JP6640794B2 - Manufacturing method of powder cosmetics - Google Patents

Description

  The present invention relates to a method for producing a powder cosmetic.

Powder cosmetics are manufactured by mixing powder and oily components, crushing the mixture with a crusher such as a pulperizer, and then filling the mixture in a metal or resin middle plate, or by dry press molding. A method referred to as a dry manufacturing method has been adopted and manufactured.
On the other hand, since properties such as feeling of use are not sufficient according to the dry manufacturing method, for the purpose of improving properties, a slurry is prepared by adding powder and an oily component to a volatile solvent, and the slurry is placed in a container in a slurry state. A method called a wet process has been proposed in which the powder is filled and then the solvent is removed by vacuum suction or the like to solidify the powder.

  As described above, the dry process leaves room for improvement in the feeling of use in application to the skin, and the wet process has room for improvement in removing the solid cosmetics into puffs because they are too hard. In the method, further improvement was required in order to obtain a satisfactory solid cosmetic.

In view of the above problems, attention is paid to the step of drying the slurry in the wet manufacturing method, the slurry is made into fine droplets by mechanical shearing force, the drying gas is sent to the fine droplets, and the slurry is dried, A method for obtaining a powder cosmetic excellent in both usability and usability has been disclosed (see Patent Document 1).
In addition, in the wet manufacturing method, in order to obtain powder solid cosmetics with excellent usability and impact resistance, by using a medium stirring mill for mixing when preparing the slurry, the powder component surface is made uniform with oily components. (See Patent Document 2).

JP 2007-055990 A JP 2001-213722 A

As described in Patent Literatures 1 and 2, attempts are being made to achieve a balance between the usability when applied to the skin and the usability such as the degree of removal into puffs and drop strength in a wet process.
On the other hand, in the case of the wet process, in order to improve the dispersibility in the preparation of the slurry and to sufficiently perform the surface treatment of the powder, a mechanical shearing mill such as a medium stirring mill as described in Patent Document 2 is used. A method of mixing using force is adopted.

However, when preparing a slurry using mechanical shearing force, a strong impact force is applied to the powder, so that the powder is excessively pulverized and the particle size becomes too small, and the powder is damaged. The present inventor has conceived that there is a problem that the inherent properties of the powder are impaired due to a reduction in glitter and the effects expected as a powder cosmetic are not sufficiently exhibited.
An object of the present invention is to provide a powder cosmetic which solves the above-mentioned problems, exhibits the inherent performance of powder, and sufficiently obtains expected effects.

MEANS TO SOLVE THE PROBLEM In order to solve the said subject, while having sufficient mixing and stirring power in the slurry preparation at the time of manufacturing a powder cosmetic, the slurry preparation means in which the damage given to a powder is reduced It was investigated. Then, they conceived that sufficient stirring and mixing can be performed by using a specific high-pressure fluid mixer, and thus completed the present invention.

The present invention includes the following.
A method for producing a powder cosmetic, comprising: a slurry preparing step of preparing a slurry by mixing at least a powder and an oily component in a solvent; and a drying step of drying the prepared slurry to obtain a powder cosmetic. And
In the slurry preparation step, a method for producing a powder cosmetic using a high-pressure fluid mixer that mixes the powder and the oil component by flowing the solvent containing the powder and the oil component in the chamber as a high-pressure fluid.

  Further, the high-pressure fluid mixer may be configured to discharge the solvent containing the powder and the oily component as a high-pressure fluid and mix the powder and the oily component by obliquely colliding the high-pressure fluids with each other, Further, the high-pressure fluid mixer may be configured to mix the powder and the oil component by generating cavitation in the chamber.

Further, the powder may be in a form comprising at least a particle size of two or more different powders, also the average particle diameter D ₅₀ of less 5μm fine, having an average particle diameter D ₅₀ of greater than 20μm structure It may be a form containing at least a pigment.

  According to the present invention, without using a medium like a medium stirring mill, that is, since the slurry can be prepared without media, without applying a strong impact force to the powder contained in the powder cosmetic, No excessive grinding of the powder occurs. Therefore, it is possible to provide a powder cosmetic in which the effects expected of the powder cosmetic are sufficiently exhibited without impairing the inherent properties of the powder.

