JP2002154923A - Method for producing emulsified cosmetic containing hydrophobized powder - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for producing an emulsified cosmetic which has high stability and high powder dispersibility. SOLUTION: This method for producing the emulsified cosmetic containing hydrophobized powder, is characterized by consistently carrying out in one device a process for dispersing non-hydrophobized powder and a powder-coating agent in an oil phase portion with a medium-stirring mill to hydrophobize the powder and the subsequent process for adding an emulsifier and a water phase portion to the obtained dispersion to emulsify the mixture. Further, the method for producing the emulsified cosmetic containing the hydrophobized powder, wherein the emulsifying process is carried out in the medium mill portion of the medium-stirring mill is provided.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a method for producing an emulsified cosmetic containing a hydrophobized powder, and more particularly to an improvement in a mechanism for hydrophobizing the powder.

[0002]

2. Description of the Related Art Various powders such as fine particle titanium dioxide and fine particle zinc oxide are sometimes blended with various compositions of emulsified cosmetics. These powders are blended in the oil phase during the production of emulsified cosmetics. In particular, inorganic powders are usually difficult to blend directly into an oily base material because their surfaces are hydrophilic. Often, aggregation occurs. When the surfactant is added to the oil phase containing the powder and the water phase is added and emulsified, the interaction between the powder and the surfactant, and water,
Aggregation may occur. As a result, there is a problem in the stability of the composition, and there is also a problem in exerting the functions inherent to the powder, such as an ultraviolet scattering effect expected from the fine particle titanium dioxide.

[0003] Therefore, conventionally, various techniques have been developed for increasing the lipophilicity by subjecting the powder surface to a hydrophobic treatment, or for dispersing the powder in advance in an oily dispersion medium together with a specific dispersant. An example of the latter is an emulsified cosmetic using a fine particle titanium dioxide silicone dispersion as described in JP-A-9-208438, which is a composition in which fine particle titanium dioxide is dispersed together with a dispersant in silicone. Is applied to emulsified cosmetics.

[0004]

However, as described above, when the surface of the powder is subjected to a hydrophobic treatment in advance, when the hydrophobic powder is blended into a composition such as a cosmetic, and mixed. The applied shearing force may cause the surface-treated portion to be scraped off, resulting in reduced dispersibility in the oil-based substrate.

[0005] In addition, the fine particle titanium dioxide silicone dispersion used in the conventional emulsified cosmetic may cause sedimentation of the powder over time in the silicone as a dispersant, and this is necessary for stable production of the product. Not preferred.

The present invention has been made in view of the above-mentioned problems of the prior art, and an object of the present invention is to provide a method for producing an emulsion cosmetic having high stability and high powder dispersibility.

[0007]

Means for Solving the Problems As a result of extensive studies by the present inventors to achieve the above object, the non-hydrophobicized powder and the powder coating agent are dispersed in the oil phase to make the powder hydrophobic. After that, the process of adding and emulsifying the emulsifier and the aqueous phase and then emulsifying in one apparatus can be performed consistently in a single medium stirring mill, whereby the stability is high and the dispersibility of the powder is high. The present invention has been found that an emulsified cosmetic composition having a high E content can be obtained, and the present invention has been completed.

That is, a method for producing an emulsified cosmetic containing a hydrophobized powder according to the present invention comprises the steps of dispersing an unhydrophobicized powder and a powder coating agent in an oil phase by a medium stirring mill to make the powder hydrophobic. Subsequently, the step of adding and emulsifying the emulsifier and the aqueous phase and emulsifying the same is performed consistently in one apparatus.

In the method for producing an emulsified cosmetic containing a hydrophobized powder, the apparatus is a batch type medium stirring mill having a medium mill section and a stirring device in one tank.

In a method for producing an emulsified cosmetic containing a hydrophobized powder, the apparatus comprises a medium mill and a pre-stirring tank, and a continuous medium in which the medium mill and the pre-stirring tank are connected by a pipe. It is a stirring mill.

In the method for producing an emulsified cosmetic containing a hydrophobized powder of the present invention, it is preferable that the emulsifying step is performed by a medium mill section of a medium stirring mill.

In the method for producing an emulsified cosmetic containing the hydrophobized powder according to the present invention, it is preferable that the non-hydrophobized powder is an ultraviolet protection powder. In the method for producing an emulsified cosmetic containing the hydrophobized powder of the present invention, the unhydrophobized powder may be selected from one or more of zinc oxide, iron oxide, cerium oxide, and titanate. It is suitable.

