in which oil was removed, a single transition peak was observed at 75 ° C. Since the emulsion is not formed in the system in which the oil is removed, the amphipathic substance and the surfactant form a gel in the aqueous phase, and this state is shown in the same figure. Emulsions 2, 3 and 4 were oil-blended systems, and the fine emulsion particle diameters were 1 to 10 μm, 0.24 μm and 0.07 μm, respectively. As the emulsified particles become finer, the peak on the high temperature side decreases in the DSC curve, and only the lowest temperature peak appears in Emulsion 4, and in the process of decreasing the particle size, the amphipathic substance and gel forming the gel in the aqueous phase and It is suggested that the surfactant migrates to the interface as the interfacial area of the emulsion increases, and both components in the aqueous phase decrease.

The average particle size of the emulsion was measured by microscopic observation when the particle size was 1 μm or more. When the average particle diameter is 1 μm or less, the measurement is performed by a dynamic light scattering method. Specifically, NICOMP-270 is used.
(Manufactured by HYAC / ROYCO) was used. The DSC curve of Emulsion 4 having an average particle size of 0.07 μm is 63 ° C.
Since there is only a single transition peak in the emulsion, most of the amphipathic substances and surfactants show a state in which they migrate to the interface of the emulsion, and as the particle size increases, the high temperature side The increase in the ratio of the peaks indicates that the amount of the gel constituents in the aqueous phase, that is, the amount of the amphipathic substance and the surfactant is increased. Here, in order to ensure the appearance of an aqueous solution and the stability at the product level, it is desirable that the DSC curve has only the low temperature side peak, but even if the high temperature side peak area is about 10% of the whole. good.

Emulsion 1, produced as described above,
The emulsion compositions of Nos. 2, 3 and 4 had the following physical properties.

[Table 2] ────────────────────────────────────                                   Emulsion                     1 2 3 4 ──────────────────────────────────── Fine emulsion particle size −1 to 10 μm 0.24 nm 0.07 nm ──────────────────────────────────── Immediately after viscosity 55 cps 220 cps 25 cps 12 cps     Appearance White turbid White turbid Slightly white turbid ──────────────────────────────────── 40 ° C 1 month later- ○ △ ○ Stability (turbidity rise, creaming) ────────────────────────────────────

As is clear from Table 2 above, emulsion 2 gives the feel of using a cream, but has a high viscosity and does not have the physical properties of an aqueous solution. Furthermore, emulsion 3
The transparency increases and the viscosity decreases, approaching the physical properties of an aqueous solution, but stability (such as generation of spots, increase in turbidity, and creaming over time) is maintained because the amphipathic substance and surfactant remain in the aqueous phase. Getting worse. On the other hand, the emulsion 4 is
It had a low viscosity, relatively high transparency, physical properties as an aqueous solution, and good stability.

Improvement of Transparency by Polyhydric Alcohol The inventors of the present invention investigated further improvement of transparency by using the above fine emulsion. That is, although the emulsion 4 has a relatively high degree of transparency, it does not go out of the semi-transparent region yet, and it is necessary to further increase the degree of transparency in order to enhance the commerciality of the lotion.

Therefore, the following fine emulsion was formed and added to an aqueous system, and the improvement of transparency by a polyhydric alcohol was examined. The fine emulsion formulation used in this study is as follows. (1) Behenyl alcohol 3.0% by weight (2) Behenic acid 2.0 (3) Liquid paraffin 16.0 (4) Butylparaben 0.4 (5) KOH 0.26 (6) Ethanol 10.0 (7) Ion-exchanged water The remainder <Production method> (1) to (4) are mixed with stirring at 70 ° C. This is added to a solution obtained by heating and dissolving the mixed solution of (5) to (7) at 70 ° C. with stirring to carry out preliminary emulsification. This emulsion was emulsified using a high pressure homogenizer at 75 ° C. under a pressure of 5000 psi to produce a fine emulsion. This fine emulsion was diluted with ion-exchanged water, and the relationship between transparency and addition of polyhydric alcohol was tested.