It is a schematic diagram which shows one Embodiment of a high pressure fluid mixer. It is a schematic diagram which shows one Embodiment of a high pressure fluid mixer.

  Hereinafter, a method for producing a powder cosmetic that is an embodiment of the present invention will be described, but the technical scope of the present invention is not limited to the following specific embodiments.

  The method for producing a powder cosmetic according to the present embodiment is a slurry preparation step of preparing a slurry by mixing at least a powder and an oil component in a solvent, and drying the prepared slurry to obtain a powder cosmetic. Drying step to obtain. Further, the method may further include a molding step of filling the mold with the powder cosmetic and molding.

<Slurry preparation process>
The slurry preparation step is a step of preparing a slurry by mixing at least a powder and an oil component in a solvent. During the preparation of the slurry, components other than the powder and oily components required for the preparation of the cosmetic can be appropriately added.

In the present embodiment, in the slurry preparation step, a high-pressure fluid mixer that mixes the powder and the oil component by flowing a solvent containing the powder and the oil component in the high-pressure fluid chamber is used.
Conventionally, slurry preparation in the production of powder cosmetics has been performed by a method using mechanical shearing force such as a medium stirring mill in order to uniformly and sufficiently coat the powder surface with an oily component. However, it has been found that the powder powder is damaged or over-pulverized because a strong impact force is applied to the powder, which may cause a situation in which the effects expected as powder cosmetics are not sufficiently exhibited. . Therefore, the present inventors, as a mixer in which the powder in the slurry is not excessively pulverized and the powder in the slurry and the oily component are sufficiently mixed, the solvent containing the powder and the oily component is subjected to high pressure. It has been found to use a high-pressure fluid mixer that flows in a fluid chamber, ie a medialess mixer.

The high-pressure fluid mixer used in the present embodiment will be described with reference to FIGS.
FIG. 1 is a schematic diagram showing one embodiment of a high-pressure fluid mixer. The high-pressure fluid mixer shown in FIG. 1 is a mixer that discharges a solvent containing a powder and an oily component as a high-pressure fluid and mixes the high-pressure fluids by oblique collision.
The high-pressure injection type mixer 10 discharges a chamber 1 for mixing powder and oily components, supply ports 2a and 2b for supplying a solvent containing powder and oily components as high-pressure fluid into the chamber, and a mixed slurry. A slurry outlet 4 is provided.
The supply ports 2a and 2b are provided at substantially the same height on opposing side surfaces of the chamber 1. The flow path extending from the supply ports 2a and 2b to the opposite side to the center of the chamber is inclined, and the direction of discharging the slurry from the supply ports is higher than horizontal.

The solvent containing the powder and the oil component is pressurized by a pressurizer (not shown) and sent as a high-pressure fluid to a flow path connected to the supply ports 2a and 2b. The high-pressure fluid is sufficiently accelerated when supplied from the supply port into the chamber, and the high-pressure fluid discharged from the opposed supply ports 2a and 2b is obliquely collided at the collision point 3 substantially in the center of the chamber 1. I do. In addition, when the flow path extending from the supply ports 2a and 2b to the side opposite to the center of the chamber is not inclined, and is substantially horizontal, no oblique collision occurs. Since the high-pressure fluid collides at a high speed, the effect of stirring and mixing by the collision can be sufficiently expected.
In FIG. 1, there are two supply ports 2a and 2b, but if each supply port is provided at substantially the same height, there are four supply ports even if there are three supply ports. Alternatively, more supply ports may be provided depending on the shape of the chamber.

  The powder and oily component that collided at the collision point 3 in the chamber 1 are discharged from the slurry discharge port 4. In the collision between powders present in the solvent, the impact force on the powder is smaller than when the powder is directly subjected to mechanical shearing force from the medium, and by colliding the high-pressure fluid at high speed, The droplets of the oily component in the slurry become flat, and it becomes possible to cover many powders. In addition, according to the oblique collision, the impact force on the powder is smaller than in the head-on collision.

