JP5053557B2 - Method for producing white turbid oil-in-water emulsified cosmetic - Google Patents

Description

  The present invention relates to a method for producing a white turbid oil-in-water emulsified cosmetic, particularly a method for producing a white turbid oil-in-water emulsified cosmetic having an average particle diameter of 100 to 500 nm and excellent stability even at low viscosity. Regarding improvements.

Conventionally, when trying to obtain nano-order (10 ^-9 m) fine emulsified droplets, a method using a strong mechanical shearing force by a high-pressure homogenizer typified by a microfluidizer or mantongaurin, or a coagulation method is called. A method of preparing an oil-in-water ultra-fine emulsion having a particle size of 50 nm or less and the like by cooling a one-component microemulsion of a nonionic surfactant and transferring to a two-liquid phase region is widely adopted ( For example, see Non-Patent Document 1 and Non-Patent Document 2.)
However, in the former manufacturing method using mechanical shearing force, when industrialized, a large amount of investment is required for equipment, and the maintenance cost increases. Furthermore, the consumption of electrical energy is enormous, and it is not a desirable method in the current situation where interest in environmental problems is increasing.

On the other hand, the latter production method by the aggregation method is desirable from the viewpoint of energy consumption, but even if nano-order emulsified droplets are obtained, the particle size is several tens of nanometers and the appearance is transparent to pale white emulsification. It becomes a thing. This two-phase microemulsion is often thermodynamically unstable.
As a recent consumer need, a cosmetic lotion-type cosmetic that can save labor by using lotion and emulsion as one cosmetic has been proposed (see, for example, Patent Document 1).
Petrochemistry, 37, 1012 (1988) J.Soc.Cosmet.Chem.Jpn., 23, 288 (1990) Japanese Patent No. 3656209

However, when the amount of oil to be blended is increased, the temporal stability of cosmetics becomes a problem, and the blending amount is limited. That is, the appearance of a skin cosmetic that has both a shabby feel like a lotion and a milky white appearance that gives a creamy feel to the emulsion and that has good stability is expected.
Accordingly, it has been desired to establish an emulsion composition that is milky white and has good stability even at low viscosity and that is suitable for industrialization.

  In view of the above circumstances, as a result of extensive studies by the present inventors, (A) a liquid agent at room temperature having a viscosity at 25 ° C. of 100 mPa · s or less, (B) a hydrogenated phospholipid, C) One or more nonionic surfactants having an HLB of 9 to 16 and selected from nonionic surfactants having a sterol skeleton, an alkyl ether skeleton, or a sorbitan fatty acid ester skeleton And (E) a white turbid oil-in-water emulsified cosmetic containing (D) a divalent glycol and (E) water, the components (A), (B) and (C) The water phase in which (D) :( E-1) was mixed at a mass ratio of 3: 7 to 7: 3 in the oil phase mixed and stirred at 0 ° C. was mixed with the mass of the oil phase: ((D) and ( E-1) total mass) = 1: 2 to 1: 5 so that the average particle size By providing a step of obtaining emulsified droplets having a diameter of 100 to 500 nm and a step of adding a uniform aqueous phase containing another aqueous component and (E-2) water and cooling to room temperature, the average of the emulsified droplets It was found that a milky white oil-in-water emulsified cosmetic having a particle size of 100 to 500 nm and having a milky white color having excellent stability even at low viscosity was obtained, and the present invention was completed.

That is, the method for producing a white turbid oil-in-water emulsified cosmetic according to the present invention contains the following components (A) to (E), and the average particle diameter of the emulsified droplets is 100 to 500 nm. In the method for producing a cloudy oil-in-water emulsified cosmetic,
(A) An oil agent having a viscosity at 25 ° C. of 100 mPa · s or less, liquid at room temperature (B) hydrogenated phospholipid (C) HLB is 9 to 16, and sterol skeleton, alkyl ether skeleton, sorbitan fatty acid ester One or more nonionic surfactants selected from nonionic surfactants having a skeleton (D) Divalent glycols (E) water The components (A), (B) and In the oil phase obtained by mixing and stirring (C) at 50 to 80 ° C., the water phase in which (D) :( E-1) was mixed at a mass ratio of 3: 7 to 7: 3 was used as the mass of the oil phase. : (The total mass of (D) and (E-1)) = step of obtaining emulsified droplets having an average particle diameter of 100 to 500 nm by adding so as to have a ratio of 1: 2 to 1: 5; Furthermore, a process of adding a homogeneous aqueous phase containing other aqueous components and (E-2) water to cool to room temperature And a step.

  In the method for producing the white turbid oil-in-water emulsified cosmetic, it is preferable that the emulsified cosmetic has a viscosity at 25 ° C. of 5 to 300 mPa · s.

  In the method for producing the white turbid oil-in-water emulsified cosmetic, the divalent glycol of component (D) is composed of propylene glycol, 1,3-butylene glycol, isoprene glycol, polyethylene glycol, and 1,2-pentanediol. It is preferable that it is 1 type, or 2 or more types selected from the group.

In the method for producing the white turbid oil-in-water emulsified cosmetic, it is preferable that the component (A) has a viscosity of 100 mPa · s or less at 25 ° C., and the blending amount of the liquid oil at room temperature is 1 to 10% by mass. It is.
Moreover, in the manufacturing method of the said white turbid oil-in-water type emulsified cosmetic, the blending amount of the component, (A) a liquid oil at room temperature and a viscosity of 100 mPa · s at 25 ° C. is 5 to 10% by mass. Is preferred.

  In the method for producing the white turbid oil-in-water emulsified cosmetic, the amount of component (B) hydrogenated phospholipid is preferably 0.1 to 1% by mass.

  In the method for producing the white turbid oil-in-water emulsified cosmetic, the component (C) HLB is 9 to 16, and the nonionic surfactant has a sterol skeleton, an alkyl ether skeleton, or a sorbitan fatty acid ester skeleton. It is preferable that the amount of the selected one or more nonionic surfactants is 0.1 to 1% by mass.

  In the method for producing the white turbid oil-in-water emulsified cosmetic, the amount of component (D) divalent glycols is preferably 5 to 20% by mass.

  Moreover, in the manufacturing method of the said cloudy oil-in-water type emulsion cosmetic, it is suitable that 5-20 mass% of component (F) ethanol is further included.

  In the method for producing the white turbid oil-in-water emulsified cosmetic, it is preferable that the component (G) further contains an anionic surfactant having phosphoric acid and / or a phosphate skeleton.

  According to the method for producing a white turbid oil-in-water emulsified cosmetic according to the present invention, a white turbid fine emulsification excellent in stability with an average particle diameter of emulsified droplets of 100 to 500 nm without using mechanical shearing force. It is possible to provide a composition, and in particular when it is used as a skin cosmetic, it is stable even at low viscosity, which gives both the feeling of shaving and the creamy feeling of emulsion with a single agent. A good oil-in-water emulsified skin cosmetic can be obtained.

The method for producing a white turbid oil-in-water emulsified cosmetic according to the present invention comprises a component (A) an oil agent having a viscosity at 25 ° C. of 100 mPa · s or less, a liquid at room temperature, (B) a hydrogenated phospholipid, and (C) 50 or more nonionic surfactants selected from nonionic surfactants having an HLB of 9 to 16 and having a sterol skeleton, alkyl ether skeleton, or sorbitan fatty acid ester skeleton An oil phase in which (D) divalent glycols: (E-1) water was mixed in a mass ratio of 3: 7 to 7: 3 in an oil phase mixed and stirred at -80 ° C was used. Mass: (the total mass of (D) and (E-1)) = step of obtaining emulsified droplets having an average particle diameter of 100 to 500 nm by adding so as to have a ratio of 1: 2 to 1: 5 Furthermore, a homogeneous aqueous phase containing other aqueous components and (E-2) remaining water is added. Characterized in that it comprises a step of cooling to room temperature with.
In the present invention, the appearance of the white turbid oil-in-water emulsified cosmetic exhibits milky white turbidity, and means about 5% or less when the transmittance is measured with a spectrophotometer.