In the method for producing an emulsified cosmetic containing a hydrophobized powder according to the present invention, it is preferable that the powder coating agent comprises trimethylsiloxysilicic acid.

Further, in the method for producing an emulsified cosmetic containing the hydrophobized powder of the present invention, the emulsified cosmetic is preferably applied to a water-in-oil type emulsified cosmetic.

[0015]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Preferred embodiments of the present invention will be described below.
explain about.Unhydrophobicized powder  Titanium oxide, acid
Zinc oxide, red iron oxide, yellow iron oxide, black iron oxide, ultramarine,
Lium, talc, mica, sericite, kaolin, silicium
Mosquito, zinc stearate, fluorinated phlogopite, synthetic talc,
Barium sulfate, magnesium carbonate, boron nitride, titanium
Inorganic powders such as phosphates,
White pigment, red iron oxide, yellow iron oxide, black iron oxide, carbon
Black, manganese violet, cobalt violet
Inorganic colored pigments such as blue, ultramarine, navy blue, titanium oxide coating
Mica, titanium oxide coated talc, colored oxide
Tank coated mica, bismuth oxychloride, fish phosphor foil
Which include pearl pigments, metal powder pigments such as alumina
It is.

As the non-hydrophobicized powder of the present invention, an organic or inorganic powder coated with an oxide or a hydrated oxide such as aluminum, silicon, titanium, zirconium, magnesium or zinc can be used. It is.

Further, as an unhydrophobized powder, tetraethoxysilane is coated on zinc oxide in an amount of 10 to 30% by weight,
It is also preferable to use a zinc oxide powder having a silica layer having a thickness of 1 to 3 nm.

Considering that the method for producing the emulsified cosmetic of the present invention is particularly effective for fine powder having an excellent ultraviolet protection effect, fine titanium oxide, fine zinc oxide and fine particles having an average particle diameter of 0.001 to 0.5 μm are considered. Red iron oxide, yellow iron oxide particles, black iron oxide particles, and cobalt blue fine particles. It is known that fine particle powder is superior to ordinary powder in ultraviolet protection effect, transparency and the like.

It is preferred that one or more of these are contained in the oil phase in an amount of 5 to 40% by weight, particularly preferably 10 to 35% by weight. If the content is less than 5% by weight, the effect of the fine particle powder may not be exhibited. If the content is more than 40% by weight, an excessive load may be applied to the medium stirring mill.

[0020]Powder coating  The powder coating preferably used in the present invention is particularly limited.
Although not specified, those that can be dispersed in the non-aqueous solvent
Especially, dimethylpoly which is a silicone compound
Siloxane methyl (polyoxyalkylene) siloxa
Polymer, trimethylsiloxysilicic acid, carboxy-modified
Silicone oil, amino-modified silicone oil, etc.
Can be raised. These silicone-based powder coatings are
1 to 40% by weight, preferably 5 to 30% by weight
Is preferred.

[0021]Oil phase dispersion medium  If a dispersion medium in the oil phase portion suitable for the present invention is exemplified,
Dynamic paraffin, squalane, isoparaffin, branched
Hydrocarbon oils such as light paraffin, isopropyl myristate
G, cetyl isooctanoate, glyceryl triocta
Ester oils such as noate, decamethylpentasiloxa
Dimethylpolysiloxane, methylphenylpolysilo
And silicone oils such as xane.

In the present invention, silicone oils are particularly preferably used, but those having a boiling point of 200 ° C. or less at normal pressure are particularly preferred from the viewpoint of feeling of use and formulation. For example, chain polysiloxanes such as dimethylpolysiloxane, methylphenylpolysiloxane, and methylhydrogenpolysiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, tetramethyltetrahydrogencyclotetrasiloxane, and the like And the like. Among these, volatile linear polysiloxanes such as low-polymerization degree dimethylpolysiloxane (polymerization degree 3 to 7) and volatile silicones such as cyclic volatile polysiloxanes such as decamethylcyclopentasiloxane and octamethylcyclotetrasiloxane. The use of oil is particularly suitable when an oily feeling is less likely to remain when applied to the skin as compared with ordinary silicone oil, and a refreshing feeling of use is required.

In the present invention, the blending amount of the oil phase part dispersion medium can be appropriately selected, but is preferably from 40 to 95% by weight, particularly preferably from 50 to 80% by weight, based on the total amount of the oil phase part. When the amount of the dispersion medium is small, an excessive load may be applied to the medium stirring mill, and when the amount of the dispersion medium is large, the ratio of the powder becomes relatively low, and the hydrophobized powder is mixed. The effect may not be obtained.