FIG. 2 is a schematic diagram illustrating an embodiment of the high-pressure fluid mixer. The high-pressure fluid mixer shown in FIG. 2 is a mixer that mixes powder and an oily component by generating cavitation in a chamber.
The high-pressure injection mixer 20 includes a chamber 11 for mixing the powder and the oily component, a supply port 12 for supplying a solvent containing the powder and the oily component into the chamber as a high-pressure fluid, and extending from the supply port into the chamber. An orifice 12a for generating cavitation 13 and a slurry outlet 14 for discharging the mixed slurry are provided.

The solvent containing the powder and the oil component is pressurized by a pressurizer (not shown) and sent to a flow path connected to the supply port 12 as a high-pressure fluid. The supply port 12 has an orifice 12a extending from the supply port into the chamber. Since the diameter of the orifice is designed to be very small, and the fluid pressurized to a high pressure inside the orifice is supplied at a high speed, cavitation 13 occurs. The powder and the oil component are mixed by the impact generated by the cavitation 13 bursting.
The fluid in which the powder and the oil component are mixed is discharged from the slurry discharge port 14 by the impact generated by the cavitation 13 bursting.
By generating cavitation in the solvent, the method of mixing the powder and the oily component reduces the impact force on the powder compared to mixing using media, and also allows the high-pressure fluid to flow at high speed. In addition, the droplets of the oily component in the slurry become flat, and it becomes possible to cover many powders.

Examples of the high-pressure fluid mixer described above include NanoVita (manufactured by Yoshida Kikai Kogyo Co., Ltd.), nano3000 (manufactured by Miyu Co., Ltd.), and Starburst (manufactured by Sugino Machine Co., Ltd.).
The high pressure means, for example, that the pressure applied by an intensifier is higher than the atmospheric pressure, preferably 10 MPa or more, more preferably 30 MPa or more.

Hereinafter, powders, oily components, and the like to be contained in the slurry in the slurry preparation step will be described. 1) Powder The powder that can be used in this embodiment is a general term for organic or inorganic solids that do not dissolve in cosmetic raw materials such as water, oils and fats, surfactants, alcohols, and silicones.
Specific examples of the powder include kaolin, talc, mica, sericite, titanium mica, laminated resin particles (glitter), Ca / Al borosilicate, titanium sericite, titanium dioxide, iron oxide, zinc oxide, ultramarine, navy blue, Red No. 102, Red No. 226, Yellow No. 4 Aluminum lake, silica, alumina, calcium silicate, magnesium silicate, calcium carbonate, magnesium carbonate, methylsiloxane network polymer, cross-linked methylpolysiloxane resin, alkyl acrylate resin, nylon , Silk, cellulose or a composite material thereof.
The shape of the powder may be spherical, amorphous, porous, hollow, fibrous, plate-like or massive. Further, the surface may be subjected to a generally known surface treatment such as a silicone coating treatment, a metal soap coating treatment, and an acyl amino acid salt coating treatment.

The powder may be used alone in the slurry, or may be used in combination of two or more.
In the present embodiment, the content of the powder in the powder cosmetic is usually 70% by mass or more, preferably 75% by mass or more, more preferably 80% by mass or more, and more preferably 85% by mass or more. Is more preferred. Further, it is usually 98% by mass or less, and preferably 95% by mass or less.

In the slurry preparation in the present embodiment, since the impact force received by the powder is small as compared with a mixer using a medium such as a medium stirring mill, it is effective when the extender pigment or the like contains a powder having a large particle diameter. is there. When the average particle diameter (D ₅₀ ) contains a powder of 20 μm or more, when the average particle diameter (D ₅₀ ) contains a powder of 25 μm or more, the powder having an average particle diameter (D ₅₀ ) of 30 μm or more is used. When it contains, it is preferably applied.
Further, since the impact force applied to the powder is small, the damage to the powder is small, which is effective when the powder contains a fragile or easily damaged powder. It is preferably applied to a case containing a glitter powder, a case of containing a flaky powder, and the like.
It is also effective when two or more kinds of powders having different particle diameters, such as the above-mentioned powder having a large particle diameter and fine powder, are contained.
Examples of the fine particle powder include fine particle titanium oxide and fine particle zinc oxide. Here, the fine particle having an average particle diameter (D ₅₀ ) of 10 μm or less is referred to as 5 μm or less, 1 μm or less, and 500 nm. Or less, and may be 100 nm or less.