The component (A) having a viscosity at 25 ° C. of 100 mPa · s or less, which is used in the present invention, may be any oil that is normally used as a raw material for cosmetics. Fatty acids, branched alcohols, ester oils, ether oils, silicone oils and the like can be used as appropriate.
Specifically, as the hydrocarbon oil, squalane (viscosity at 25 ° C., 32 mPa · s, hereinafter, only the viscosity value at 25 ° C. is indicated), squalene (35), liquid paraffin (43), α-olefin oligomer (45), Examples thereof include hydrogenated polyisobutene (45) and isoparaffin (30).
Examples of branched fatty acids and branched unsaturated alcohols include isostearic acid (77), isostearyl alcohol (56), octyldodecanol (57), hexyldecanol (41) decyltetradecanol (81), and oleyl alcohol (33). Can be mentioned.
Further, as ester oils, 2-ethylhexyl 2-ethylhexanoate (11), isononyl 2-ethylhexanoate (12), diisobutyl adipate (6), di-2-ethylhexyl succinate (11), 2-ethylhexanoic acid Cetyl (13), 2-ethylhexanoic acid 2-hexyldecyl (11), di-2-ethylhexanoic acid neopentyl glycol (13), tri-2-ethylhexanoic acid trimethylolpropane (52), tri (capryl capric acid ) Glycerin (25), neopentyl glycol dicaprate (19), 2-ethylhexyl isononanoate (5), isononyl isononanoate (6), isodecyl isononanoate (7), isotridecyl isononanoate (12), hexyl laurate (6) ), Isopropyl myristate (5), myristic 2-hexyldecyl acid (5), 2-octyldodecyl myristate (28), isopropyl palmitate (7), 2-ethylhexyl palmitate (11), 2-hexyldecyl stearate (27), ethyl isostearate (8) ), Isopropyl isostearate (10), 2-hexyldecyl isostearate (34), isostearyl isostearate (38), isodecyl neopentanoate (4), isostearyl neopentanoate (16), octyldodecyl neopentanoate (15), 2-octyldodecyl dimethyloctanoate (25), 2-ethylhexyl hydroxystearate (64), 2-octyldecyl 12-stearyl stearate (89), oleyl oleate (28), 2-ethylhexyl salicylate (9) Dialkyl carbonate (55), and the like.
Examples of ether oils include dioctyl ether and polyoxyethylene / polyoxypropylene dimethyl ether.
Examples of the silicone oil include octamethyltrisiloxane (1), decamethyltetrasiloxane (1.5), decamethylcyclopentasiloxane (4), caprylmethicone (10), and methylpolysiloxane.

  One or more of the above-mentioned liquid oils at room temperature can be blended in the cloudy oil-in-water emulsified cosmetic according to the present invention. The compounding quantity of a component (A) becomes like this. Preferably it is 1-10 mass%, More preferably, it is 5-10 mass%. If it is less than 1% by mass, the moist feeling and softness imparted to the skin, which are the effects of an emulsion, will not be satisfactory, and if it exceeds 10% by mass, there will be a problem with stability as an emulsified cosmetic. Occurs.

Component (B) hydrogenated phospholipid used in the present invention preferably has an iodine value of 40 or less. For example, natural lecithin such as soybean lecithin and egg yolk lecithin is hydrogenated according to a conventional method, phosphatidylcholine, phosphatidyl. What hydrogenated ethanolamine, phosphatidylserine, etc. are mentioned. Hydrogenated phospholipids have improved stability due to fewer unsaturated groups, and when they are blended into cosmetics, they are more stable against heat and oxidation.
Commercially available products include NIKKOL Resinol S-10, NIKKOL Resinol S-10E, NIKKOL Resinol S-10EX, NIKKOL Resinol S-10M, NIKKOL Resinol S-PIE (above, Nikko Chemicals Co., Ltd.), COATSOME NC-21, COATSOME NC-61 (manufactured by Nippon Oil & Fats Co., Ltd.), SLP-White H (manufactured by Sakai Oil Co., Ltd.) and the like.

  In addition, the hydrogenated phospholipid has a high purity with a high content of phosphatidylcholine, and is more excellent in terms of stability when used as a cosmetic. It is relatively expensive as an industrial material. In the present invention, the purity of the hydrogenated phospholipid is not limited, and an oil-in-water emulsion cosmetic having excellent stability is obtained by appropriately combining the nonionic surfactant of the component (C) blended together. It is possible to get a fee.

  One or two or more of the above hydrogenated phospholipids can be combined and blended in the cloudy oil-in-water emulsion cosmetic according to the present invention. It is preferable that the compounding quantity of a component (B) is 0.1-1 mass%. If it is less than 0.1% by mass, it becomes difficult to make the emulsified particle diameter of the emulsified skin cosmetic of the present invention 100 to 500 nm, which is not suitable. Moreover, when it mixes exceeding 1 mass%, the crystal | crystallization of hydrogenated phospholipid may arise and it is unpreferable.

  Next, the component (C) nonionic surfactant used in the present invention will be described. In the present invention, a nonionic surfactant having a sterol rule ether skeleton, an alkyl ether skeleton, or a sorbitan fatty acid ester skeleton having an HLB of 9 to 16 is suitable. Specific examples include the following.

Examples of the sterol ether skeleton include polyoxyethylene cholesteryl ether and polyoxyethylene phytosterol ether. Examples of commercially available products include EMALEX CS-10 (polyoxyethylene (10 mol) cholesteryl ether, HLB; 10), EMALEX CS-15 (polyoxyethylene (15 mol) cholesteryl ether, HLB; 11) manufactured by Nippon Emulsion Co., Ltd. ), EMALEX CS-20 (polyoxyethylene (20 mol) cholesteryl ether, HLB; 12), EMALEX CS-24 (polyoxyethylene (24 mol) cholesteryl ether, HLB; 13), EMALEX CS-30 (polyoxyethylene) (30 mol) cholesteryl ether, HLB; 14) and the like.
NIKKOL BPS-5 (polyoxyethylene (5 mol) phytosterol, HLB; 9.5), NIKKOL BPS-10 polyoxyethylene (10 mol) phytosterol, HLB; 12.5), NIKKOL BPS, manufactured by Nikko Chemicals Co., Ltd. -20 polyoxyethylene (20 mol) phytosterol, HLB; 15.5).