[0024]emulsifier  The emulsifier added in the present invention stabilizes the composition in milk.
The present invention is not particularly limited as long as it can be
Considering that it is suitable for use in water-in-oil emulsion cosmetics
For example, sorbitan sesquiisostearate, sorbitan
Tandiisostearate, sorbitan sesquiolate,
Sorbitandiolate, glyceryldiolate, glycer
Ryl diisostearate, polyoxyalkylene modified
Luganopolysiloxane and the like. Oil phase dispersion medium
When a silicone dispersion medium is used as the
Silico such as ethylene / methyl polysiloxane copolymer
Modified emulsifiers, organically modified bentonite, etc.
It is preferable to use earth minerals. The oil phase of the present invention
Also, if necessary, mix these emulsifiers
Can be.

[0025]Medium stirring mill  The medium stirring mill used in the present invention to disperse powder is
Batch type bead mills such as skew mills, horizontal type / vertical type
Annular type continuous bead mill and sand grinder
-Mill, ball mill and the like are used. Medium stirring mill
The material of the medium such as beads, sand and balls used is
Glass, alumina, zirconia, titanium, steel, etc.
However, zirconia is particularly preferred. Also,
As for the size, usually a diameter of about 0.3 to 2.0 mm
Is used, but in the present invention, in particular, 0.5 to 1.0 m
m is preferred. Disperse the powder with a stirring medium mill
Normal powder such as homomixer or homogenizer before
Ability to crush powder used in the powder dispersion process to some extent
It is desirable to carry out the primary treatment with a dispersing machine having power.
It is to break up particles in the aggregate state in the primary treatment.
With the subsequent secondary processing, crushing with a medium stirring mill,
Reduce the load required for dispersion, efficiently disintegrate the powder, and
This is because they can be dispersed.

In the present invention, it is necessary to carry out a treatment with a medium stirring mill so that the powder is highly dispersed in the essential components.

The medium stirring mill, which is a dispersion apparatus suitably used in the production method of the present invention, can be either a batch type or a continuous type. FIG. 1A shows an example of a batch type medium stirring mill. ).

As shown in FIG. 1A, a medium stirring mill used in the manufacturing method of the present invention includes a basket section (medium mill section) 10 in a tank 18 and a premixing section 10 provided therewith. One or more in-tank stirrers 20 that also serve for the dispersion liquid flow are provided. The basket section 10 is provided with a top cover jacket 28 and the rod 16.
The position is fixed by. And basket part 10
Are provided with a large number of small holes made of slits. The basket unit 10 has an in-basket stirring device 14 for stirring the inside of the basket unit 10.

First, the raw material containing the powder is preliminarily mixed into a mixed liquid by the in-tank agitator 20 provided, and then the rotating shaft of the in-basket agitator 14 above the basket unit 10 attached to the apparatus. It flows into the basket part 10 from the surrounding opening.

Here, the inside of the basket section 10 is shown in FIG.
It is shown in (B). The inside of the basket portion 10 is filled with a solid dispersion medium (beads) 22, and the stirring device 14 in the basket has a stirring pin disk 26 (or a stirring disk) mounted perpendicular to the rotation axis. . The stirring pin disk 26 has a pin 24 for stirring.

The mixed liquid that has flowed into the basket portion 10 is crushed and dispersed by the solid dispersion medium (beads) 22 by the high-speed rotating stirring pin disk 26 to crush various powder agglomerated particles in the powder component. It flows out from small holes 12 formed of a number of slits provided on the side wall of the basket portion 10.

The arrows in FIG. 1A indicate the overall fluid path.

The outflowing dispersion liquid is supplied to the tank stirring device 2
0, a part flows again into the basket portion 10 through the opening above the basket portion 10 and flows into the tank 1
Circulate in 8. It is important that the agitating portion of the in-tank agitator 20 is located at a position that does not obstruct the fluid path in and out of the basket section 10. The medium agitating mill is an apparatus having a process of keeping the dispersion of the powder in the tank 18 uniform in this way. As a suitable dispersing apparatus for the method for producing an emulsified cosmetic containing the hydrophobized powder of the present invention, a dispersing apparatus described in JP-B-8-17930 can be mentioned.

