JP4157500B2 - Multi-layer composition - Google Patents

Description

  The present invention relates to a multilayer composition, and more particularly to a multilayer composition having a powder dispersion layer as an uppermost layer of an aqueous phase and excellent in redispersibility.

  Multi-layer composition, especially non-viscous or low-viscosity multi-layer composition with powder, demands for sebum adsorption effect, convergence effect, skin unevenness correction effect, non-sticky feeling, etc. by powder Is expensive. These are powder sediment type multi-layer compositions having a powder layer in the lower layer, and conventionally used powders include inorganic powders such as zinc oxide, titanium oxide, silicic anhydride, mica, talc, polyethylene, polymethacrylate Resin powders such as cellulose, organic powders such as cellulose and starch, clay minerals and the like have been used.

  However, these powders are prone to agglomeration, and even if the redispersibility in the multilayer composition is improved by some method, they settle in the composition in a stationary state. There was a problem that redispersibility was lowered by vibration and vibration. In consideration of redispersibility, the powder is preferably located in the upper layer in the composition in a stationary state.

  On the other hand, with diversification of lifestyles, various functions are required for the composition, and among them, a composition excellent in light touch is required. In particular, in order to improve the light touch feeling of the skin care composition, improvement of the feeling is attempted by using a spherical powder or a surface-treated powder as the powder.

Various techniques are known as a low-viscosity multilayer composition containing a powder.
For example, in Patent Document 1, a two-phase composition using a powder covering the surface of a resin powder is mentioned, but even in this case, if the powder is in a stationary state, the powder is precipitated, It cannot be denied that the redispersibility of the powder decreases with time and vibration.
On the other hand, a cosmetic in which a silicone crosslinked elastic body is stably dispersed in an aqueous phase is obtained by containing an alkyl-modified carboxyvinyl polymer (see Patent Document 2), but this cosmetic does not undergo layer separation, Uniformly dispersed.

  Furthermore, as a powdery cosmetic material that has a powder phase that does not harden and is soft when applied, it is formulated by combining active powders such as kaolin and zinc oxide with hollow particles based on acrylic or methacrylic polymers or copolymers. Is known (see Patent Document 3). However, active powders such as kaolin and zinc oxide have a high specific gravity, and if this powder and hollow resin powder are simply blended, caking (solidification) occurs in the upper layer of the aqueous phase, resulting in poor redispersibility. It could not be stably blended into the upper layer.

Japanese Patent No. 3273573 JP 2002-226320 A JP 2000-143434 A

  Therefore, with a multilayer composition containing powder, the powder disperses quickly when shaken, and the redispersibility of the powder can be maintained over time and external vibration, etc., and the powder dispersion layer is clearly visible in appearance Development of a composition having a separated layer structure has been desired.

  As a result of intensive studies in view of the above problems, the present inventors have dispersed a specific hollow resin powder and a polymethylsilsesquioxane-coated cross-linked silicone elastomer powder as a powder in an aqueous composition. A multi-layered composition that does not settle to the lower layer is obtained, and a composition that has a light feel and that has a powder layer on the liquid surface and that can express a light feel is also obtained. The inventors have found that dispersibility can be maintained, and have completed the present invention.

  That is, the present invention is a multilayer composition comprising an aqueous phase composed of two or more layers, the uppermost layer of the aqueous phase being a powder dispersion layer, wherein the powder dispersion layer is (a) true in a dry state. A multilayer composition comprising at least a hollow resin powder having a specific gravity of 0.01 to 0.9 and (b) a polymethylsilsesquioxane-coated crosslinked silicone elastomer powder.

  In the present invention, it is desirable to further blend a lower alcohol.

  Moreover, in this invention, it is desirable that the total compounding quantity of the said (a) component and the said (b) component is 0.1-15.0 mass% with respect to multilayer type composition whole quantity.

  Furthermore, in this invention, it is desirable that the compounding quantity of (a) component and (b) component is (a) :( b) = 2: 8-9: 1 by mass ratio.

  According to the present invention, when allowed to stand, the boundary between the aqueous layer and the upper powder dispersion layer is clearly a multilayered structure, and when shaken, the powder is excellent in redispersibility. It can be set as the multilayer type composition with a favorable feeling of use.

The best mode of the present invention will be described below.
(A) The hollow resin powder used in the present invention is a hollow resin powder having a true specific gravity of 0.01 to 0.9 in a dry state, and examples of the resin forming the outer shell include vinyl chloride, vinyl acetate, Vinyl monomers such as methyl vinyl ether, acrylic monomers such as acrylic acid, acrylic ester, methacrylic acid, methacrylic ester, acrylonitrile, methacrylonitrile, homopolymers or copolymers such as styrene, vinylidene chloride, divinylbenzene, ethylene glycol dimethacrylate Is mentioned.

