JP3274024B2 - Manufacturing method of cosmetics - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a method for producing a cosmetic containing fine inorganic powder which has been surface-coated with a specific organosilicon compound.

[0002]

2. Description of the Related Art Fine-particle inorganic powders such as fine-particle titanium oxide and fine-particle zinc oxide have an ultraviolet shielding effect and are therefore used as sunscreen cosmetics by blending them into cosmetics (Japanese Patent Publication No. 47-42502). JP-A-49-45
0, JP-A-64-7941 and the like).

[0003] In order to sufficiently exhibit the ultraviolet shielding effect of the fine particle inorganic powder blended in the above-mentioned cosmetics, it is necessary to use them in a state of being sufficiently dispersed in the blending system. A method has been studied in which an inorganic powder is surface-coated with an organic compound, an organometallic compound, or the like, and then blended into a cosmetic (JP-A-58-49307, JP-A-59-172415, and JP-A-59-172415). 621-2450
No. 11, JP-A-62-67015).

[0004]

However, even if the powder is surface-coated with an organic compound or an organometallic compound, the surface-coated powder provided by a general treatment has a low cohesive force of the base material. Despite the size of the particles due to the difference, the surface treatment is usually performed on aggregated particles of several tens to several hundreds of single particles.

[0005] For this reason, if a strong dispersion is applied when blended into a cosmetic, the agglomerated particles of the above-mentioned surface-coated powder are broken or a paste formed by three rolls or formed by pressing. In this case, as a result, a force as a re-grinding process acts, so that the agglomerated particles are broken even by such a process, and as a result, the surface not subjected to the surface coating treatment is exposed, and the characteristics are deteriorated. Had become.

When the surface-coated powder is blended into a cosmetic, a homogenizer or a Henschel mixer or other disperser or pulverizer having only a weak dispersing power does not expose the uncoated surface, but the powder is not exposed. It could not be blended with the body fully dispersed.

[0007] Moreover, in the actual production of cosmetics,
In addition to inorganic ultraviolet shielding agents such as fine-particle titanium oxide, in many cases, plate-like mineral powders such as sericite, mica, and talc are blended. Even the powdery powder is crushed, which impairs the properties of the manufactured cosmetic in terms of slipperiness and the like.

In addition, it is not impossible to mix only the surface-coated fine inorganic powder into a cosmetic after pre-dispersion. However, in this case, the number of steps is increased, and especially in the case of a solid, It also disturbs the state of dispersion of the cosmetic.

For the above reasons, there has been a demand for a cosmetic composition which can be sufficiently dispersed even when blended with a weak dispersing power and has a high ultraviolet shielding effect.

[0010]

According to the present invention, there is provided a fine particle inorganic powder which can be easily dispersed even with a weak dispersing power, and which does not expose a surface which has not been subjected to surface coating even when a strong dispersion is applied. To provide cosmetics with excellent ultraviolet shielding effect.

That is, the present invention uses a step of wet pulverization or wet pulverization using a sand grinder mill to select from fine particle titanium oxide and fine particle zinc oxide having an average particle diameter of 0.1 to 0.01 μm. At least one selected from the group consisting of at least one selected from the group consisting of fine inorganic powder or fine titanium oxide and fine zinc oxide, and 10 wt% of the whole fine silica or fine iron oxide as a sub-base material
A fine particle inorganic powder containing:
1 to 30 parts by weight of methyl hydrogenated polysiloxane, decylsilane, tetramethylcyclotetrasiloxane, dimethylpolysiloxane having a viscosity of 2 to 100 cs, one or more organic substances selected from octamethylcyclotetrasiloxane and dimethylsilane with respect to parts by weight The present invention relates to a method for producing a cosmetic by applying a surface coating treatment with a silicon compound and blending a fine inorganic powder surface-treated with the organic silicon compound.

In the present invention, utilizing a step of wet pulverization or wet pulverization by a sand grinder mill,
Since the specific fine particle inorganic powder is surface-coated with a specific organic silicon compound, the resulting surface-coated fine particle inorganic powder is fine and uniform, so that it has only a weak dispersing power when dispersing. Even if a disperser is used, the dispersion can be sufficiently dispersed, and even if strong dispersion is applied, the surface coating does not peel off.