The basket section filled with the solid dispersion medium (beads) installed in the medium stirring mill has a large number of small holes formed by slits on its side wall, and the size thereof is determined by the size of the solid dispersion medium to be used. Since the (beads) have such a size that they do not flow out of the basket portion, the resulting dispersion does not contain a solid dispersion medium.

As described above, in the medium stirring mill suitably used in the present invention, the small hole is provided in the side wall of the basket portion filled with the solid dispersion medium. In this case, since the solid dispersion medium concentrates on the side wall portion, the powder passes through a place where the density of the solid dispersion medium is high, so that the dispersion efficiency can be increased.

As the stirring device having both the pre-mixing and the dispersing flow used in the present invention, a stirring device suitable for ordinary cosmetics production can be used. It is particularly preferable to use a disper or a homogenizer equipped with a turbine type rotor.

FIG. 2 shows an example of a continuous medium stirring mill attached to a preliminary stirring tank suitably used in the production method of the present invention. The continuous medium agitating mill device shown in FIG.
This is a device in which a liquid containing powder can be circulated by connecting a medium milling section 30 containing the powder and a preliminary stirring tank 32 capable of being stirred by a disper 42 by rotation of a motor 38 via a pipe 34 via a pump 34.

First, the raw material containing the powder is supplied to the preliminary stirring device 32.
After being preliminarily mixed by the disperser 42 to form a mixed liquid, the mixture flows into the medium agitating mill 30 connected by a pipe by the pump 34.

The mixed liquid that has flowed into the medium mill 30 is crushed and dispersed by a solid dispersion medium (beads) 40 by a high-speed stirring agitator to crush various powder agglomerated particles in the powder component. It is sent to the preliminary stirring tank 32 again by the pump 34.

The continuous medium stirring mill is an apparatus having a process for making the dispersion of powder uniform as described above. The stirring time in the preliminary stirring tank, the stirring time in the medium stirring mill, and the number of Passes of the present apparatus can be appropriately determined as needed.

As a stirrer for the pre-stirring tank suitably used in the present invention, a stirrer suitable for ordinary production of cosmetics or the like can be used. It is particularly preferable to use a disperser or a homogenizer equipped with. A biaxial type disper with a disper blade and a scraping blade can also be suitably used.

Next, the method for producing an emulsified cosmetic containing the hydrophobized powder of the present invention will be described more specifically with reference to examples.

When a batch-type medium stirring mill having a stirring device in a tank is used, a dispersion medium such as silicone oil is mixed with the stirring device in the tank using a medium stirring mill having a stirring device in the tank. Thereafter, the mixture is dispersed and mixed for a short period of time, for example, about 3 to 10 minutes, in a basket section, which is a medium mill section. Thereafter, an unhydrophobicized powder such as titanium oxide and a powder coating agent such as trimethylsiloxysilicic acid are added, and Dispersion and mixing are performed at a high shearing force for a time of, for example, about 10 minutes to 2 hours. During this time, the titanium dioxide is coated with trimethylsiloxysilicic acid to become hydrophobic titanium dioxide.

Subsequently, an emulsified cosmetic containing a hydrophobized powder is added to the tank by adding an aqueous phase, mixing the dispersion in the tank with a mixing / stirring unit, and emulsifying using a medium mill. Can be obtained.

When a continuous medium stirring mill with a pre-stirring device is used, a dispersion medium such as silicone oil is stirred and mixed in the pre-stirring device, and then the nonhydrophobized powder such as titanium oxide and trimethyl are mixed. A powder coating agent such as siloxysilicic acid is added to the preliminary stirring tank, and the mixture is stirred and mixed for a short time, for example, for about 3 to 10 minutes, and then, for example, 10
The dispersion and mixing process is performed by high shearing force and high impact force for about 10 minutes to about 10 hours, about 3 to 10 times of pass, or about 3 to 10 minutes of pass. During this time, the unhydrophobicized powder such as the titanium oxide is coated with trimethylsiloxysilicic acid to become hydrophobic titanium oxide. Subsequently, the aqueous phase is added to the preliminary stirring tank, and emulsified by a mixer. In some cases, emulsification is continuously performed using a medium mill in order to homogenize the contents in the apparatus.

The method for producing such emulsified cosmetics of the present invention can be suitably used particularly for a water-in-oil type.

According to this production method, it is possible to produce an emulsified cosmetic containing a hydrophobized powder in a single apparatus in a short time, with easy operability and at low cost. Moreover, the emulsified cosmetic containing the hydrophobized powder obtained according to the present invention has a high dispersibility and therefore exhibits a high ultraviolet protection effect, and exhibits a smooth and creamy texture when emulsified by a medium mill. be able to.