Examples of alkyl ether skeletons include polyoxyethylene cetyl ether, polyoxyethylene oleyl ether, polyoxyethylene stearyl ether, polyoxyethylene lauryl ether, polyoxyethylene isocetyl ether, polyoxyethylene isostearyl ether, polyoxyethylene octyl Examples include dodecyl ether, polyoxyethylene behenyl ether, polyoxyethylene decyl tetradecyl ether, and polyoxyethylene / polyoxypropylene decyl ether.
Examples of commercially available products include EMALEX 107 (polyoxyethylene (7 mol) cetyl ether, HLB; 10), EMALEX 110 (polyoxyethylene (10 mol) cetyl ether, HLB; 11), EMALEX 112 manufactured by Nippon Emulsion Co., Ltd. (Polyoxyethylene (12 mol) cetyl ether, HLB; 12), EMALEX 115 (Polyoxyethylene (15 mol) cetyl ether, HLB; 12), EMALEX 117 (Polyoxyethylene (17 mol) cetyl ether, HLB; 13) ), EMALEX 120 (polyoxyethylene (20 mol) cetyl ether, HLB; 14), EMALEX 125 (polyoxyethylene (25 mol) cetyl ether, HLB; 15), EMALEX 130 (polyoxyethylene (30 mol) cetyl ether , HLB; 15), EMALEX 508 (polyoxyethylene (8 mol) oleyl ether, HLB; 10), EMALEX 510 (polyoxyethylene (10 mol) oleyl Tel, HLB; 11), EMALEX 512 (polyoxyethylene (12 mol) oleyl ether, HLB; 11), EMALEX 515 (polyoxyethylene (15 mol) oleyl ether, HLB; 12), EMALEX 520 (polyoxyethylene ( 20 mol) oleyl ether, HLB; 13), EMALEX 523 (polyoxyethylene (23 mol) oleyl ether, HLB; 14), EMALEX 550 (polyoxyethylene (50 mol) oleyl ether, HLB; 16), EMALEX 608 ( Polyoxyethylene (8 mol) stearyl ether, HLB; 10), EMALEX 611 (polyoxyethylene (11 mol) stearyl ether, HLB; 11), EMALEX 615 (polyoxyethylene (15 mol) stearyl ether, HLB; 12) , EMALEX 620 (polyoxyethylene (20 mol) stearyl ether, HLB; 13), EMALEX 625 (polyoxyethylene (25 mol) stearyl Ether, HLB; 14), EMALEX 630 (polyoxyethylene (30 mol) stearyl ether, HLB; 15), EMALEX 640 (polyoxyethylene (40 mol) stearyl ether, HLB; 16), EMALEX 705 (polyoxyethylene ( 5 mol) lauryl ether, HLB; 10), EMALEX 707 (polyoxyethylene (7 mol) lauryl ether, HLB; 11), EMALEX 709 (polyoxyethylene (9 mol) lauryl ether, HLB; 12), EMALEX 712 ( Polyoxyethylene (12 mol) lauryl ether, HLB; 13), EMALEX 715 (polyoxyethylene (15 mol) lauryl ether, HLB; 14), EMALEX 720 (polyoxyethylene (20 mol) lauryl ether, HLB; 15) , EMALEX 725 (polyoxyethylene (25 mol) lauryl ether, HLB; 16), EMALEX 730 (polyoxyethylene (30 mol) lauryl ether) HLB; 16), EMALEX 1610 (polyoxyethylene (10 mol) isocetyl ether, HLB; 11), EMALEX 1615 (polyoxyethylene (15 mol) isocetyl ether, HLB; 13), EMALEX 1620 (polyoxyethylene ( 20 mol) isocetyl ether, HLB; 14), EMALEX 1625 (polyoxyethylene (25 mol) isocetyl ether, HLB; 15), EMALEX 1810 (polyoxyethylene (10 mol) isostearyl ether, HLB; 11), EMALEX 1815 (polyoxyethylene (15 mol) isostearyl ether, HLB; 12), EMALEX 1820 (polyoxyethylene (20 mol) isostearyl ether, HLB; 13), EMALEX 1825 (polyoxyethylene (25 mol) isostearyl Ether, HLB; 14), EMALEX OD-10 (polyoxyethylene (10 mol) octyldodecyl ether, HLB; 10), EMALEX OD-16 (poly Xylethylene (16 mol) octyldodecyl ether, HLB; 12), EMALEX OD-20 (polyoxyethylene (20 mol) octyldodecyl ether, HLB; 13), EMALEX OD-25 (polyoxyethylene (25 mol) octyldodecyl ether) HLB; 14), EMALEX OD-25JJ (polyoxyethylene (25 mol) octyldodecyl ether, HLB; 14), EMALEX BHA-10 (polyoxyethylene (10 mol) behenyl ether, HLB; 10), EMALEX BHA- 20 (polyoxyethylene (20 mol) behenyl ether, HLB; 13), EMALEX BHA-30 (polyoxyethylene (30 mol) behenyl ether, HLB; 14), EMALEX 2410 (polyoxyethylene (10 mol) decyltetradecyl) Ether, HLB; 9), EMALEX 2415 (polyoxyethylene (15 mol) decyltetradecyl ether, HLB; 11), EMALEX 2420 (polyoxyethylene) (20 mol) decyl tetradecyl ether, HLB; 12), EMALEX 2425 (polyoxyethylene (25 mol) decyl tetradecyl ether, HLB; 13), EMALEX DAPE-0205 (polyoxyethylene (5 mol) polyoxypropylene (2 mol) Decyl ether, HLB; 9), EMALEX DAPE-0207 (Polyoxyethylene (7 mol) Polyoxypropylene (2 mol) Decyl ether, HLB; 11), EMALEX DAPE-0210 (Polyoxyethylene (10 mol) ) Polyoxypropylene (2 mol) decyl ether, HLB; 12), EMALEX 0212 (polyoxyethylene (12 mol) polyoxypropylene (2 mol) decyl ether, HLB; 13), EMALEX 0215 (polyoxyethylene (15 mol) ) Polyoxypropylene (2 mol) decyl ether, HLB; 13), EMALEX 0220 (polyoxyethylene (20 mol) polyoxypropylene 2 moles) decyl ether, HLB; 14), EMALEX 0230 (polyoxyethylene (30 mol) polyoxypropylene (2 mol) decyl ether, HLB; 16), and the like.

NIKKOL BL-2 (polyoxyethylene (2 mol) lauryl ether, HLB; 9.5), NIKKOL BL-4.2 (polyoxyethylene (4.2 mol) lauryl ether, HLB; 5), NIKKOL BL-9EX (polyoxyethylene (9 mol) lauryl ether, HLB; 14.5), NIKKOL BC-5.5 (polyoxyethylene (5.5 mol) cetyl ether, HLB; 10.5), NIKKOL BC-7 (polyoxyethylene (7 mol) cetyl ether, HLB; 11.5), NIKKOL BC-10TX (polyoxyethylene (10 mol) cetyl ether, HLB; 13.5), NIKKOL BC-15TX (polyoxy Ethylene (15 mol) cetyl ether, HLB; 15.5), NIKKOL BS-4 (polyoxyethylene (4 mol) stearyl ether, HLB; 9.0), NIKKOL BO-7V (polyoxyethylene (7 mol) oleyl) Ether, HLB; 10.5), NIKKOL BO-10V ( Reoxyethylene (10 mol) oleyl ether, HLB; 14.5), NIKKOL BO-15V (polyoxyethylene (15 mol) oleyl ether, HLB; 16.0), NIKKOL BB-10 (polyoxyethylene (10 mol) ) Behenyl ether, HLB; 10.0), NIKKOL BB-20 (polyoxyethylene (20 mol) behenyl ether, HLB; 16.5), NIKKOL BD-2 (polyoxyethylene (2 mol) (C12-15) Alkyl ether, HLB; 9.0), NIKKOL BD-4 (polyoxyethylene (4 mol) (C12-15) alkyl ether, HLB; 10.5), NIKKOL BD-10 (polyoxyethylene (10 mol) ( C12-15) alkyl ether, HLB; 15.5) and the like.
The products made by Toho Chemical Industry Co., Ltd. include Pegnol L-4 (polyoxyethylene (4 mol) lauryl ether, HLB; 9.7), Pegnol TH-8 (polyoxyethylene (8 mol) lauryl ether, HLB; 12.9), pegnol L-9A (polyoxyethylene (9 mol) lauryl ether, HLB; 13.6), pegnol L-12S (polyoxyethylene (12 mol) lauryl ether, HLB; 14.8), pegnol T-6 (polyoxyethylene (6 mol) tridecyl ether, HLB; 11.4), peganol TE-10A (polyoxyethylene (10 mol) tridecyl ether, HLB; 14.1), peganol ST-7 ( Polyoxyethylene (7 mol) (C12-14) alkyl ether, HLB; 12.8), pegnol ST-12 (polyoxyethylene (12 mol) (C12-14) alkyl ether, HLB; 3.2), pegnol O-6A (polyoxyethylene (6 mol) oleyl ether, HLB; 9.6), pegnol O-107 (polyoxyethylene (7 mol) oleyl ether, HLB; 10.7), pegnol O-16A (polyoxyethylene (16 mol) oleyl ether, HLB; 14.5), peganol O-20 (polyoxyethylene (20 mol) oleyl ether, HLB; 15.4), peganol C-18 (polyoxy) And ethylene (18 mol) cetyl ether, HLB; 15.3).

Examples of sorbitan fatty acid ester skeletons include sorbitan fatty acid esters and polyoxyethylene sorbitan fatty acid esters.
Specifically, EMALEX SPE-100S (Sorbitan stearate, HLB; 9), EMALEX SPO-100 (Sorbitan oleate, HLB; 9), EMALEX SPIS-100 (Sorbitan isostearate) manufactured by Nippon Emulsion Co., Ltd. HLB; 10), EMALEX ET-2020 (monococonut oil fatty acid polyoxyethylene (20 mol) sorbitan, HLB; 15), EMALEX ET-8020 (polyoxyethylene (20 mol) sorbitan monooleate, HLB; 14), And EMALEX ET-8040 (polyoxyethylene (40 mol) sorbitan monooleate, HLB; 16).
NIKKOL TP-10V (polyoxyethylene (20 mol) sorbitan monopalmitate, HLB; 15.6), NIKKOL TS-10V (polyoxyethylene (20 mol) sorbitan monostearate), manufactured by Nikko Chemicals Co., Ltd. HLB; 14.9), NIKKOL TS-10MV (polyoxyethylene (20 mol) sorbitan monostearate, HLB; 14.9), NIKKOL TS-106V (polyoxyethylene (6 mol) sorbitan monostearate, HLB; 9.5), NIKKOL TS-30V (polyoxyethylene (20 mol) sorbitan tristearate, HLB; 10.5), NIKKOL TI-10V (polyoxyethylene (20 mol) sorbitan monoisostearate, HLB; 15. 0), NIKKOL TO-10V (polyoxyethylene monooleate (20 mol) sorbitan, HLB; 15.0), NIKKOL TO-10MV (polyoxymonooleate polyoxy) Tylene (20 mol) sorbitan, HLB; 15.0), NIKKOL TO-106V (polyoxyethylene monooleate (6 mol) sorbitan, HLB; 10.0), NIKKOL TO-30V (polyoxyethylene trioleate ( 20 mol) sorbitan, HLB; 11.0) and the like.
The products manufactured by Toho Chemical Industry Co., Ltd. include sorbon T-40 (polyoxyethylene (20 mol) sorbitan monolaurate, HLB; 15.7), sorbon T-60 (polyoxyethylene (20 mol) sorbitan monostearate). , HLB; 14.9), sorbon T-80 (polyoxyethylene (20 mol) sorbitan monooleate, HLB; 15.0), sorbon T-85 (polyoxyethylene (20 mol) sorbitan trioleate, HLB) 11.0) and the like.