Hereinafter, the present invention will be described in more detail. The fine particle inorganic powder used in the present invention is composed of at least one selected from fine particle titanium oxide and fine particle zinc oxide, or is composed mainly of one or more fine particle inorganic powder selected from fine particle titanium oxide and fine particle zinc oxide. Containing 10% by weight or less of the entirety of fine silica or fine iron oxide as a sub-base material. In other words, as in the latter case, when one or more fine particles of inorganic oxide selected from fine particles of titanium oxide and fine particles of zinc oxide are used as the main substrate, the fine particles of the present invention use the main substrate as a sub-substrate. 90% by weight in total
The above is included. The description of these fine particles of titanium oxide, fine particles of zinc oxide, fine particles of silica and fine particles of iron oxide is as follows.

Fine particle titanium oxide: Unlike ordinary titanium oxide for white pigments, having an average particle diameter of 0.1 to 0.01 μm, it has light transmittance in the visible light region and ultraviolet light, particularly UV-light. Since it has an excellent ultraviolet shielding effect in the B region, it is used in cosmetics and the like as described above. In the present invention, the fine particle titanium oxide can be used in any crystal form such as rutile type, anatase type and amorphous type.

Fine-particle silica: A finer powder than fine-particle titanium oxide is commercially available. By mixing this fine-particle silica, aggregation of fine-particle titanium oxide can be suppressed, and the distance between individual fine-particle titanium oxide particles can be increased. it can.
As a result, although the particulate silica itself has almost no ultraviolet ray shielding effect, the ultraviolet ray shielding effect as a composite is improved.

Fine particle zinc oxide: The particles themselves are particles having strong aggregation, and it is necessary to disintegrate the particles and perform a surface coating treatment. One of the disadvantages of UV
The ultraviolet shielding effect in the -A region can be complemented.

Fine-particle iron oxide: It complements the characteristics of fine-particle inorganic powder such as fine-particle titanium oxide having an ultraviolet shielding effect, and can provide a beige composite powder.
Such a composite powder is obtained, for example, by subjecting uniformly mixed fine particles of titanium oxide and iron oxide to a surface coating treatment with the above-mentioned organosilicon compound, and thus, when doping or depositing titanium oxide and iron oxide. In the same manner as described above, the powder can be finished without causing color separation.

The organic silicon compound used in the present invention is at least one selected from methyl hydrogenated polysiloxane, decylsilane, tetramethylcyclotetrasiloxane, dimethylpolysiloxane having a viscosity of 2 to 100 cs, octamethylcyclotetrasiloxane, and dimethylsilane. It becomes.

Here, the organosilicon compound used in the present invention will be described more specifically.

The methyl hydrogenated polysiloxane specifically refers to methyl hydrogenated polysiloxane, methyl hydrogenated cyclopolysiloxane and the like.

The dimethylpolysiloxane specifically refers to dimethylpolysiloxane, cyclodimethylpolysiloxane and the like.
100 cs (centistokes) is used. If the viscosity is lower than 2 cs, it is difficult to perform the surface coating treatment, and if the viscosity is higher than 100 cs, the dispersibility is not sufficient.

The surface coating treatment of the fine inorganic powder to be incorporated into the cosmetic composition of the present invention is essentially required to utilize a step of wet pulverization or wet pulverization using a sand grinder mill. As a specific example, first,
Usually, after the above-mentioned specific fine inorganic powder, organic silicon compound, solvent and the like are preliminarily mixed, the mixture is supplied to a sand grinder mill to perform a surface coating treatment, and then the solvent is removed to form a powder.

A sand grinder mill is a method in which beads are filled as media in a container, and a stirring disk attached perpendicularly to a rotation axis is rotated at a high speed to crush and disperse agglomerated particles of the base material powder. There are various types of devices, such as a vertical type and a horizontal type, a continuous type and a batch type, for the structure of the device. Any material can be used as long as the surface coating treatment can be performed on the organic silicon compound while the inorganic powder is wet pulverized or wet pulverized.