  The viscosity of the prepared slurry is not particularly limited, but is usually 100 mPa · s or more, preferably 1000 mPa · s or more, and usually 6000 mPa · s or less, and preferably 5000 mPa · s or less.

2) Oily component Specific examples of the oily component that can be used in the present embodiment include macadamia nut oil, avocado oil, corn oil, olive oil, rapeseed oil, sesame oil, castor oil, safflower oil, cottonseed oil, jojoba oil, coconut oil, Animal and vegetable oils such as palm oil and liquid lanolin; hydrocarbon oils such as liquid paraffin, squalane and pristane; liquid fatty acids such as oleic acid and isostearic acid; liquid higher alcohols such as isostearyl alcohol and octyl dodecanol; cetyl isooctanoate and myristine Isopropyl acid, hexyldecyl isostearate, diisopropyl adipate, di-2-ethylhexyl sebacate, cetyl lactate, diisostearyl malate, ethylene glycol di-2-ethylhexanoate, neopentyl glycol dicaprate, di-2-heptyl Glycerin undecanoate, glyceryl tri-2-ethylhexanoate, cetyl ethylhexanoate, trimethylolpropane tri-2-ethylhexanoate, trimethylolpropane triisostearate, pentaneerythrit tetra-2-ethylhexanoate, glyceryl triisoate Synthetic ester oils such as stearate and glyceryl triisooctanoate; chain polysiloxanes such as dimethylpolysiloxane, methylphenylpolysiloxane and diphenylpolysiloxane; octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexanesiloxane and the like Cyclic polysiloxanes such as amino-modified polysiloxane, polyether-modified polysiloxane, alkyl-modified polysiloxane, and fluorine-modified polysiloxane Silicone oils such as Rokisan; and the like. However, those belonging to a specific surfactant group described later are not treated as oily components.

The oil component may be used alone or in combination of two or more.
When the oil component is blended in this embodiment, it is usually at least 5% by mass, preferably at least 10% by mass in the cosmetic. Further, it is usually at most 25 mass%, preferably at most 20 mass%.

3) Solvent The solvent may be any solvent that is generally used for preparing a slurry. Examples include purified water, volatile silicone oils, lower alcohols, ethers, volatile hydrocarbon oils, pyrrolidones, and the like. Further, these may be used as a mixture.
The amount of the solvent may be an amount sufficient to mix the powder and the oil component, and is usually used in an amount of 50 parts by mass or more and 200 parts by mass or less based on 100 parts by mass of the powder.

4) Others The powder cosmetics manufactured in the present embodiment can widely mix components commonly used in powder cosmetics.

For example, examples of the active ingredient include a whitening ingredient, an anti-inflammatory ingredient, a plant extract and the like.
Examples of the surfactant include anionic surfactants such as fatty acid soaps (sodium laurate, sodium palmitate, etc.), potassium lauryl sulfate, triethanolamine ether alkyl sulfate, stearyltrimethylammonium chloride, benzalkonium chloride, lauryl Cationic surfactants such as amine oxides,
Betaine surfactants (alkyl betaine, amidobetaine, sulfobetaine, etc.), imidazoline amphoteric surfactants (2-cocoyl-2-imidazolinium hydroxide-1-carboxyethyloxy disodium salt, etc.), acylmethyltaurine Amphoteric surfactants such as
Sorbitan fatty acid esters (sorbitan monostearate, sorbitan sesquioleate, etc.), glycerin fatty acids (glycerin monostearate, etc.), propylene glycol fatty acid esters (propylene glycol monostearate, etc.), hydrogenated castor oil derivatives, glycerin alkyl ether POE sorbitan fatty acid esters (POE sorbitan monooleate, polyoxyethylene sorbitan monostearate, etc.), POE sorbite fatty acid esters (POE-sorbitol monolaurate, etc.), POE glycerin fatty acid esters (POE-glycerin monoisostearate) Rate), POE fatty acid esters (polyethylene glycol monooleate, POE distearate, etc.), POE alkyl ethers (POE2-octylde Sile ethers), POE alkyl phenyl ethers (POE nonyl phenyl ether, etc.), pluronics, POE / POP alkyl ethers (POE / POP2-decyl tetradecyl ether, etc.), tetronics, POE castor oil / hardened castor Non-ionic surfactants such as oil derivatives (POE castor oil, POE hardened castor oil, etc.), sucrose fatty acid esters, alkyl glucosides, and the like.