  One or two or more nonionic surfactants having a sterol rule ether skeleton, an alkyl ether skeleton, or a sorbitan fatty acid ester skeleton having the above component (C) HLB of 9 to 16 can be used. It is preferable that the compounding quantity of a component (C) is 0.1-1 mass%. If it is less than 0.1% by mass, it is difficult to make the emulsified particle size of the emulsified skin cosmetic of the present invention 100 to 500 nm, which is inappropriate. Moreover, when it mixes exceeding 1 mass%, it will become easy to produce stickiness in a usability | use_condition.

Specific examples of component (D) divalent glycols used in the present invention include propylene glycol, 1,3-butylene glycol, isoprene glycol, polyethylene glycol, and 1,2-pentanediol. Of these, 1,3-butylene glycol is particularly preferably used. Further, the above divalent glycols may be used alone or in combination of two or more. In this invention, the suitable compounding quantity of a component (D) is 5-20 mass%. If it is less than 5% by mass, the average particle size of the emulsified droplets cannot be made 100 to 500 nm, and if it exceeds 20% by mass, problems may occur in terms of stability such as creaming and separation. There is not preferable.
In the present invention, the blending amount of component (D) divalent glycols is only the amount contained in the previously prepared emulsion composition, or the amount contained in the previously prepared emulsion composition and others. It may be any of the total amount to be blended as the aqueous component.

  In the present invention, (F) ethanol may be further blended. It is preferable that the compounding quantity of ethanol is 5-20 mass%. When the amount is less than 5% by mass, the effect of the skin lotion when the skin lotion and the emulsion are combined into one agent is inferior in refreshing and refreshing feeling, and more than 20% by mass is added. Even if the amount is increased, the improvement of the effect is not recognized, and there may be a problem in terms of stability.

  In the present invention, (G) an anionic surfactant having phosphoric acid and / or phosphate skeleton may be further blended. By blending component (G), a more turbid oil-in-water emulsified cosmetic can be obtained. Specific examples of the component (G) include the following.

  NIKKOL DLP-10 (dipolyoxyethylene (10 mol) sodium lauryl ether phosphate), NIKKOL DOP-8NV (dipolyoxyethylene (8 mol) sodium oleyl ether phosphate) manufactured by Nikko Chemicals Co., Ltd. NIKKOL DDP-2 (dipolyoxyethylene (2 mol) (C12-15) alkyl ether phosphate), NIKKOL DDP-4 (dipolyoxyethylene (4 mol) (C12-15) alkyl ether phosphate), NIKKOL DDP-6 (dipolyoxyethylene (6 mol) (C12-15) alkyl ether phosphate), NIKKOL DDP-8 (dipolyoxyethylene (8 mol) (C12-15) alkyl ether phosphate), NIKKOL DDP- 10 (dipolyoxyethylene (10 mol) (C12-15) alkyl ether phosphoric acid), NIKKOL TLP-4 (tripolyoxyethylene (4 mol) lauryl ether Acid), NIKKOL TCP-5 (tripolyoxyethylene (5 mol) cetyl ether phosphate), NIKKOL TOP-OV (trioleyl phosphate), NIKKOL TDP-2 (tripolyoxyethylene (2 mol) (C12-15) Alkyl ether phosphoric acid), NIKKOL TDP-6 (tripolyoxyethylene (6 mol) (C12-15) alkyl ether phosphoric acid), NIKKOL TDP-8 (tripolyoxyethylene (8 mol) (C12-15) alkyl ether phosphoric acid) ), NIKKOL TDP-10 (tripolyoxyethylene (10 mol) (C12-15) alkyl ether phosphoric acid) and the like.

  The amount of the anionic surfactant having the phosphoric acid and / or phosphate skeleton is preferably 0.01 to 0.5% by mass. If the amount is less than 0.01% by mass, the effect of blending the above components is not recognized, and even if the amount exceeds 0.5% by mass, the improvement of the effect due to the increase is not recognized.

  In the present invention, in addition to the above essential components, in a range that does not interfere with the object of the present invention, a fragrance, a pigment, an antiseptic, a bactericidal agent, a moisturizing agent, an ultraviolet absorber, and an ultraviolet scattering agent that are blended in ordinary lotions and emulsions. , Salts, chelating agents, thickeners, pearl agents, surfactants, oil agents, various agents, and the like can be appropriately blended.

In the production method according to the present invention, an emulsion average particle diameter is 100 to 500 nm by adding a uniform aqueous phase containing other aqueous components to the emulsion phase containing the components (A) to (E). In addition, a highly stable emulsified cosmetic can be obtained even at low viscosity.
The other aqueous component is not particularly limited as long as it is an aqueous component having water or an aqueous solvent as a main medium. In addition to water or an aqueous solvent, components usually used in cosmetics, pharmaceuticals, etc. You may mix | blend with the compounding quantity of the range which does not affect stability.
In addition, in this invention, the compounding quantity of final (E) water is in the homogeneous water phase containing the compounding quantity of water (E-1) contained in the emulsion composition prepared previously, and another aqueous component. This corresponds to the sum of the amount of water (E-2) contained in the water. That is, (E) = (E-1) + (E-2).

Obtained by the production method of cloudy-like oil-in-water type emulsified cosmetic of the average particle diameter of the present invention, the average particle size of the emulsified droplets characterized in that it is a 100 to 500 nm. When it is an ultrafine emulsion of less than 100 nm, it is an appearance region that is different from milky white that exhibits transparency to translucency and gives a creamy feeling. In the present invention, in consideration of providing an oil-in-water type skin cosmetic intended for use in a single preparation of skin lotion and emulsion, preparation of emulsified droplets having a particle diameter of 100 to 500 nm that does not become transparent to translucent. It is carried out.

The measurement of the average particle diameter of the emulsified droplets is performed as follows, for example.
The test sample is diluted 200 times with ion-exchanged water and measured at 25 ° C. using FPAR-1000 (manufactured by Otsuka Electronics Co., Ltd.).

Viscosity The viscosity of the cosmetic obtained by the method for producing a cloudy oil-in-water emulsified cosmetic according to the present invention is characterized in that the viscosity at 25 ° C. is 5 to 300 mPa · s. If it exceeds 300 mPa · s, it is not preferable because the skin lotion as a lotion in the case of a skin cosmetic in which lotion and emulsion are combined into one agent is not obtained. Moreover, since it may lack the moist feeling as an emulsion as it is less than 5 mPa * s, a suitable viscosity is 5-300 mPa * s.
According to the production method of the present invention, it is possible to provide a white turbid oil-in-water emulsified cosmetic having good stability without creaming even in a composition having a relatively low viscosity within the above range.

In the present invention, the viscosity is measured as follows, for example.
Using a digital bismetholone viscometer VDA2 (manufactured by Shibaura System Co., Ltd.), the test sample placed in a measurement container is immersed in a constant temperature water bath at 25 ° C. for 1 hour and then measured.

Hereinafter, the principle of the present invention will be described with reference to an example of a method for producing a white turbid oil-in-water emulsified cosmetic according to the present invention.
Production Example (Step 1) (A) An oil agent having a viscosity at 25 ° C. of 100 mPa · s or less, liquid at room temperature, (B) hydrogenated phospholipid, (C) HLB is 9 to 16, and An oil phase obtained by mixing and stirring at 50 to 80 ° C. with one or two or more nonionic surfactants selected from nonionic surfactants having a sterol skeleton, an alkyl ether skeleton, and a sorbitan fatty acid ester skeleton (D) Divalent glycols: (E) Water phase mixed at a mass ratio of 3: 7 to 7: 3 at 50 to 80 ° C., and oil phase mass: ((D) and The total mass of (E-1)) is added so as to have a ratio of 1: 2 to 1: 5, and an emulsion having a milky white color with an average particle diameter of the emulsified droplets of 100 to 500 nm is obtained.
(Step 2) While stirring the emulsion, a uniform aqueous phase containing other aqueous components at room temperature and (E-2) water is added to obtain the desired white turbid oil-in-water emulsion cosmetic.
At this time, when the viscosity of the obtained cosmetic at 25 ° C. was measured, it was confirmed to be 5 to 300 mPa · s.

Principle (A) An oil agent having a viscosity at 25 ° C. of 100 mPa · s or less, liquid at room temperature, (B) hydrogenated phospholipid, (C) HLB of 9 to 16, and sterol skeleton, alkyl ether In an oil phase obtained by mixing and stirring one or more nonionic surfactants selected from nonionic surfactants having a skeleton and a sorbitan fatty acid ester skeleton, (D) a divalent glycol When a mixed water phase of water and (E-1) water is added, a slightly viscous pale white transparent phase is formed as an initial stage. This is because the water-in-oil type (W / O) emulsified state in the process of adding the aqueous phase to the oil phase changes due to the change in the spacing between the adjacent surfactant molecules as the proportion of the aqueous phase increases. This is presumably due to the formation of lamella liquid crystals.