The results are shown in Table 3. In addition, in Table 3,
The amount of the fine emulsion is represented by the amount of the amphipathic substance, the surfactant and the oil content in (1) to (5), and the amount of the component (6),
(7) was added to the amount of ion-exchanged water. Ingredient (5) is consumed in forming the surfactant in the fine emulsion.
The stability over time was also examined by storing at 50 ° C for 1 month.

[Table 3] ─────────────────────────────────── Fine emulsion 0.005 0.01 0.1 1.0 5.0 Deionized water balance ─────────────────────────────────── Appearance (transparency) ○ △ △ △ × Usability   No stickiness ○ ○ ○ ○ △   Rich △ ○ ○ ○ ○ Stability over time ○ ○ ○ ○ ○ ───────────────────────────────────

As is clear from Table 3 above, the appearance and the feeling of use are in the relationship of a trade-off, and in the system of 0.005% of fine emulsion having an excellent appearance, there is no richness, and an excellent richness is obtained. In a system containing 0.01% or more of a fine emulsion that can be used, the transparency tends to decrease.

Therefore, the present inventors have examined the improvement of transparency by adding a polyhydric alcohol. The results are shown in Table 4.

[Table 4] ─────────────────────────────────── Fine emulsion 0.01 0.1 1.0 1.0 5.0 5.0 7.0 Dynamite Glycerin        3.0 3.0 5.0 10.0 20.0 25.0 40.0 1,3-Butylene recall---5.0 10.0 10.0 10.0 Deionized water balance ─────────────────────────────────── Appearance (transparency) ○ ○ △ ○ △ ○ ○ Usability   No stickiness ○ ○ ○ ○ ○ ○ ×   Rich ○ ○ ○ ○ ○ ○ ○ Stability over time ○ ○ ○ ○ ○ ○ ○ ───────────────────────────────────

As is clear from Table 4, even if the fine emulsion is 0.01% or more, the transparency can be improved by adding a polyhydric alcohol such as dynamite glycerin or 1,3-butylene glycol. it can.
However, if 40% or more of a polyhydric alcohol is blended, stickiness will occur, which is not preferable. Here, for example, even if the same fine emulsion 0.1% or 5.0% is seen, it is understood that the transparency changes depending on the amount of the polyhydric alcohol.
Therefore, the amount of fine emulsion was fixed to 1.0% and the amount of polyhydric alcohol was changed.

The results are shown in Table 5.

[Table 5] ─────────────────────────────────── Fine emulsion 1.0 Dynamite Glycerin        0.0 2.0 5.0 10.0 20.0 30.0 40.0 1,3-Butylene glycol 5.0 Deionized water balance ─────────────────────────────────── Appearance (transparency) △ ○ ○ ○ ○ ○ ○ Usability   No stickiness ○ ○ ○ ○ ○ ○ ×   Rich ○ ○ ○ ○ ○ ○ ○ Stability over time ○ ○ ○ ○ ○ ○ ○ ───────────────────────────────────

As is clear from the above table, the blending amount of the fine emulsion and the required blending amount of the polyhydric alcohol are closely related, and from Table 4, it can be seen that in the system of 5.0% or less of the fine emulsion, the polyhydric alcohol It is understood that the required blending amount is 7 times or more the blending amount of the fine emulsion.

Fine Emulsion Particle Size Next, the present inventors examined the correlation between the fine emulsion particle size of the oil phase according to the present invention, stability and appearance. That is, when the fine emulsion particle size of the oil phase, which is the internal phase of the emulsion composition according to the present invention, is large, the physical properties of the aqueous solution are impaired due to an increase in turbidity and an increase in viscosity, and stability (creaming, etc.) May worsen.