As the beads using the above-mentioned sand grinder mill, balls made of glass, alumina, zircon, zirconia, steel, flint stone or the like can be used, but those having high hardness and true specific gravity in order to avoid contamination are used. Zirconia and zircon are particularly preferred. In addition, the size of the beads is usually about 1 to 2 mm in diameter, but since the base powder used in the present invention is fine particles, it is 0.3 to 1.0 mm.
It is preferable to use one having a size of about mm.

As the stirring disk used in the sand grinder mill, various materials such as stainless steel, nylon, ceramics and the like can be usually used, and the base powder used in the present invention is an inorganic powder. For this reason, it is preferable to use a ceramic made of abrasion resistance. In particular, when using zirconia or zircon beads as described above, it is preferable to use a zirconia disk.

There are no particular restrictions on the solvent used for wet grinding or wet grinding, and various alcohols such as water, methanol, ethanol and isopropyl alcohol,
Various organic solvents such as benzene, toluene, paraffin and the like may be used singly or as a mixture of two or more, depending on the degree of dispersion of the fine inorganic powder and the characteristics of the organosilicon compound to be used.

In the wet pulverization or wet pulverization, the mixing ratio of each component such as the fine inorganic powder of the base material, the organosilicon compound, the solvent, and the like depends on the intended quality of the final product and the efficient wet process conditions. For the selection, it is necessary to appropriately select the ratio depending on the type and combination of the medium to be used.
Used in the range of 30 parts by weight.

The fine inorganic powder which has been surface-coated with the organosilicon compound obtained by the above-mentioned process can be used as a raw material for cosmetics as it is or dispersed in a solvent such as alcohol or water. Or kneaded in resin.

By using the finely divided inorganic powder surface-coated with the organosilicon compound obtained above, white powder,
Foundation, pressed powder, water-based foundation, oil-based foundation, emulsified foundation, lipstick, blusher, eyeshadow, eyebrow ink, eyeliner,
It is possible to produce cosmetics such as mascara, nail color, cheek color, base foundation, sunscreen, emulsion, lotion and the like.

The cosmetics of the present invention include oils, powders, solvents, surfactants, ultraviolet absorbers, preservatives, sterilizers and the like which are usually used in cosmetics within a range that achieves the object of the present invention. Agents, preservatives, antioxidants, hormones, vitamins, humectants, fragrances and the like can be arbitrarily compounded.

[0033]

According to the present invention, the fine particle inorganic powder surface-treated with the organic silicon compound is pulverized into fine particles and simultaneously surface-coated with the organic silicon compound, and the organic silicon compound is brought to a particle surface close to the primary particles. Surface coating treatment, it can be sufficiently dispersed in cosmetics even if using a disperser with only a weak dispersing power. Cosmetic with excellent properties such as UV shielding as a result of greatly improved dispersibility compared to cosmetics containing surface-coated powders that are generally provided without the appearance of a treated surface Is effective as

[0034]

Next, the present invention will be described in more detail with reference to specific examples, but the present invention is not limited to these examples.

A. Manufacture of Surface-Coated Fine Particle Inorganic Powder Sample 1-12 In this sample 1-12, Table 1 and Table 2 show the total of 1,000 g of the fine particle inorganic powder containing the fine particle titanium oxide as the base material. Each type and amount of the surface treating agent and the solvent were blended and mixed with a stirrer to prepare a slurry, which was further subjected to wet pulverization using a horizontal continuous sand grinder mill. The residence time of the slurry in the mill was 5 minutes. The slurry after the treatment was put into a kneader, and the solvent was removed by heating under reduced pressure to obtain a surface-coated powder. Samples 1 to 10 belong to the present invention, and samples 11 to 12 are out of the present invention. These will be described in more detail below. In Sample 2-5, as a fine particle inorganic powder serving as a base material, a type and amount of a sub-base material shown in Table 1 were mixed with fine particle titanium oxide to make a total of 1,000 g. Sample 1-
Regarding 5, 9, 10 and 12, the surface-coated powder obtained by the above-mentioned surface-coating treatment is further added with 120 to 15 particles.
The curing was performed at a temperature of 0 ° C. In addition, the size of each fine particle titanium oxide is the same as that of samples 1, 2, 4, 5,
For 35, 35 nm (nanometer), sample 3,
For 6-12, those having an average particle diameter of 15 nm were used.