If a uniform aqueous phase containing other aqueous components at room temperature and (E-2) water is added at the time of liquid crystal formation, a W / O / W type multiple emulsion is produced. This multiple emulsion often has low stability due to problems such as coalescence.
Therefore, in the present invention, after the liquid crystal is formed, the addition of (D) a divalent glycol: (E-1) mixed water phase of water is continued to form an oil-in-water (O / W) emulsion. . This emulsion is milky white in appearance and is confirmed to be 5% or less when the transmittance is measured with a spectrophotometer.
Moreover, when the average particle diameter of this emulsion is measured with the particle size distribution analyzer FPAR-1000 (made by Otsuka Electronics Co., Ltd.), it is recognized that it is an emulsified droplet in the range of 100 to 500 nm.
In the step of preparing the emulsion, the heating temperature during mixing and stirring is preferably 50 to 80 ° C.

  In order to obtain the emulsion having a milky white color, the aqueous phase added to the oil phase is a mixed aqueous phase of (D) divalent glycols: (E-1) water. The cloud point of the nonionic surfactant contained can be raised and emulsification can be improved.

After the milky white emulsion is generated, as a second step, a uniform aqueous phase containing other aqueous components at room temperature and the remaining water (E-2) is added to the milky white emulsion. Then, by cooling to room temperature, the desired cloudy oil-in-water emulsified cosmetic can be obtained.
The viscosity of the obtained cosmetic belongs to the low-viscosity region prescribed as a lotion.
An oil-in-water emulsion that exhibits a milky white color is generally stable over time in a relatively viscous composition such as an emulsion or cream, but in a low-viscosity composition, due to creaming, The problem is that separation is likely to occur.

However, in the present invention, since the emulsion droplets having an average particle diameter of 100 to 500 nm or less are prepared in advance by the above production method, oil-in-water is unlikely to cause creaming even if the aqueous phase is added to lower the viscosity thereafter. Type emulsified cosmetics.
In addition, the white turbid oil-in-water emulsified cosmetic obtained as described above can be easily produced by simply mixing and stirring without using a special device such as a high-pressure emulsifier during emulsification. .

  The white turbid oil-in-water emulsified cosmetic obtained by the production method according to the present invention is a skin cosmetic in which lotion and emulsion are combined into one agent, a skin care product such as a cosmetic liquid, after-shave lotion, hair nick, hair liquid, It can also be used for hair cosmetics such as hair nourishing and hair styling.

EXAMPLES Hereinafter, although an Example is given concretely and this invention is demonstrated in more detail, this invention is not limited by these Examples.
1. Production method of white turbid oil-in-water emulsified cosmetic First, an example of producing an oil-in-water cosmetic used in the present invention will be described. The blending ratio (mass%) of each component described in the description of the following production examples is a value relative to the total amount of the cosmetic composition.
Production Example 1-1
(A) Liquid paraffin 5 mass%, isostearic acid 0.5 mass%, cetyl 2-ethylhexanoate 1 mass%, (B) hydrogenated phospholipid 0.4 mass%, (C) non As an ionic surfactant, polyoxyethylene (10 mol) phytosterol ether 0.4% by mass and perfume 0.1% by mass were mixed and dissolved at 70 ° C. (oil phase). On the other hand, (D) 1,3-butylene glycol as a divalent glycol and (E-1) water were mixed at a ratio of 1: 1 at 70 ° C. to obtain a uniform aqueous phase, and the mass of the oil phase: ((D ) And (E-1) were added to the oil phase so as to have a ratio of 1: 2.7 to obtain a milky white emulsion.
Subsequently, while stirring the emulsion, a normal aqueous phase containing 0.01% by mass of edetate as another aqueous component, 0.5% by mass of phenoxyethanol, and the balance water (E-2) was added. And it cooled to normal temperature and obtained the target cloudy oil-in-water type emulsified cosmetic.

Production Example 1-2
(A) Liquid paraffin 5% by mass as liquid oil at normal temperature, 0.5% by mass isostearic acid and 1% by mass cetyl 2-ethylhexanoate, (B) Trade name NIKKOL S-10 (Nikko Chemicals) as hydrogenated phospholipid Co., Ltd., phosphatidylcholine content 25-30%) 0.4% by mass, (C) nonionic surfactant polyoxyethylene (10 mol) phytosterol ether 0.4% by mass, (E) water remaining, The fragrance | flavor 0.1 mass% was made into the state of solubilization by uniform stirring at 80 degreeC, and it cooled to 25 degreeC rapidly under the ice example.
Next, (D) 10% by mass of 1,3-butylene glycol, 0.01% by mass of edetate, and 0.5% by mass of phenoxyethanol were added as divalent glycols to obtain an oil-in-water skin cosmetic. .

Production Example 1-3
(A) Liquid paraffin 5% by mass as liquid oil at normal temperature, 0.5% by mass isostearic acid and 1% by mass cetyl 2-ethylhexanoate, (B) Trade name NIKKOL S-10 (Nikko Chemicals) as hydrogenated phospholipid Co., Ltd., phosphatidylcholine content 25-30%) 0.4% by mass, (C) polyoxyethylene (10 mol) phytosterol ether 0.4% by mass as a nonionic surfactant, (D) divalent glycol As a class, 1,3-butylene glycol 10% by mass, (E) water remaining, fragrance 0.1% by mass, edetate 0.01% by mass, phenoxyethanol 0.5% by mass is a microfluidic device that is a high-pressure emulsifier. Emulsification was performed using a Tizer (manufactured by Mizuho Kogyo Co., Ltd.) to obtain an oil-in-water type skin cosmetic.

Production Example 1-4
(A) Liquid paraffin 6% by mass as liquid oil at normal temperature, 0.5% by mass isostearic acid and 1% by mass cetyl 2-ethylhexanoate, (B) Trade name NIKKOL S-10 (Nikko Chemicals) as hydrogenated phospholipid Manufactured by Co., Ltd., phosphatidylcholine content 25-30%) 0.7% by mass, (C) polyoxyethylene (10 mol) phytosterol ether 1% by mass as a nonionic surfactant, tripolyoxyethylene as an anionic surfactant (4 mol) 0.2% by mass of lauryl ether phosphoric acid, 0.3% by mass of stearyl alcohol, and 0.1% by mass of fragrance were mixed and dissolved at 70 ° C. (oil phase). (E-1) water at 70 ° C. was added to the oil phase at a blending ratio of 20% by mass to obtain an emulsion having a milky white color.
Subsequently, while stirring the above emulsion, the other aqueous components 9% by mass of ethanol, 0.01% by mass of edetate, 0.5% by mass of phenoxyethanol, 0.5% by mass of dipropylene glycol, and the remaining water A room temperature uniform aqueous phase containing (E-2) was added and cooled to room temperature to obtain an oil-in-water skin cosmetic.

Production Example 1-5
(D) The same operation as in Production Example 1-1 was performed except that the ratio of 1,3-butylene glycol and (E-1) water as divalent glycols was 2: 8.

Production Example 1-6
(D) The same operation as in Production Example 1-1 was performed except that the ratio of 1,3-butylene glycol and (E-1) water as divalent glycols was 3: 7.

Production Example 1-7
(D) The same operation as in Production Example 1-1 was performed except that the ratio of 1,3-butylene glycol and (E-1) water as divalent glycols was 8: 2.

Production Example 1-8
(A) Liquid paraffin 5% by mass as liquid oil at normal temperature, 0.5% by mass isostearic acid and 1% by mass cetyl 2-ethylhexanoate, (B) Trade name NIKKOL S-10 (Nikko Chemicals) as hydrogenated phospholipid Co., Ltd., phosphatidylcholine content 25 to 30%) 0.4% by mass, (C) polyoxyethylene (10 mol) phytosterol ether 0.4% by mass, fragrance 0.1% by mass as nonionic surfactant Were mixed and dissolved at 70 ° C. (oil phase). On the other hand, a homogeneous aqueous phase in which (D) 1,3-butylene glycol and (E-1) water as a divalent glycol are mixed at a ratio of 1: 1 at 70 ° C. is added to the oil phase to obtain a viscous solution. The addition of the mixed aqueous phase was interrupted when a clear pale white phase appeared.
Subsequently, while stirring the above mixture, a uniform aqueous phase at room temperature containing 0.01% by mass of edetate as another aqueous component, 0.5% by mass of phenoxyethanol, and the remaining water (E-2) was added. After cooling to room temperature, a W / O / W type skin cosmetic was obtained.