[0048]Other ingredients  In the present invention, an oily component is further added to the oil phase portion.
Can be added. Examples of such oily components include
For example, cetyl isooctanoate, glyceryl trihexa
Ester oils such as noate and isopropyl myristate,
Hydrocarbons such as petrolatum, liquid paraffin, and squalane
Oil, castor oil, olive oil, camellia oil, jojoba oil, lanori
Used in combination with natural animal and vegetable oils such as oil.

In the present invention, the components to be mixed in the aqueous phase include polyhydric alcohols such as glycerin, water-soluble substances such as ethyl alcohol, and water.

The emulsified cosmetic of the present invention further includes a surfactant, a dispersant, a stabilizer, a coloring agent, a preservative, an antioxidant, an ultraviolet absorber, a humectant, a fragrance and the like. It can be appropriately blended within the range reached.

The production method of the present invention is applied, for example, to the production of emulsified cosmetics such as emulsified sunscreens and emulsified foundations.

Further, the emulsified cosmetic according to the present invention has excellent usability, water resistance and oil resistance in addition to the excellent ultraviolet shielding effect of the highly dispersed ultraviolet protective powder, and has excellent emulsion stability and chemical properties. It has the advantage of excellent stability.

Next, test examples of the present invention will be described.
First, the present inventors prepared an emulsified cosmetic containing a hydrophobized powder by the following production method, and examined the stability over time. In addition, smoothness, powderiness, uniform finish, and transparency were evaluated by sensory evaluation, and SPF was measured. The evaluation criteria are as follows.

[0054]Evaluation criteria  Apply the sample to 20 female panelists,
The length, uniform finish, and transparency were evaluated. (Evaluation) 17 or more respondents are good ◎ 12 to 16 respondents are good ○ 9 to 11 respondents are good △ 5 to 8 respondents are good × 4 or less respondents are good ×× Table 1 shows the results.

[0055]

[Table 1]  Sunscreen test example test example test example test example1 2 3 4  Oil phase Volatile silicone 36 36 36 36 Methyl polysiloxane 33 33 33 Polyoxyethylene-methyl polysiloxane copolymer 0.6 0.6 0.6 0.6 Organically modified bentonite 0.6 0.6 0.6 0.6 Fine zinc oxide 15 15 15 15 Trimethylsiloxysilicic acid 4.8 4.8 4.8-Additive component Nylon powder 55 55 octyl methoxycinnamate 77 77 77 Polyoxyethylene-methyl polysiloxane copolymer 0.5 0.5 0.5 0.5 Isostearic acid 0.5 0.5 0.5 0.5 Water phase humectant 5 55 5 5 Remaining Remaining Remaining Remaining  Separation Immediately after production ○ ○ ○ △ One month later ○ ○ △ ×  Smoothness ◎ ○ △ △ Powderiness ◎ ○ × △ Uniform finish ◎ ◎ △ × Transparency ◎ ◎ △ △ SPF 48 46 36 33

Production method (Test Example 1) : Volatile silicone, methylpolysiloxane, polyoxyethylene / methylpolysiloxane copolymer, and organically modified bentonite were premixed (medium stirring mill for 5 minutes), and fine particles were added thereto. Zinc oxide and trimethylsiloxysilicic acid are added and dispersed by a medium stirring mill for 50 minutes (oil phase). Subsequently, nylon powder, octyl methoxycinnamate, polyoxyethylene / methyl polysiloxane copolymer, and isostearic acid are added to the oil phase in the same tank, and the mixture is stirred and mixed with a disper for 5 minutes, and further moisturized. The resulting mixture was stirred and mixed with a disper for 5 minutes, and then emulsified with a medium stirring mill for 5 minutes.

Production method (Test Example 2) : volatile silicone, methylpolysiloxane, polyoxyethylene / methylpolysiloxane copolymer, and organically modified bentonite were premixed (medium stirring mill for 5 minutes), and fine particles were added thereto. Zinc oxide and trimethylsiloxysilicic acid are added and dispersed by a medium stirring mill for 50 minutes (oil phase). Subsequently, nylon powder, octyl methoxycinnamate, polyoxyethylene / methyl polysiloxane copolymer, and isostearic acid are added to the oil phase in the same tank, followed by stirring and mixing with a homogenizer for 5 minutes, and further moisturizing. The mixture was added to the mixture and ion-exchanged water, and further stirred and mixed with a homogenizer for 5 minutes to emulsify.