Sample 13 Sample 13 is obtained by subjecting a fine particle inorganic powder as a base material to a surface coating treatment by a conventional method, and using the same kind of base material, surface treatment agent and solvent as in Sample 1, After mixing with the same ratio as Sample 1 and mixing with a blade-type stirrer to prepare a slurry, the mixture was directly charged into a kneader without performing wet disintegration treatment by a sand grinder mill, heated under reduced pressure, and the solvent was removed to remove the solvent. The coated powder was obtained and further cured at a temperature of 120 to 150 ° C.

Sample 14-16 This sample 14-16 uses a material containing fine zinc oxide as a substrate and belongs to the present invention. That is, with respect to a total of 1,000 g of the fine particle inorganic powder containing the fine particle zinc oxide, the types and amounts of the surface treatment agent and the solvent shown in Table 3 were blended and mixed with a stirrer to prepare a slurry. The wet crushing treatment was performed using a horizontal continuous sand grinder mill. The residence time of the slurry in the mill was 5 minutes. The slurry after treatment is
The mixture was put into a kneader, and the solvent was removed by heating under reduced pressure to obtain a surface-coated powder, which was further cured at a temperature of 120 to 150 ° C. In addition, about the sample 14,
Samples 15, 16 using fine zinc oxide as the base material
As for the base material, a type and amount of a sub-base material shown in Table 3 were mixed with fine-particle zinc oxide to give a total of 1,000 g.

[0038]

[Table 1]

[0039]

[Table 2]

[0040]

[Table 3]

* 1 KF99 manufactured by Shin-Etsu Chemical Co., Ltd. * 2 KBM3103 * 3 manufactured by Shin-Etsu Chemical Co., Ltd. LS-8600 * 4 KF96 20CS manufactured by Shin-Etsu Chemical Co., Ltd. * 5 KF994 manufactured by Shin-Etsu Chemical Co., Ltd. * 6 Shin-Etsu Chemical KBM22 * 7 manufactured by Kogyo Co., Ltd. KF96 1000CS * 8 manufactured by Shin-Etsu Chemical Co., Ltd. LS-6970 manufactured by Shin-Etsu Chemical Co., Ltd. In addition, the fine particle inorganic powder which was surface-coated with the organosilicon compound of Samples 1-10 and 14-16 was compounded. The cosmetic is a cosmetic belonging to the present invention.

B. Comparison of dispersibility The light transmittance of a liquid paraffin dispersion system was measured using a paint conditioner to evaluate the dispersibility of each surface-coated powder of Sample 1-16 produced above. 1.35 g of each sample powder is placed in a glass bottle with a capacity of 140 ml and covered with liquid paraffin.
70 was added to 52.0 g and a dispersant 5.2 g, and 1.5
60 g of mm glass beads were added and dispersed for 5 minutes with a paint conditioner (Red Devil). The obtained paste is applied on a polyester film by using a bar coater # 8, and a spectrophotometer (UV-31 manufactured by Shimadzu Corporation) is used.
00), the light transmittance (ultraviolet transmittance) of ultraviolet (300 nm) was measured.

Table 4 shows the obtained results. Since the fine particle titanium oxide has a function of scattering ultraviolet light, if the surface-coated powder is sufficiently dispersed, as a result, the ultraviolet light transmittance of the paste becomes small. Therefore,
The smaller the UV transmittance, the better the dispersibility.

[0044]

[Table 4]

As shown in Table 4 above, when dispersed in liquid paraffin, which is a kind of oil frequently used in cosmetics, as is apparent from the difference in ultraviolet transmittance between Sample 1 and Sample 13, a sand grinder was used. The product of the present invention (sample 1 blended product) in which fine inorganic powder surface-treated with a specific organosilicon compound is blended by utilizing a process of wet pulverization or wet disintegration using a mill has the same dispersion conditions. However, since the ultraviolet transmittance is lower than that of the comparative product (compound of sample 13), it is understood that the dispersibility is more excellent. Furthermore, as is clear from comparison of the ultraviolet transmittances of Samples 1-10 and Samples 11 and 12, even when the surface coating treatment is performed through the same wet crushing step, the organic silicon compound as a surface treatment agent is treated. The dispersibility differs depending on the type, and it can be seen that the samples belonging to the present invention have excellent dispersibility.