  Polyhydric alcohols include polyethylene glycol, glycerin, 1,3-butylene glycol, erythritol, sorbitol, xylitol, maltitol, propylene glycol, dipropylene glycol, diglycerin, isoprene glycol, 1,2-pentanediol, 2,4 -Hexylene glycol, 1,2-hexanediol, 1,2-octanediol and the like.

  Examples of the thickener include guar gum, quince seed, carrageenan, galactan, gum arabic, pectin, mannan, starch, xanthan gum, curdlan, methylcellulose, hydroxyethylcellulose, carboxymethylcellulose, methylhydroxypropylcellulose, chondroitin sulfate, dermatan sulfate, glycogen, Heparan sulfate, hyaluronic acid, sodium hyaluronate, tragacanth gum, keratan sulfate, chondroitin, mucoitin sulfate, hydroxyethyl guar gum, carboxymethyl guar gum, dextran, kerato sulfate, locust bean gum, succinoglucan, caronic acid, chitin, chitosan, carboxymethyl Chitin, agar, polyvinyl alcohol, polyvinylpyrrolidone, carboxyvinyl polymer, al Le-modified carboxyvinyl polymers, sodium polyacrylate, polyethylene glycol, and bentonite.

Examples of the ultraviolet absorber include a paraaminobenzoic acid ultraviolet absorber, an anthranilic acid ultraviolet absorber, a salicylic acid ultraviolet absorber, a cinnamic acid ultraviolet absorber, a benzophenone ultraviolet absorber, a sugar ultraviolet absorber, and 2- (2 UV absorbers such as'-hydroxy-5'-t-octylphenyl) benzotriazole and 4-methoxy-4'-t-butyldibenzoylmethane.

  The method of forming the slurry in the slurry preparation is not particularly limited as long as the above-mentioned fluid mixer is used, and a known method can be used. For example, a slurry can be formed by introducing a solvent to which a powder, an oily component, and other components are added as necessary, into the above-described mixer, and flowing the same as a high-pressure fluid in the chamber.

<Drying process>
The drying step is a step of drying the prepared slurry to obtain a powder cosmetic. The method is not particularly limited, and a known method can be used.
For example, a powder cosmetic may be obtained by making the slurry into fine droplets by mechanical shearing force and sending the drying gas to the fine droplets to dry the slurry. The obtained powder cosmetic may be molded by press molding or the like as necessary.
The solid powder cosmetic may be obtained by removing the solvent from the prepared slurry, filling the slurry into a container such as a metal or resin middle plate, and then performing dry press molding. In this case, a pulverizing step of pulverizing the remaining bulk after removing the solvent from the slurry may be provided.
Alternatively, after the prepared slurry is filled in a container such as a metal or resin middle plate, suction press molding may be performed.

  Hereinafter, the present invention will be described in more detail by way of examples, but the technical scope of the present invention is not limited to only the illustrated examples.

(Example 1, Comparative Example 1)
<Slurry preparation>
100 parts by mass of the mixture of the powder and the oil agent shown in Table 1 was added to 60 parts by mass of the solvent (hydrogenated polyisobutene). A solvent containing a powder and an oil agent was introduced into a high-pressure fluid mixer Starburst (manufactured by Sugino Machine Co., Ltd.) schematically shown in FIG. 2 to prepare a slurry (Example 1). In preparing the slurry, the pressure of the fluid in the mixer was increased to about 70 MPa by a pressure intensifier.
As Comparative Example 1, a slurry was prepared using a PICO MILL “PCM-LR” (manufactured by Asada Iron Works Co., Ltd.), which is a stirrer using media instead of starburst.
<Molding>
The prepared slurry was filled in a resin-made middle dish and dried to obtain powdered solid cosmetics according to Examples and Comparative Examples.