Production method (Test Example 3) : A volatile silicone, methylpolysiloxane, polyoxyethylene / methylpolysiloxane copolymer, and an organically modified bentonite were premixed (disperse for 5 minutes), and fine zinc oxide was added thereto. And trimethylsiloxysilicic acid, and dispersed for 50 minutes by a disperser usually used in the manufacture of cosmetics (oil phase). Subsequently, nylon powder, octyl methoxycinnamate, polyoxyethylene / methyl polysiloxane copolymer, and isostearic acid were added to the oil phase in the same tank, and stirred for 5 minutes with a disper.
After mixing, a humectant and ion-exchanged water were added, and the mixture was further stirred and mixed with a disper for 5 minutes.

Production method (Test Example 4) : According to Test Example 1.

As is clear from Table 1 above, Test Example 3 in which the fine zinc oxide is not sufficiently hydrophobized and Test Example 4 in which the microparticle zinc oxide was not hydrophobized at all were low in stability, indicating that the fine particles of zinc oxide were not hydrophobic. The evaluation was low. On the other hand, the cosmetics according to the present invention (Test Examples 1 and 2) were excellent in stability and dispersed in powder, so that the cosmetics exhibited an excellent effect in evaluation.

From the results shown in Table 1 above, the emulsified cosmetic according to the present invention not only has improved dispersibility of fine zinc oxide, but also has the fine zinc oxide surface hydrophobically coated with a coating agent. In order to coat the zinc oxide fine particles with trimethylsiloxysilicic acid,
It can be understood that dispersion by a medium stirring mill is necessary.

[0062]

Embodiments of the present invention will be described below. Note that the present invention is not limited to these examples.

[0063]Example 1 Water-in-oil type sunscreen cosmetics  (Method) Volatile silicone in oil phase, methyl polysilo
Xanth, organic modified clay mineral in batch type medium stirring mill
After dispersing with a disper for 5 minutes,
Add methylsiloxysilicic acid and dispers for 5 minutes
After the dispersion, the mixture is dispersed in a medium mill for 30 minutes. Then add
After adding the aqueous phase and dispersing for 5 minutes with a disper, 5 minutes
The mixture is dispersed and emulsified in a medium mill.

(Method) Volatile silicone, methylpolysiloxane, and organically modified clay mineral in the oil phase were dispersed for 5 minutes by a disperser in a pre-stirring tank of a continuous medium stirring mill provided with a pre-stirring tank. After adding zinc and trimethylsiloxysilicic acid and dispersing for 5 minutes with a disper, pass with a medium mill five times to disperse. Thereafter, the added component and the aqueous phase are added to the preliminary stirring tank, dispersed for 5 minutes by a disper, then dispersed and emulsified by 1 pass in a medium mill.

(Oil phase) Volatile silicone 30 Methylpolysiloxane 5 Polyoxyethylene-methylpolysiloxane copolymer 0.3 Organically modified bentonite 0.3 Fine zinc oxide (untreated product) 15 Trimethylsiloxysilicic acid 5 (Additive component) Silicone resin powder 3 Octyl methoxycinnamate 7.5 Polyoxyethylene-methylpolysiloxane copolymer 1.2 Isostearic acid 0.5 Perfume Appropriate amount (aqueous phase) Moisturizer 5 Preservative Appropriate ion exchange water to 100

[0066]Example 2 Water-in-oil emulsion foundation  (Method) Volatile silicone in oil phase, methyl polysilo
Xane, fine zinc oxide and trimethylsiloxysilicic acid
Disperse for 5 minutes with a disper in a batch type media stirring mill
Thereafter, the mixture is dispersed in a medium mill for 30 minutes. Then additional ingredients,
Add the aqueous phase, disperse with a disper for 5 minutes, and media for 5 minutes
Disperse and emulsify in the body mill.

(Method) Volatile silicone, methylpolysiloxane, fine particle zinc oxide and trimethylsiloxysilicic acid in the oil phase were dispersed for 5 minutes by a disperser in a pre-stirring tank of a continuous medium stirring mill equipped with a pre-stirring tank. Thereafter, the mixture is dispersed five times by passing through a media mill. Thereafter, the added component and the aqueous phase are added to the preliminary stirring tank, dispersed for 5 minutes by a disper, then dispersed and emulsified by 1 pass in a medium mill.