Example 1 A foundation was prepared according to the following formulation. The compounding amount is% by weight. (1) Surface coated fine particles of sample 1 Titanium oxide 10.0 (2) Titanium oxide 10.0 (3) Talc 28.0 (4) Sericite 32.0 (5) Iron oxide 5.0 (6) Flow Paraffin 10.0 (7) Methylpolysiloxane 4.0 (8) Sorbitan monooleate 1.0 (9) Antioxidant appropriate amount (10) Fragrance appropriate amount Mix (1) to (5) with a Henschel mixer, (6) to (10), which were previously mixed and dissolved uniformly, were added and mixed well. Next, this was pulverized and compression-molded.

Comparative Example 1 A foundation was prepared in the same manner as in Example 1 except that the sample 13 was coated with the surface-coated titanium oxide particles instead of the surface-coated titanium oxide particles.

Using the foundations prepared in Example 1 and Comparative Example 1, the UV transmittance at 300 nm was measured in the same manner as in "B. Comparison of dispersibility" described above.
Table 5 shows the obtained results.

Example 2 A sunscreen was prepared according to the following formulation. The compounding amount is% by weight. (1) UV absorber (phenyl salicylate) 2.0 (2) Surface-coated fine particle titanium oxide of sample 10 10.0 (3) Kaolin 2.5 (4) Cetyl alcohol 4.0 (5) Vaseline 5.0 (6) Liquid paraffin 10.0 (7) Silicon oil 2.0 (8) Glyceryl monostearate 2.5 (9) Polyoxyethylene cetyl alcohol ether 3.0 (10) Propylene glycol 5.0 (11) Ethanol 54.0 (12) Appropriate amount of fragrance (13) Appropriate amount of preservative Mix and dissolve components other than (2) and (3) uniformly, and gradually add (2) and (3) to it. And mixed and dispersed with a homomixer to obtain a product.

Comparative Example 2 A sunscreen agent was prepared in the same manner as in Example 2 except that the surface-coated fine particle titanium oxide of Sample 12 was used instead of the surface-coated fine particle titanium oxide of Sample 10.

The sunscreen agents prepared in Example 2 and Comparative Example 2 were applied as they were on a quartz plate using a film applicator (gap 34 μm),
Was measured for ultraviolet transmittance. Table 5 shows the obtained results.
Shown in

[0054]

[Table 5] As is clear from Table 5, the foundation of Example 1 had a lower ultraviolet transmittance at 300 nm and an excellent ultraviolet shielding effect than the corresponding foundation of Comparative Example 1. Further, the sunscreen agent of Example 2 had a lower ultraviolet transmittance at 300 nm and an excellent ultraviolet shielding effect than the corresponding sunscreen agent of Comparative Example 2.

──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-4-202109 (JP, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) A61K ^7/ 00-7/50

Claims (1)

(57) [Claims] 1. A sand grinder with mill By giving you access to the step of wet-milling or wet pulverization, fine titanium oxide average particle diameter 0.1～0.01Myuemu, fine
One or more particulate inorganic powders selected from particulate zinc oxide
Or one selected from fine particle titanium oxide and fine particle zinc oxide
Fine silica or fine iron oxide with at least seed
Is used as a sub-base material in an amount of 1 to 10 parts by weight based on 100 parts by weight of the fine particle inorganic powder.
30 parts by weight of methyl hydrogenated polysiloxane, decylsila
, Tetramethylcyclotetrasiloxane, viscosity 2-1
00cs dimethylpolysiloxane, octamethylcycl
Selected from rotetrasiloxane and dimethylsilane
Surface coating with one or more organosilicon compounds
A method for producing a cosmetic, comprising mixing a fine particle inorganic powder surface-treated with a silicon compound .