<Evaluation>
The obtained powdery solid cosmetics were evaluated as follows. Table 2 shows the results.
・ Amount of removal The amount of removal was evaluated by using a puff (52 × 44 × 8.5 mm) made of NBR (nitrile rubber) and sliding the powdered solid cosmetic surface three times under a load of 2.9 N, and placing it on the puff. This was done by measuring the powdered cosmetics.
(Standard)
◎: 9 or more of the 10 respondents answered that the puff was good ○: 6 to 8 of 10 respondents answered that the puff was good △: 3 to 5 out of 10 responded to the puff Good ×: 0 to 2 out of 10 responded that puff was good

・ Smoothness (standard)
◎: 9 or more out of 10 respondents answered that the feel was smooth ○: 6 to 8 out of 10 respondents felt that the feel was smooth Δ: 3 to 5 out of 10 respondents felt that the feel was smooth ×: 0 out of 10 ~ 2 respondents felt smooth

・ Gloss (standard)
◎: 9 or more of 10 respondents have gloss ○: 6 to 8 of 10 respondents have gloss △: 3 to 5 of 10 respondents have gloss ×: 0 of 10 ~ 2 respondents have gloss

・ SPF
Each pressed powder was applied to a surgical tape (Transpore 3M Healthcare Co., Ltd.) at a loading amount of ² mg / cm ² in an area of 6.4 cm × 6.4 cm, and L
The SPF value was determined from the average protection spectrum obtained by measuring 10 times using a UV-2000S SPF analyzer manufactured by Absphere. In Table 2, the relative values are shown with the measured value of Example 1 taken as 1.

From the results in Tables 1 and 2, although the prescription was the same, there was a difference in the evaluation of the removal amount, smoothness, and gloss. This difference is due to the fact that the use of a medialess mixer in the preparation of the slurry in Example 1 makes it possible to use a synthetic metal powder that imparts functions such as easy removal from puffs, smoothness, and luster to cosmetics. This is due to the fact that mica (D ₅₀ : 12 μm), boron nitride (D ₅₀ : 6 μm), and bismuth oxychloride (D ₅₀ : 10 μm) were blended into the cosmetic while keeping their particle diameters almost unchanged. In addition, the talc and mica, which are extenders, do not show a significant decrease in average particle size.
On the other hand, in Comparative Example 1, which was a stirrer using a medium, the particle size of the powder imparting the above function was reduced by over-pulverization, and the particle size of talc and mica, which are extenders, was reduced throughout. I was

10, 20 high-pressure fluid mixer 1, 11 chamber 2a, 2b material supply port 12 material supply port 12a orifice 3 collision point 13 cavitation 4, 14 discharge port

Claims (4)

A method for producing a powder cosmetic, comprising: a slurry preparation step of preparing a slurry by mixing at least a powder and an oily component in a solvent; and a drying step of drying the prepared slurry to obtain a powder cosmetic. And
The powder contains at least two kinds of powder having different particle diameters,
In the slurry preparation step, using a high-pressure fluid mixer that mixes the powder and the oily component by flowing the solvent containing the powder and the oily component through the chamber as a high-pressure fluid of 30 MPa to 70 MPa , Production method.   2. The powder according to claim 1, wherein the high-pressure fluid mixer discharges a solvent containing the powder and the oil component as a high-pressure fluid, and mixes the powder and the oil component by obliquely colliding the high-pressure fluids with each other. 3. Manufacturing method of body cosmetics.   The method for producing a powder cosmetic according to claim 1, wherein the high-pressure fluid mixer mixes the powder and the oily component by an impact generated by rupture of cavitation generated in the chamber. The powder had an average particle diameter D ₅₀ of less 5μm fine, having an average particle diameter D ₅₀ of at least the above extender pigment 20 [mu] m, the powder cosmetic according to any one of claims 1 to 3 Production method.

Images