(Oil Phase) Volatile Silicone 30 Methylpolysiloxane 5 Fine Particle Zinc Oxide (Untreated) 15 Trimethylsiloxysilicic Acid 4.5 (Additional Component) Silicone Resin Powder 3 Octylmethoxycinnamate 7.5 Polyoxyethylene -Methylpolysiloxane copolymer 1 Isostearic acid 0.5 Perfume proper amount (aqueous phase) Humectant 5 Preservative proper amount Sodium glutamate 1 Deionized water to 100

[0069]Example 3 Water-in-oil emulsion foundation  (Method) Volatile silicone in oil phase, methyl polysilo
Xanth, organic modified clay mineral in batch type medium stirring mill
After dispersing with a disper for 5 minutes,
Add Limethylsiloxysilicic acid and dispers for 5 minutes
After the dispersion, the mixture is dispersed in a medium mill for 30 minutes. Then add
After adding the components and the aqueous phase and dispersing for 5 minutes with a disper, add
Disperse and emulsify in a medium mill for 0 minutes.

(Method) The volatile silicone, methylpolysiloxane, and organically modified clay mineral in the oil phase were dispersed for 5 minutes by a disperser in a pre-stirring tank of a continuous medium stirring mill provided with a pre-stirring tank. Titanium and trimethylsiloxysilicic acid are added, and the mixture is dispersed for 5 minutes by a disper. Thereafter, the added component and the aqueous phase were added to the preliminary stirring tank, and dispersed for 5 minutes with a disper.
Disperse and emulsify 2 passes in the media mill.

(Oil phase) Volatile silicone 20 Methylpolysiloxane 15 Polyoxyethylene-methylpolysiloxane copolymer 1 Organically modified bentonite 1 Fine particle titanium oxide (aluminum-treated product) 5 Trimethylsiloxysilicic acid 1.5 (Additives) Nylon powder 3 Silicone-treated talc 10 Silicone-treated titanium oxide 8 Silicone-treated yellow iron oxide 2 Silicone-treated red iron oxide 1 Silicone-treated black iron oxide 0.5 Polyoxyethylene-methylpolysiloxane copolymer 1.5 Isostearic acid 0. 5 (Aqueous phase) Moisturizer 8 Preservatives Appropriate amount Deionized water to 100

[0072]Example 4 Water-in-oil emulsification foundation  (Method) Volatile silicone in oil phase, methyl polysilo
Xanth, organic modified clay mineral in batch type medium stirring mill
After dispersing with a disper for 5 minutes, fine particles of titanium oxide, color
Material, extender and trimethylsiloxysilicic acid
After dispersing for 5 minutes in dispers, dispersing in medium mill for 30 minutes
I do. Then add the added ingredients and the aqueous phase and disperse
After dispersion for 5 minutes, the mixture is dispersed and emulsified in a medium mill for 5 minutes.

(Method) The volatile silicone, methylpolysiloxane and organically modified clay mineral in the oil phase were dispersed for 5 minutes by a disperser in a preliminary stirring tank of a continuous medium stirring mill provided with a preliminary stirring tank. Titanium, a coloring material, an extender pigment, and trimethylsiloxysilicic acid are added, and the mixture is dispersed by a disper for 5 minutes. Thereafter, the added component and the aqueous phase are added to the preliminary stirring tank, dispersed for 5 minutes by a disper, and then dispersed and emulsified by 2 passes in a medium mill.

(Oil Phase) Volatile Silicone 20 Methylpolysiloxane 15 Polyoxyethylene-Methylpolysiloxane Copolymer 1 Organically Modified Bentonite 1 Fine Particle Titanium Oxide (Aluminum Treated Product) 5 Titanium Oxide 8 Yellow Iron Oxide 2 Red Iron Oxide Reference Signs List 1 black iron oxide 0.5 talc 10 trimethylsiloxysilicic acid 4.5 (additive component) nylon powder 3 polyoxyethylene-methylpolysiloxane copolymer 1 (aqueous phase) humectant 8 preservative proper amount ion-exchanged water to 100

[0075]Example 5 Water-in-oil emulsification foundation  (Method) Volatile silicone in oil phase, methyl polysilo
Xane, fine particle titanium oxide, coloring material, extender pigment, trimethyl
Dispersing luciroxysilicic acid in a batch-type media stirring mill
And then disperse for 30 minutes in the media mill.
You. After that, the added component and the aqueous phase were added, and the mixture was
After dispersion for 5 minutes, the mixture is dispersed and emulsified in a medium mill for 5 minutes.