Therefore, the present inventors produced an emulsion based on the following formulation. At this time, emulsification was performed using manton-goulin, and the shearing force was adjusted to adjust each fine emulsion particle size. (1) Behenyl alcohol 1.0% (2) Stearyl alcohol 0.5% (3) Behenic acid 0.5% (4) Stearic acid 0.5% (5) Liquid paraffin 5.0% (6) Potassium hydroxide 0.15% (7) 1,3-butylene glycol 10.0% (8) Ion-exchanged water 10.0% (9) Ion-exchanged water Remaining amount (production method) Stirring (1) to (5) at 80 ° C Mix. This was mixed with a mixture of (6) to (8) heated and dissolved at 80 ° C. with stirring, and the mixture was emulsified at 80 ° C. using a homomixer and a high pressure homogenizer under various pressures, and then (9). Were mixed by stirring to obtain samples having different fine emulsion particle sizes. In the above formulation, behenic acid, stearic acid, and potassium hydroxide make a fatty acid soap, which functions as a surfactant.
Further, non-neutralized behenic acid, stearic acid, and behenyl alcohol and stearyl alcohol function as amphiphilic substances.

The results are shown in Table 6 below.

[Table 6] ──────────────────────────── Fine emulsion particle size Viscosity Stability ────────────────────────────   0.05μ 13.5cps ○   0.06μ 13.5cps ○   0.09μ 14.5cps ○   0.11μ 13.0cps ○   0.14μ 15.2cps ○ ────────────────────────────   0.17μ 17.1cps △   0.20μ 18.5cps △     1-5μ 37.0 cps × ────────────────────────────   Stability: Stability after 1 month was assessed visually.

As is clear from Table 6, the stability is extremely good up to a fine emulsion particle size of about 0.1 μm. When the particle size exceeds 0.15 μm, the stability deteriorates (creaming) and the appearance tends to be cloudy. Therefore, it is understood that the preferable fine emulsion particle size in the emulsion composition according to the present invention is 0.15 μm or less, particularly 0.10 μm or less.

The total amount of amphiphile and surfactant and oil
Amount Ratio Next, the present inventors examined the ratio of the total amount of amphiphile and surfactant to the amount of oil. That is, as described above, in the lotion according to the present invention, it is preferable that substantially all the amounts of the amphipathic substance and the surfactant are transferred to the oil droplet interface. There is a limit to the miniaturization of emulsified particles, and the interfacial area becomes relatively small when the amount of oil blended is small. Therefore, it becomes difficult to sufficiently transfer the amphipathic substance and the surfactant to the interface, and as a result, the gel constituent remains and the stability of the emulsion composition may be significantly deteriorated.

Therefore, an emulsion was prepared based on the following formulation, and the particle size and stability over time of each emulsion were examined.

[Table 7] ──────────────────────────────────── 1) Behenyl alcohol 1.0 1.0 1.0 1.0 1.0 1.0 1.0 2) Stearyl alcohol 0.5 0.5 0.5 0.5 0.5 0.5 0.5 3) Behenyl chloride   Trimethylammonium 1.0 1.0 1.0 1.0 1.0 1.0 1.0 4) Liquid paraffin 1.0 1.25 2.5 5 10 20 5) 1,3-butylene recall 15.0 15.0 15.0 15.0 15.0 15.0 6) Ion-exchanged water 15.0 15.0 15.0 15.0 15.0 15.0 7) Ion-exchanged water Remaining amount Remaining amount Remaining amount Remaining amount Remaining amount ──────────────────────────────────── Fine emulsion particle size 0.020 0.023 0.025 0.035 0.070 0.140 Stability over time × ○ ○ ○ ○ ○ ────────────────────────────────────

(Production method) (1), (2), (4) at 80 ° C.
Stir to mix. This is mixed with a mixture of (3), (5) and (6) heated and dissolved at 80 ° C. with stirring, and at 80 ° C. under a pressure of 5000 psi,
After emulsifying with a high-pressure homogenizer, (7) was stirred and mixed to obtain a sample. As is clear from Table 7, when the liquid paraffin as the oil phase was changed to 2.0 to 10.0% with respect to the total amount of the surfactant-amphipathic substance (2.5%), It is understood that the smaller the amount of liquid paraffin, the smaller the fine emulsion particle size, but rather the stability over time decreases, and the ratio of the total amount of surfactant-amphiphile to the oil phase is 1 /. It is suggested to be 0.5 or more, preferably 1/1 or more.