  From the viewpoint of dispersibility of the hollow resin powder and good usability when used on the skin, the hollow resin powder has a true specific gravity of 0.01 to 0.9 in a dry state, and further has a true specific gravity of 0.3. It is preferable that it is -0.8, and the hollow resin powder which consists of an acryl-type polymer which consists of 1 type, or 2 or more types of monomers chosen from acrylic acid and / or methacrylic acid is used preferably.

  Even if these polymers are not bridge | crosslinked, they may be bridge | crosslinked with crosslinking agents, such as divinylbenzene, ethylene glycol dimethacrylate, and triacryl formal. The surface of the hollow powder may be coated with an inorganic material or may be coated with a hollow resin powder that is not coated with an inorganic powder in order to stably disperse it in the upper layer of the aqueous layer. It is preferable. Furthermore, it may be silicone-treated.

  The method for producing the hollow resin powder (a) used in the present invention is not particularly limited. For example, as disclosed in JP-B-59-53290, the thermoplastic resin powder containing a volatile foaming agent is heated. One obtained by a foaming method or one obtained by a non-foaming method obtained by subjecting a resin to suspension polymerization using an organic solvent and drying.

  Hollow resin powders are generally commercially available. For example, Matsumoto Microsphere MFL series [MFL-50STI (particle size 10-30 μm, true specific gravity 0.20), MFL-50SCA (particle size 10-30 μm) manufactured by Matsumoto Yushi Seiyaku Co., Ltd. , True specific gravity 0.29), MFL-80GCA (particle size 10-30μm, true specific gravity 0.20), MFL-80CA (particle size 90-110μm, true specific gravity 0.13), MFL-100SCA (particle size 20-40μm, true specific gravity 0.20) , MFL-100CA (particle size 90-110 μm, true specific gravity 0.13), MFL-30STI (particle size 10-30 μm, true specific gravity 0.20)] and Matsumoto Microsphere F-80ED (particle size 90-110 μm, true specific gravity 0.020) EXPANCEL microsphere 551 DE 40 d42 (particle size 30-50 μm, true specific gravity 0.042), 551 DE 40 d60 (particle size 15-25 μm, true specific gravity 0.06), 551 DE 80 d42 (particle size 50-80μm, true specific gravity 0.042), 461 DE 40 d60 (particle size 20-40μm, true specific gravity 0.06), 461 DE 20 d70 (particle size 15-25μm, true ratio) 0.07), 051 DE 40 d60 (particle size 20-40μm, true specific gravity 0.06), 091 DE 40 d30 (particle size 35-55μm, true specific gravity 0.03), 091 DE 80 d30 (particle size 60-90μm, true specific gravity 0.03) , 092 DE 40 d30 (particle size 35 to 55 μm, true specific gravity 0.032), 092 DE 80 d30 (particle size 60 to 90 μm, true specific gravity 0.032), Gantz Pearl GMH-0850 (particle size 8 μm, true specific gravity manufactured by Ganz Kasei Co., Ltd.) 0.65).

  Although the compounding quantity of the hollow resin powder in this invention is suitably prepared with the dosage form of a composition, Preferably it is 0.5-5 mass%, More preferably, it is 1-3 mass%. If the blending amount is less than 0.5% by mass, the smooth touch feeling of light touch is not sufficiently exhibited. On the other hand, if the blending amount exceeds 5% by mass, the whiteness when applied becomes remarkable, and the usability Is not preferable from the viewpoint of deterioration.

In the present invention, (a) a specific hollow resin powder and (b) a polymethylsilsesquioxane-coated crosslinked silicone elastomer powder are blended.
(A) When the hollow resin powder is blended alone, caking (solidification) occurs when left standing for a long period of time, and even if shaken, a part of the agglomerates does not re-disperse and the powder cannot be blended stably. However, by combining (a) hollow resin powder and (b) polymethylsilsesquioxane-coated crosslinked silicone elastomer powder, the powder layer is stable in the upper layer of the aqueous layer without caking (solidifying). When placed and shaken, it shows a remarkable effect of uniform redispersion.

  The (b) polymethylsilsesquioxane-coated crosslinked silicone elastomer powder used in the present invention is a silicone resin-coated silicone rubber powder obtained by coating a silicone rubber with a silicone resin. Examples of commercially available products include KSP100, KSP101, and KSP105. (Shin-Etsu Chemical Co., Ltd.).