The test results of Production Examples 1-1 to 1-8 are shown in Table 1 below together with the composition of various compositions. The contents of evaluation are as follows.
<Appearance>
The appearance of each obtained sample was visually evaluated in three stages: cloudiness, translucency, and transparency.

<Average particle diameter of emulsified droplet>
The average particle size of the emulsified droplets of each of the obtained samples was measured with a particle size distribution meter (FPAR-1000 (manufactured by Otsuka Electronics Co., Ltd.). In the case of 500 nm or less, an actual measurement value is written, and when it exceeds 500 nm. It was written as “×”.

<Viscosity>
Using a digital bismetholone viscometer VDA2 (manufactured by Shibaura System Co., Ltd.), the test sample placed in the measurement container was immersed in a constant temperature water bath at 25 ° C. for 1 hour and then measured.

<Stability test>
The appearance of the sample after standing for 1 month at each temperature of 0 ° C., 25 ° C., and 50 ° C. was judged by visual and microscopic observation according to the following evaluation criteria.
○: No separation or crystal precipitation was observed.
(Triangle | delta): Separation and crystal precipitation are hardly seen.
X: Separation of liquid phase (oil phase or water phase) or crystal precipitation is observed.

The following evaluation was implemented about the usability | use_condition at the time of using skin cosmetics as a sample with the manufacturing method of the cloudy oil-in-water type emulsion cosmetics concerning this invention.
<Feeling of use; moist feeling>
An actual use test was conducted by a female professional panel (10 persons), and the familiarity with the skin was determined according to the following evaluation criteria.
A: All 10 people evaluated that there was a moist feeling.
A: Seven to nine people evaluated that they had a moist feeling.
(Triangle | delta): 3-6 persons evaluated that there was a moist feeling.
X: 0-2 persons evaluated that there was a moist feeling.

<Feeling of use; no stickiness>
An actual use test was conducted by a female panel (10 persons), and stickiness was determined according to the following evaluation criteria.
A: All 10 people evaluated that they were not sticky and moist.
○: Seven to nine people evaluated that they were not sticky and moist.
(Triangle | delta): Three to six persons evaluated that there was no stickiness and was moist.
X: 0-2 persons evaluated that it was moist without stickiness.

<Usage feeling; refreshing feeling>
An actual use test was conducted by a panel dedicated to women (10 persons), and the refreshing feeling was determined according to the following evaluation criteria.
A: All 10 people evaluated that there was a refreshing feeling.
○: Seven to nine people evaluated that there was a refreshing feeling.
Δ: 3 to 6 people evaluated that there was a refreshing feeling.
X: 0-2 persons evaluated that there was a refreshing feeling.

<Usage feeling: Emollient feeling (feeling to feel flexibility in skin)>
An actual use test was conducted by a female panel (10 persons), and the emollient feeling was determined according to the following evaluation criteria.
A: All 10 people evaluated that there was an emollient feeling.
A: 7 to 9 people evaluated that there was an emollient feeling.
Δ: 3 to 6 people evaluated that there was an emollient feeling.
X: 0-2 persons evaluated that there was an emollient feeling.

※１：商品名 NIKKOL BPS-10, HLB;12.5(日光ケミカルズ株式会社製)
※２：商品名 NIKKOL S-10 ホスファチジルコリン含有率25-30%(日光ケミカルズ株式会社製)

* 1: Product name NIKKOL BPS-10, HLB; 12.5 (Nikko Chemicals)
* 2: Product name NIKKOL S-10 Phosphatidylcholine content 25-30% (Nikko Chemicals)

As shown in Table 1 above, in Production Example 1-1 obtained by the production method of the present invention, a low-viscosity white cosmetic composition having excellent stability was obtained.
On the other hand, according to the agglomeration method (Production Example 1-2) and the method using mechanical shear force (Production Example 1-3), which are conventionally known as methods for obtaining fine emulsified droplets, the particle diameter is Although it becomes finer than 100 nm, it tends to be inferior in stability in a low-viscosity composition, or does not conform to the present invention that is clouded to give a creamy feeling, from translucent to transparent It will be presented.

  Production Examples 1-4 to 1-7 are the mixing ratio of (D) 1,3-butylene glycol and (E-1) water in the aqueous phase, which is added to the oil phase heated to 70 ° C. and mixed and dissolved. Are variously changed. In Production Example 1-4 in which only water was added to the oil phase, emulsion droplets of 100 to 500 nm were not obtained, and the stability was poor. When 1,3-butylene glycol was mixed with water, stability was obtained when 1,3-butylene glycol occupied 30% or more of the aqueous phase (Production Example 1-6). When it reaches 80%, it becomes higher than the phase inversion temperature at 70 ° C. and cannot be miniaturized, and it can be miniaturized in the cooling process. However, in the present invention, it is not preferable from the viewpoint of stability. From the above results, in the present invention, the mixing ratio of (D) 1,3-butylene glycol and (E-1) water in the aqueous phase is from 3: 7 to 7: 3 in which both are moderately mixed. It is clearly preferred.

  Production Example 1-8 appears in an initial stage in which an aqueous phase having a mixing ratio of (D) 1,3-butylene glycol and (E-1) water of 1: 1 is added to the oil phase. After a clear pale transparent phase is observed, the addition of the aqueous phase is stopped and an aqueous phase at room temperature containing other aqueous components is added, but the resulting cosmetic is transparent in appearance, The low viscosity composition was inferior in stability.

※３：商品名 NIKKOL S-10E ホスファチジルコリン含有率75-80%(日光ケミカルズ株式会社製)
※４：商品名 NIKKOL S-10 ホスファチジルコリン含有率25-30%(日光ケミカルズ株式会社製)
※５：商品名 NIKKOL TI-10V, HLB;15（日光ケミカルズ株式会社製）
※６：商品名 NIKKOL BPS-10, HLB;12.5（日光ケミカルズ株式会社製）
※７：商品名 EMALEX SPIS-100, HLB;10.0（日本エマルジョン株式会社製）
※８：商品名 NIKKOL TLP-4, HLB;13.0（日光ケミカルズ株式会社製）
※９：商品名 EMALEX HC-40, HLB;12.0（日本エマルジョン株式会社製）
※１０：商品名 NIKKOL MYS-25V, HLB;15.0（日光ケミカルズ株式会社製） 2. Following compounding ingredients cloudy shaped oil-in-water type emulsified cosmetic, the present inventors have found that according to the above-mentioned Production Example 1-1 was carried out considering the suitable conditions for the various ingredients used in the manufacturing method of the present invention.

* 3: Product name NIKKOL S-10E Phosphatidylcholine content 75-80% (Nikko Chemicals)
* 4: Product name NIKKOL S-10 Phosphatidylcholine content 25-30% (Nikko Chemicals)
* 5: Product name NIKKOL TI-10V, HLB; 15 (Nikko Chemicals)
* 6: Product name NIKKOL BPS-10, HLB; 12.5 (Nikko Chemicals)
* 7: Product name EMALEX SPIS-100, HLB; 10.0 (manufactured by Nippon Emulsion Co., Ltd.)
* 8: Product name NIKKOL TLP-4, HLB; 13.0 (manufactured by Nikko Chemicals Corporation)
* 9: Product name EMALEX HC-40, HLB; 12.0 (Nippon Emulsion Co., Ltd.)
* 10: Product name NIKKOL MYS-25V, HLB; 15.0 (Nikko Chemicals)

As shown in Table 2 above, various kinds of nonionic surfactants to be blended were changed, and a nonionic surfactant having a sterol skeleton, an alkyl ether skeleton, and a sorbitan fatty acid ester skeleton was used in the present invention. The compositions obtained by such a production method (Test Examples 1 to 3) had good stability with white turbidity at the intended viscosity with a shabby feeling.
On the other hand, in Test Examples 4 and 5 in which a nonionic surfactant having a hardened castor oil skeleton and a linear nonionic surfactant were blended, a fine emulsified droplet could not be obtained and the cosmetic was poor in stability. there were.
Further, Test Example 6 in which one kind of stearyl alcohol, which is a solid higher alcohol at room temperature, was also inferior in stability.

（※１１：比較製造例１）
モノイソステアリン酸ポリオキシエチレン（２０モル）ソルビタンと、水素添加リン脂質と、流動パラフィンと、イソステアリン酸と、２−エチルヘキサン酸セチルと、香料を７０℃にて混合攪拌した（油相）。続いて、７０℃に加温した油相を攪拌ばねを用いて混合攪拌しながら、イオン交換水と、エタノールと、ジプロピレングリコールと、エデト酸塩と、フェノキシエタノールとを均一に混合した水相を常温にて添加し、目的の水中油型乳化白濁皮膚化粧料を得た。 Table 3 below shows the results of studies on the amount of oil to be blended.
In the following test examples, the evaluation results of the feeling of use in the case of skin cosmetics were shown.