Composition of Amphiphile or Surfactant Next, the present inventors examined the composition of the surfactant and the amphiphile. That is, the surfactant and amphipathic substance used in the present invention is a surfactant-amphipathic substance-water system, it is necessary to form a gel in the temperature range of at least room temperature from the freezing point of the aqueous phase, Preferably the transition temperature of the gel is above 60 ° C. Here, generally, the transition temperature of the gel formed by the surfactant-amphiphile-water system is 10 to 20 ° C. higher than the temperature at which gel is not formed (begins to flow), and the transition temperature of 60 ° C. or higher. When it shows, it is considered that a gel can be formed at room temperature.

Therefore, changes in the characteristics due to the combination of the surfactant and the amphipathic substance with respect to the following basic composition were examined. Emulsified composition (1) Liquid paraffin 5.0 (2) Surfactant 1.0 (3) Amphiphile 1.5 (4) 1.3-BG 10.0 (5) Ion-exchanged water 20.0 (6) Ion-exchanged water balance gel (1) Surfactant 1.0 (2) Amphiphile 1.5 (3) Ion-exchanged water balance (manufacturing method) Emulsion composition: (1), (3) Are mixed by stirring at 70 to 80 ° C. Add the mixture of (2), (4) and (5) to 80 ℃
Add to the solution that was heated and dissolved with stirring with stirring to emulsify.
This emulsion was emulsified using a high pressure homogenizer at 70-80 ° C. under a pressure of 7000 psi, and then (6) was mixed by stirring to obtain a sample. Gel: (2) is stirred and mixed at 80 ° C. This is (1),
The mixed solution of (3) was heated and dissolved at 80 ° C., added while stirring, and treated with a homomixer to obtain a sample.

The results are shown in Tables 8-10. When two types of surfactants or amphipathic substances are described in each table, they are blended in a composition of 1: 1 by weight.

[Table 8] ──────────────────────────────────── Surfactant Sodium cetyl sulfate, sodium lauryl sulfate, behenyl chloride, stearyl chloride                                                 Trimethyl ammonium trimethyl ammonium Amphiphile behenyl alcohol behenyl alcohol behenyl alcohol behenyl alcohol                     Stearyl alcohol ──────────────────────────────────── Gel transition temperature 75 ℃ 68 ℃ 79 ℃ 77 ℃ Emulsion composition (40 ℃ ・ 1M) ○ ○ ○ ○ Stability (5 ℃ ・ 1M) ○ ○ ○ ○ ────────────────────────────────────

[Table 9] ──────────────────────────────────── Surfactant POE (15) Potassium behenate Potassium stearate Potassium stearate                     Oleyl ether potassium stearate Amphiphiles Cetyl alcohol Behenyl alcohol Behenyl alcohol Cetyl alcohol                     Stearyl alcohol Stearyl alcohol Stearyl alcohol Stearyl alcohol ──────────────────────────────────── Gel transition temperature 57 ° C 78 ° C 73 ° C 67 ° C Emulsion composition (40 ° C ・ 1M) × ○ ○ △ Stability (5 ℃ ・ 1M) △ ○ ○ ○ ────────────────────────────────────

[0047]

[Table 10] ──────────────────────────────────── Surfactant Potassium stearate Potassium stearate Potassium stearate                     Potassium palmitate Amphiphiles Cetyl alcohol Stearyl alcohol Cetyl alcohol                     Stearyl alcohol ──────────────────────────────────── Gel transition temperature 64 ℃ 69 ℃ 64 ℃ Emulsion composition (40 ° C / 1M) △ △ × Stability (5 ℃ ・ 1M) ○ ○ △ ────────────────────────────────────   Stability evaluation: Good                   △ Increased turbidity or formation of aggregates                   × Solidification