  (B) The blending amount of the polymethylsilsesquioxane-coated crosslinked silicone elastomer powder is appropriately adjusted according to the dosage form of the composition, but is preferably 0.1 to 10% by mass, and more preferably 1 to 5%. % By mass. If the blending amount is less than 0.1% by mass, the anti-caking effect is reduced and the light touch feeling is not sufficient. On the other hand, if the blending amount exceeds 10% by mass, the whiteness becomes remarkable and the usability is increased. It is not preferable in terms of deterioration.

  (A) When powder other than (b) polymethylsilsesquioxane-coated cross-linked silicone elastomer powder is used as the powder combined with the hollow resin powder, a powder layer is present at the top and bottom, and caking is performed. There is a disadvantage that it ends up.

  When (a) hollow resin powder is not blended and (b) polymethylsilsesquioxane-coated cross-linked silicone elastomer powder is blended alone, a small amount of emulsifier is added without the powder itself getting wet with aqueous components. However, it floats on the surface like a part of it is agglomerated and cannot be stably arranged. In addition, when polymethylsilsesquioxane-coated crosslinked silicone elastomer powder is blended alone in an aqueous phase containing alcohol, a part of the powder is divided into an upper layer and a lower layer, and cannot be stably disposed in the upper layer of the aqueous layer.

  In the present invention, the total amount of (a) the hollow resin powder and (b) the polymethylsilsesquioxane-coated crosslinked silicone elastomer powder is preferably 0.6 to 15 with respect to the total amount of the multilayer composition. It is 1 mass%, More preferably, it is 1-5 mass%. When the blending amount is less than 0.6% by mass, the feeling of smoothness is not sufficient. On the other hand, when the blending amount exceeds 15% by mass, the coating color becomes too whitish and the usability deteriorates. Is not preferable.

  In the present invention, the blending ratio (mass ratio) of (a) hollow resin powder and (b) polymethylsilsesquioxane-coated crosslinked silicone elastomer powder is preferably (a) :( b) = 1: 9. -9: 1, more preferably 2: 8-5.5. By blending (a) and (b) at a specific ratio, caking (solidification) of the hollow resin powder can be prevented, and the powder layer can be stably disposed on the upper layer of the aqueous layer.

  In the present invention, powders other than (a) hollow resin powder and (b) polymethylsilsesquioxane-coated crosslinked silicone elastomer powder may be blended. It is preferable that it is 0.3 mass% or less.

  The multilayer composition of the present invention preferably further contains (c) a lower alcohol. (C) By blending the lower alcohol, the powder layer can be wetted, the specific gravity of the liquid itself can be reduced, and the effect of suppressing caking on the liquid surface of the hollow powder can be obtained.

  (C) Lower alcohol becomes like this. Preferably it is 1.0-45.0 mass% with respect to multilayer type composition whole quantity, More preferably, it is 20-38 mass%. If the blending amount is less than 1.0% by mass, it is not sufficient for wetting of the powder and also for suppressing caking. On the other hand, when the blending amount exceeds 45.0% by mass, the lower alcohol itself erodes into the hollow powder, and the powder phase settles, which is not preferable from the viewpoint of stability.

  The multilayer composition of the present invention can be obtained by dispersing a powder containing a silicone crosslinked elastic body in an aqueous component according to a conventional method.

  The multilayer composition of the present invention is a liquid composition and preferably has a viscosity at 25 ° C. of 500 mPa · s or less. When allowed to stand, the powder layer is stably disposed on the upper layer of the aqueous layer. In addition to the upper powder layer, it may be a composition of three or more layers in which another powder layer is disposed in the lower layer, or may be a composition of three or more layers in which an oily layer or the like is disposed in addition to the aqueous layer. .

  The multilayer composition of the present invention can be used as a lotion, antiperspirant, cleansing lotion, fragrance, colon, fragrance, deodorant spray, bathing agent, and the like. The multi-layer composition of the present invention is preferably used as a cosmetic because the powder has an interesting appearance with the powder positioned in the upper layer, and a good smooth feeling is obtained when applied to the skin.

  Furthermore, in the multilayer composition of the present invention, in addition to the above essential components, oils, activators, moisturizers, drugs, sequestering agents, polyhydric alcohols, antioxidants, as long as the effects are not disturbed Agents, preservatives, fragrances and the like can be blended.