(* 11: Comparative production example 1)
Polyoxyethylene (20 mol) sorbitan monoisostearate, hydrogenated phospholipid, liquid paraffin, isostearic acid, cetyl 2-ethylhexanoate, and fragrance were mixed and stirred at 70 ° C. (oil phase). Subsequently, an aqueous phase in which ion-exchanged water, ethanol, dipropylene glycol, edetate, and phenoxyethanol are uniformly mixed is mixed while stirring the oil phase heated to 70 ° C. using a stirring spring. It added at normal temperature and obtained the target oil-in-water type emulsified white skin cosmetic.

As shown in Table 3 above, Test Example 7 is inferior in moist feeling and emollient feeling because the blending amount of oil (A) is small. Therefore, when the oil content was increased to 5% by mass or more (Test Example 8), the composition obtained by the production method applied to Test Example 7 had an emulsified particle size of 750 nm, and the stability decreased.
On the other hand, in Test Example 9, although the oil content was 5% by mass or more, as described in Production Example 1-1, a mixed solution of water and 1,3-butylene glycol was added to the oil phase. In order to obtain a composition by further adding a uniform aqueous phase containing other aqueous components after forming the emulsion droplets, the emulsion particle diameter was as fine as 190 nm and excellent in stability. Moreover, according to this manufacturing method, even if it mix | blended oil content to about 10 mass%, it was what was excellent in stability. The compositions of Test Examples 9 and 10 were milky white compositions having a transmittance of 5% or less.

  From the above results, according to the production method according to the present invention, even when the oil component (A) is blended in a relatively large amount of 5 to 10% by mass, a cloudy oil-in-water excellent in stability in a low-viscosity cosmetic. It is clear that a type emulsified cosmetic is obtained.

Hereinafter, the present invention will be further described with reference to examples which are specific formulation examples, but the present invention is not limited thereto.
Example 2-1: Oil-in-water emulsified cloudy skin cosmetic (component) (mass%)
(1) Ion-exchanged water Remaining (2) Ethanol 5.0
(3) Glycerin 2.0
(4) 1,3-butylene glycol 10.0
(5) Polyethylene glycol 1.0
(6) Polyoxyethylene (10 mol) behenyl ether 0.5
(Product name: NIKKOL BB-10, HLB 10, Nikko Chemicals)
(7) Hydrogenated phospholipid 0.5
(Product name: NIKKOL Resinol S-10, manufactured by Nikko Chemicals Co., Ltd.)
(8) Tripolyoxyethylene (10 mol) (C12-15) alkyl ether 0.1
(Product name: NIKKOL TDP-10, manufactured by Nikko Chemicals Corporation)
(9) Squalane 4.0
(10) Decamethylcyclopentasiloxane 3.0
(11) Isononyl isononanoate 1.0
(12) Octyl methoxycinnamate 0.5
(13) Edetate 0.01
(14) Paraben 0.15
(15) Rosemary extract 0.1
(16) Fragrance 0.1
(17) Ascorbic acid glucoside 0.5
(18) Potassium hydroxide appropriate amount

Production Method The above components (6) to (12) and (16) were mixed and stirred (oil phase) at 75 ° C. using a stirring spring to be uniform. A mixed aqueous phase having a mass ratio of a part of component (1) and (4) of 1: 1 was added to the oil phase to obtain an emulsified phase. An aqueous phase in which the emulsified phase is uniformly mixed with the remainder of (1) and components (2), (3), (5), (13) to (15), (17), and (18) at room temperature. Was added to obtain the desired oil-in-water emulsified cloudy skin cosmetic. The obtained oil-in-water emulsified white turbid skin cosmetic is composed of fine particles having an average emulsified particle diameter of the emulsified droplets of 263 nm, and the stability for 1 month at each temperature of 0 ° C., 25 ° C. and 50 ° C. Precipitation was not seen and it was favorable. In addition, it was excellent in moist feeling, non-stickiness, refreshing feeling and emollient feeling in use.
Transmittance: 3.0%

Example 2-2: Oil-in-water emulsified cloudy hair cosmetic (component) (mass%)
(1) ion-exchanged water remainder (2) ethanol 7.0
(3) Glycerin 1.0
(4) 1,3-butylene glycol 9.0
(5) Dipropylene glycol 2.0
(6) Polyoxyethylene (5 mol) phytosterol ether 0.2
(Product name: NIKKOL BPS-5, HLB 9.5, manufactured by Nikko Chemicals Co., Ltd.)
(7) Polyoxyethylene (20 mol) phytosterol ether 0.2
(Product name: NIKKOL BPS-20, HLB 15.5, manufactured by Nikko Chemicals Co., Ltd.)
(8) Hydrogenated phospholipid 0.2
(Product name: NIKKOL Resinol S-10, manufactured by Nikko Chemicals Corporation)
(9) Hydrogenated polyisobutene 2.0
(10) α-olefin oligomer 3.0
(11) 2-ethylhexyl palmitate 3.0
(12) Hexametaphosphate 0.01
(13) Paraben 0.15
(14) Sodium hyaluronate 0.01
(15) Fragrance 0.2

Production Method The above components (6) to (11) and (15) were mixed and stirred uniformly at 70 ° C. using a stirring spring (oil phase). A mixed aqueous phase having a mass ratio of a part of component (1) and (4) of 1: 1 was added to the oil phase to obtain an emulsified phase. At room temperature, an aqueous phase in which the remainder of (1) and the components (2), (3), (5), (12) to (14) are uniformly mixed is added to this emulsified phase, and the desired oil-in-water A type emulsified cloudy hair cosmetic was obtained. The obtained oil-in-water emulsified cloudy hair cosmetic is composed of fine particles having an average emulsified particle diameter of 213 nm, and the stability for 1 month at each temperature of 0 ° C., 25 ° C. and 50 ° C. is separated or crystallized. Precipitation was not seen and it was favorable. In addition, it was excellent in moist feeling, non-stickiness, refreshing feeling and emollient feeling in use.
Transmittance: 2.2%

Example 2-3: Oil-in-water emulsified cloudy skin cosmetic (component) (mass%)
(1) Ion-exchanged water The remainder (2) Ethanol 10.0
(3) Glycerin 2.5
(4) 1,3-butylene glycol 12.0
(5) Isoprene glycol 0.5
(6) Sorbitan isostearate 0.4
(Product name: EMALEX SPIS-100, HLB 10, Nikko Chemicals)
(7) Hydrogenated phospholipid 0.3
(Product name: COATSOME NC-21, manufactured by NOF Corporation)
(8) Liquid paraffin 4.5
(9) Squalene 0.5
(10) Isononyl 2-ethylhexanoate 2.5
(11) Pyrophosphate 0.01
(12) Phenoxyethanol 0.5
(13) Peonies extract 0.01
(14) Fragrance 0.01

Production Method The above components (6) to (10) and (14) were mixed and stirred uniformly at 65 ° C. using a stirring spring (oil phase). A mixed aqueous phase having a mass ratio of a part of component (1) and (4) of 1: 1 was added to the oil phase to obtain an emulsified phase. At room temperature, an aqueous phase in which the remainder of (1) and the components (2), (3), (5), (11) to (13) are uniformly mixed is added to this emulsified phase to obtain the desired oil-in-water A type emulsified cloudy skin cosmetic was obtained. The obtained oil-in-water emulsified white turbid skin cosmetic is composed of fine particles having an average emulsified particle diameter of emulsified droplets of 359 nm, and the stability for one month at each temperature of 0 ° C., 25 ° C. and 50 ° C. is separated or crystallized. Precipitation was not seen and it was favorable. In addition, it was excellent in moist feeling, non-stickiness, refreshing feeling and emollient feeling in use.
Transmittance: 1.7%

Example 2-4: Oil-in-water emulsified cloudy skin cosmetic (component) (mass%)
(1) Ion-exchanged water Remaining (2) Ethanol 5.0
(3) Glycerin 2.0
(4) 1,3-butylene glycol 13.0
(5) Propylene glycol 1.0
(6) Polyoxyethylene (10 mol) cholesteryl ether 0.4
(Product name: EMALEX CS-10, HLB 10, manufactured by Nippon Emulsion Co., Ltd.)
(7) Hydrogenated phospholipid 0.4
(Product name: COATSOME NC-61, manufactured by NOF Corporation)
(8) Trioleic phosphate 0.05
(Product name: NIKKOL TOP-OV, manufactured by Nikko Chemicals Corporation)
(9) Squalane 4.0
(10) Dimethylpolysiloxane 3.0
(Product name: KF-96A-6cs, manufactured by Shin-Etsu Chemical Co., Ltd.)
(11) 2-ethylhexyl 2-ethylhexanoate 3.0
(12) Octocrelin 0.1
(13) Ethylenediaminetetraacetate 0.01
(14) Paraben 0.15
(15) Artemisia extract 0.1
(16) Fragrance 0.1