(Method) Volatile silicone, methylpolysiloxane, fine particle titanium oxide, coloring material, extender pigment, and trimethylsiloxysilicic acid in the oil phase were mixed in a premixing tank of a continuous medium stirring mill equipped with a premixing tank. 5 at Disper
After dispersing for 1 minute, pass 3 times with a media mill to disperse. Thereafter, the added component and the aqueous phase are added to the preliminary stirring tank, dispersed for 5 minutes by a disper, and then dispersed and emulsified by 2 passes in a medium mill.

(Oil Phase) Volatile Silicone 20 Methylpolysiloxane 15 Fine Particle Titanium Oxide (Aluminum Treated Product) 5 Organically Modified Bentonite 1 Titanium Oxide 8 Yellow Iron Oxide 2 Red Iron Oxide 1 Black Iron Oxide 0.5 Talc 10 Trimethylsiloxy Silicic acid 4.5 (Additive component) Nylon powder 3 Polyoxyethylene-methylpolysiloxane copolymer 2 Sorhitan sesquiisostearate 1 (Aqueous phase) Moisturizer 8 Preservatives Appropriate amount Sodium glutamate 2 Ion exchange water to 100

[0078]

As described above, according to the method for producing an emulsified cosmetic containing a hydrophobized powder according to the present invention, an unhydrophobized powder and a powder coating agent are added to an oil phase by a medium stirring mill. Since the steps of dispersing and hydrophobizing and the subsequent steps of adding and emulsifying an emulsifier and an aqueous phase are consistently performed in one apparatus, production can be performed at low cost. Further, the produced emulsified cosmetic is excellent in stability and excellent in dispersion of powder.

Further, by using the powder as an ultraviolet ray protective powder, it is possible to improve the dispersibility and improve the ultraviolet ray protective ability.

[Brief description of the drawings]

FIG. 1 is an explanatory diagram of an example of a medium stirring mill suitably used in the method for producing an emulsified cosmetic containing a hydrophobic powder according to the present invention.

FIG. 2 is an explanatory view of an example of a medium stirring mill suitably used in the method for producing an emulsified cosmetic containing a hydrophobic powder according to the present invention.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 10 Basket part (medium mill part) 12 Small hole which consists of a slit 14 Stirring device in a basket 16 Rod 18 Tank 20 Stirring device (disper) in a tank which has both premixing and dispersion liquid flow 22 Solid dispersion medium (beads) 24 Pin 26 Stirring Pin Disc 28 Jacket 30 Medium Mill 32 Pre-stirring Tank 34 Pump 36 Motor 38 Motor 40 Bead 42 Disper

 ────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Kazuhisa Ohno 2-2-1 Hayabuchi, Tsuzuki-ku, Yokohama-shi, Kanagawa F-term in Shiseido Research Center (Shin-Yokohama) (reference) 4C083 AB211 AB212 AB231 AB232 AB241 AB242 AB432 AB442 AC262 AC342 AC442 AC582 AC911 AC912 AD072 AD152 AD162 BB01 BB25 BB46 CC12 CC19 DD32 EE17 FF01 FF05

Claims (8)

[Claims] 1. An apparatus comprising: a step of dispersing an unhydrophobized powder and a powder coating agent in an oil phase by a medium stirring mill to make the powder coating hydrophobic; and a step of adding an emulsifier and an aqueous phase to emulsify the mixture. A method for producing an emulsified cosmetic containing a hydrophobized powder, wherein the emulsified cosmetic is performed consistently within the composition. 2. The emulsion according to claim 1, wherein the apparatus is a batch-type medium stirring mill having a medium mill section and a stirring device in one tank. Manufacturing method of cosmetics. 3. The production method according to claim 1, wherein the apparatus comprises a medium mill section and a preliminary stirring tank, and the medium mill section and the preliminary stirring tank are continuous medium stirring mills connected by piping. A method for producing an emulsified cosmetic comprising a hydrophobized powder. 4. The method according to claim 1, wherein the emulsifying step is performed by a medium mill section of a medium stirring mill. . 5. The method according to claim 1, wherein the non-hydrophobicized powder is an ultraviolet protection powder. 6. The method according to claim 1, wherein the non-hydrophobized powder is selected from one or more of zinc oxide, iron oxide, cerium oxide, and titanate. A method for producing an emulsified cosmetic containing a hydrophobic powder. 7. The method according to claim 1, wherein the powder coating agent comprises trimethylsiloxysilicic acid. 8. The method according to claim 1, which is applied to a water-in-oil type emulsified cosmetic, characterized by comprising a hydrophobic powder.