As is clear from the above Tables 8 to 10, the combination of the surfactant and the amphipathic substance is such that the combination having a high gel transition temperature is good in stability and the combination having different carbon chain lengths is used. If so, extremely good stability can be obtained. Specific examples of the composition according to the present invention are shown below. Example 1 Transparent lotion (1) Behenyl alcohol 0.6 (2) Behenic acid 0.4 (3) Liquid paraffin 2.0 (4) Vitamin E acetate Appropriate amount (5) Butylparaben 0.1 (6) KOH 0 .04 (7) Ethanol 5.0 (8) Fragrance 0.03 (9) Ion-exchanged water 15.0 (10) 1,3-Butylene glycol 10.0 (11) Trisodium edetate 0.01 (12) Ion-exchanged water The remaining amounts (1) to (5) are mixed with stirring at 70 ° C. This (6)
The mixed solution of (9) to (9) is heated and dissolved at 70 ° C. and added with stirring to emulsify. This emulsion was emulsified using a high pressure homogenizer at a pressure of 4000 psi at 75 ° C., and then (10) to (12) were mixed with stirring to obtain a transparent lotion.

[0049]

As described above, according to the transparent lotion according to the present invention, the amphipathic substance (higher fatty acid and / or
Are higher alcohols) and surfactants (cationic surfactants )
Agent or anionic surfactant) and a fine emulsion formed by an oil phase, and a polyhydric alcohol in an aqueous phase can provide a transparent cosmetic having both transparency and usability.

[Brief description of drawings]

FIG. 1 is a conceptual diagram of an emulsified state of a general oil-in-water emulsion composition.

FIG. 2 is an explanatory diagram of factors that deteriorate the emulsion stability of a general oil-in-water emulsion composition.

FIG. 3 is an explanatory diagram of an emulsified state of the transparent lotion according to the present invention.

FIG. 4 is an explanatory diagram of a DSC temperature rising curve of the transparent lotion according to the present invention.

─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Kenzo Ito 1050, Shinba-cho, Kohoku-ku, Yokohama-shi, Kanagawa Shiseido Daiichi Research Center Co., Ltd. (56) Reference JP-A-2-78432 (JP, A) JP-A 64-85906 (JP, A) JP-A 63-154606 (JP, A) JP-A 1-176446 (JP, A) JP-A 62-234540 (JP, A) JP-A 59-203633 (JP, A) JP 4-149112 (JP, A) JP 4-48925 (JP, A) JP 6-40849 (JP, A) JP 5-279651 (JP, A) Kai 63-126542 (JP, A) JP 63-270533 (JP, A) JP 5-194274 (JP, A) JP 6-271421 (JP, A) JP 7-267814 ( JP, A) JP 7-26244 (JP, A) JP 4-193814 (JP, A) HEI 4-11939 (JP, A) JP 61-271029 (JP, A) JP 63-154605 (JP, A) JP 61-54231 (JP, A) JP 63-305930 (JP , A) (58) Fields investigated (Int.Cl. ⁷ , DB name) A61K ^7/ 00-7/50

Claims (5)

(57) [Claims] 1. A gel is formed in an amphipathic substance-surfactant-water system at room temperature or higher, and the transition temperature of the gel is 67 ° C. or higher.
An amphipathic substance and a surfactant selected from the above , oil, and water, wherein the amphiphile is a higher alcohol having a carbon chain length of 16 or more.
Cole and / or higher fatty acid, and the surfactant is a cationic surfactant or an anionic interface.
An active agent, which is an oil relative to the total amount of the amphiphile and the surfactant.
The phase is mixed in an amount of ½ or more, and 0.01 to 5% by weight of a fine emulsion formed of the amphipathic substance, the surfactant and the oil is dispersed in water, and the polyhydric alcohol is contained in the water. A transparent lotion containing 1 to 40% by weight. 2. A transparent lotion according to claim 1, wherein the amount of polyhydric alcohol is at least 7 times the amount of the fine emulsion. 3. The lotion according to claim 1 or 2,
A transparent lotion characterized in that the amphipathic substance and the surfactant are present in the emulsion interface in a substantially total amount. 4. The lotion according to any one of claims 1 to 3, wherein the amount of the amphipathic substance and the surfactant existing on the boundary surface is 90% or more in terms of peak area ratio by DSC. A transparent lotion. 5. The lotion according to any one of claims 1 to 4 , wherein the fine emulsion particle size is 0.15 μm or less.