Production Method The above components (6) to (12) and (16) were mixed and stirred at 70 ° C. using a stirring spring so as to be uniform (oil phase). A mixed aqueous phase having a mass ratio of a part of component (1) and (4) of 1: 1 was added to the oil phase to obtain an emulsified phase. At room temperature, an aqueous phase in which the remainder of (1) and the components (2), (3), (5), (13) to (15) are uniformly mixed is added to this emulsified phase, and the desired oil-in-water A type emulsified cloudy skin cosmetic was obtained. The obtained oil-in-water emulsified white turbid skin cosmetic is composed of fine particles having an average emulsified particle diameter of the emulsified droplets of 263 nm, and the stability for 1 month at each temperature of 0 ° C., 25 ° C. and 50 ° C. Precipitation was not seen and it was favorable. In addition, it was excellent in moist feeling, non-stickiness, refreshing feeling and emollient feeling in use.
Transmittance: 4.1%

Example 2-5: Oil-in-water emulsified cloudy skin cosmetic (component) (mass%)
(1) ion-exchanged water remainder (2) ethanol 7.0
(3) Glycerin 2.0
(4) 1,3-butylene glycol 8.0
(5) Dipropylene glycol 1.0
(6) Polyoxyethylene monooleate (20 mol) sorbitan 0.45
(Product name: NIKKOL TO-10V, HLB 10, Nikko Chemicals)
(7) Hydrogenated phospholipid 0.45
(Product name: NIKKOL Resinol S-10E, manufactured by Nikko Chemicals Corporation)
(8) Tripolyoxyethylene (10 mol) (C12-15) alkyl ether 0.1
(Product name: NIKKOL TDP-10, manufactured by Nikko Chemicals Corporation)
(9) Liquid paraffin 4.0
(10) Hydrogenated polyisobutene 1.0
(11) Isotridecyl isononanoate 1.0
(12) Octyl methoxycinnamate 0.5
(13) Edetate 0.01
(14) Paraben 0.15
(15) Hydrolyzed collagen solution 0.1
(16) Tranexamic acid 0.7
(17) Fragrance 0.1

Production Method The above components (6) to (12) and (17) were mixed and stirred at 70 ° C. using an agitation spring (oil phase). A mixed aqueous phase having a mass ratio of a part of component (1) and (4) of 1: 1 was added to the oil phase to obtain an emulsified phase. At room temperature, an aqueous phase in which the remainder of (1) and components (2), (3), (5), and (13) to (16) are uniformly mixed is added to this emulsified phase to obtain the desired oil-in-water A type emulsified cloudy skin cosmetic was obtained. The obtained oil-in-water emulsified white turbid skin cosmetic is composed of fine particles having an average emulsified particle diameter of the emulsified droplets of 263 nm, and the stability for 1 month at each temperature of 0 ° C., 25 ° C. and 50 ° C. Precipitation was not seen and it was favorable. In addition, it was excellent in moist feeling, non-stickiness, refreshing feeling and emollient feeling in use.
Transmittance: 2.3%

Example 2-6: Oil-in-water emulsified cloudy skin cosmetic (component) (mass%)
(1) Ion-exchanged water Remaining (2) Ethanol 5.0
(3) Glycerin 2.0
(4) 1,3-butylene glycol 10.0
(5) Polyethylene glycol 1.0
(6) Polystearic acid polyoxyethylene (20 mol) sorbitan 0.5
(Product name: Sorbon T-60, manufactured by Toho Chemical Co., Ltd.)
(7) Hydrogenated phospholipid 0.5
(Product name: NIKKOL Resinol S-10, manufactured by Nikko Chemicals Co., Ltd.)
(8) Tripolyoxyethylene (10 mol) (C12-15) alkyl ether 0.1
(Product name: NIKKOL TDP-10, manufactured by Nikko Chemicals Corporation)
(9) Squalane 4.0
(10) Decamethylcyclopentasiloxane 3.0
(11) Isononyl isononanoate 1.0
(12) Octyl methoxycinnamate 0.5
(13) Edetate 0.01
(14) Paraben 0.15
(15) Enmeso extract 0.1
(16) Yukinoshita extract 0.1
(17) Ascorbic acid glucoside 0.5
(18) Potassium hydroxide appropriate amount (19) Fragrance 0.1

Production Method The above components (6) to (12) and (19) were mixed and stirred at 70 ° C. using a stirring spring (oil phase). A mixed aqueous phase having a mass ratio of a part of component (1) and (4) of 1: 1 was added to the oil phase to obtain an emulsified phase. At room temperature, an aqueous phase in which the remainder of (1) and the components (2), (3), (5), (13) to (18) are uniformly mixed is added to this emulsified phase, and the desired oil-in-water A type emulsified cloudy skin cosmetic was obtained. The obtained oil-in-water emulsified white turbid skin cosmetic is composed of fine particles having an average emulsified particle diameter of the emulsified droplets of 263 nm, and the stability for 1 month at each temperature of 0 ° C., 25 ° C. and 50 ° C. Precipitation was not seen and it was favorable. In addition, it was excellent in moist feeling, non-stickiness, refreshing feeling and emollient feeling in use.
Transmittance: 3.1%

Claims (9)

In the method for producing a white turbid oil-in-water emulsified cosmetic comprising the following components (A) to (E) and having an average particle diameter of emulsified droplets of 100 to 500 nm:
(A) 1 to 10% by mass of a liquid agent at room temperature having a viscosity of 100 mPa · s or less at 25 ° C.
(B) Hydrogenated phospholipid (C) One or two selected from nonionic surfactants having 9 to 16 HLB and having a sterol skeleton, alkyl ether skeleton, or sorbitan fatty acid ester skeleton Nonionic surfactant (D) Divalent glycols (E) water The components (A), (B) and (C) are mixed and stirred at 50 to 80 ° C. in an oil phase (D ): (E-1) mixed at a mass ratio of 3: 7 to 7: 3, the oil phase mass: (total mass of (D) and (E-1)) = 1: 2 A step of obtaining emulsified droplets having an average particle diameter of 100 to 500 nm by adding to a ratio of 1: 5;
And a step (E-2) of adding a uniform aqueous phase containing water and (E-2) water and cooling to room temperature, and producing a white turbid oil-in-water emulsified cosmetic.   The method for producing a white turbid oil-in-water emulsified cosmetic according to claim 1, wherein the emulsified cosmetic has a viscosity at 25 ° C of 5 to 300 mPa · s. Production method.   The method for producing a white turbid oil-in-water emulsified cosmetic according to claim 1 or 2, wherein the divalent glycol of component (D) is propylene glycol, 1,3-butylene glycol, isoprene glycol, polyethylene glycol, 1 , 2-pentanediol, or one or more selected from the group consisting of 2-pentanediol. A method for producing a white turbid oil-in-water emulsified cosmetic.   In the manufacturing method of the white turbid oil-in-water type emulsion cosmetic in any one of Claims 1-3, the compounding quantity of the liquid agent at room temperature which is a component and (A) viscosity is 100 mPa * s or less at 25 degreeC. A method for producing a white turbid oil-in-water emulsified cosmetic, which is 5 to 10% by mass. In the manufacturing method of the white turbid oil-in-water type emulsion cosmetic in any one of Claims 1-4 , the compounding quantity of a component (B) hydrogenated phospholipid is 0.1-1 mass%, It is characterized by the above-mentioned. A method for producing a white turbid oil-in-water emulsified cosmetic. The method for producing a white turbid oil-in-water emulsified cosmetic according to any one of claims 1 to 5 , wherein the component (C) HLB is 9 to 16, and a sterol skeleton, an alkyl ether skeleton, and a sorbitan fatty acid ester skeleton. A cloudy oil-in-water emulsification, wherein the blending amount of one or more nonionic surfactants selected from among the nonionic surfactants is 0.1 to 1% by mass A method for producing cosmetics. The method for producing a white turbid oil-in-water emulsified cosmetic according to any one of claims 1 to 6 , wherein the blending amount of component (D) divalent glycols is 5 to 20% by mass. A method for producing a white turbid oil-in-water emulsified cosmetic. The white turbid oil-in-water emulsified cosmetic according to any one of claims 1 to 7 , further comprising 5 to 20% by mass of component (F) ethanol. Manufacturing method. The method for producing a white turbid oil-in-water emulsified cosmetic according to any one of claims 1 to 8 , further comprising a component (G) an anionic surfactant having phosphoric acid and / or a phosphate skeleton. A method for producing a cloudy oil-in-water emulsified cosmetic.