  Next, the present invention will be described more specifically with reference to examples. The present invention is not limited to the examples. All compounding amounts are mass%. The evaluation method used the method mentioned later. In the table, (* 1) is Gantzpearl GMH-0850 (manufactured by Gantz Chemical Co., Ltd.), (* 2) is KSP100 (manufactured by Shin-Etsu Chemical Co., Ltd.), (* 3) is Tospearl 2000 (polymethylsilsesquioxane). At the end, GE Toshiba Silicone Co., Ltd. (* 4) used Trefill E506-S (Toray Dow Corning Silicone Co., Ltd.).

Examples 1-13, Comparative Examples 1-4
With the formulation shown in the following Tables 1 to 3, a lotion-like two-layer composition is prepared by the following method, and the evaluation in a stationary state and the evaluation of caking (redispersibility of powder) are as follows. Evaluated by criteria.

[Production method]
Based on the formulations shown in Tables 1 to 3, the powder layer was dispersed in ethanol, mixed with water, filled into a container, and a lotion-like composition was obtained.

[Evaluation methods]
The following method evaluated whether the Example mentioned later exhibits the effect of this invention.

(1) Evaluation in a stationary state The arrangement | positioning (upper layer, lower layer) of the powder dispersion layer was evaluated by the state after leaving the composition with which the container was filled at 40 degreeC for 3 hours by a special panel.
<Evaluation criteria>
A: All powders are arranged in the upper layer.
○: 95% or more of the powder is disposed in the upper layer.
(Triangle | delta): A part of powder settles down and a powder layer is arrange | positioned at an upper layer and a lower layer.
X: Powder settles in the lower layer.

(2) Evaluation of caking (solidification) After the composition filled in the container was stored in a state of standing at 25 ° C. for 3 months, the state in which the powder was redispersed by shaking the container with a specialized panel was evaluated. did.
<Evaluation criteria>
A: The powder layer was quickly and uniformly dispersed.
○: The powder layer was uniformly dispersed.
(Triangle | delta): A part of powder layer caked (solidified), and when it repeated violent shaking, it disperse | distributed uniformly.
X: The powder layer was caked (solidified) and was not uniformly dispersed even when vigorously shaken.

  In Examples 1 and 2, the powder layer was stably disposed on the upper layer, and quickly and uniformly dispersed without caking. In Comparative Example 1 in which only polymethylsilsesquioxane-coated crosslinked silicone elastomer powder (silicone resin-coated silicone rubber powder) was blended as a powder, the powder settled down. In Comparative Example 2 in which only the hollow resin powder was blended as the powder, caking occurred over time.

  In Example 3, a part of the powder layer was settled and separated vertically. In Examples 4 to 6, the powder was arranged in the upper layer without caking. In Example 7, caking was partially caused, but it was uniformly dispersed when vigorously shaken.

  Part of Example 8 was slightly caked. Examples 9 to 12 were arranged in the upper layer without caking. In Example 13, a part of the sample settled and separated into upper and lower parts.

Example 14: Antiperspirant (Body Lotion)
Ethanol 35.0% by mass
Triclosan 0.2
Zinc sulfocoborate 0.3
Fragrance 0.2
Menthol 0.2
Hollow resin powder 1.5
(Matsumoto Microsphere MFL-50STI manufactured by Matsumoto Yushi Co., Ltd.)
Silicone resin coated silicone rubber powder 2.5
(KSP100 manufactured by Shin-Etsu Chemical Co., Ltd.)
Water residue The antiperspirant was a two-layer cosmetic, and the powder layer was placed in the upper layer.

Example 15: Cosmetic (carmine lotion)
Ethanol 20.0% by mass
Zinc oxide 2.0
Trimethylglycine 3.0
Phenoxyethanol 0.1
Silicone-treated hollow resin powder 1.5
(Silicone surface treatment Gantz Pearl GMH-0850 manufactured by Miyoshi Kasei Co., Ltd.)
Silicone resin coated silicone rubber powder 2.5
(KSP105 manufactured by Shin-Etsu Chemical Co., Ltd.)
Water residue The cosmetic (carmine lotion) is a three-layer cosmetic, and the powder layers were arranged in the uppermost layer and the lowermost layer.

Example 16: Cologne perfume 2.0 mass%
Ethanol 40.0
1,3-butylene glycol 1.0
Sodium hexametaphosphate 0.01
Citric acid 0.01
Sodium citrate 0.05
POE (60) hydrogenated castor oil 0.1
Hollow resin powder 1.5
(Matsumoto Microsphere MFL-50SCA manufactured by Matsumoto Yushi Co., Ltd.)
Silicone resin coated silicone rubber powder 2.5
(KSP101 manufactured by Shin-Etsu Chemical Co., Ltd.)
Water residue The above-mentioned eau de cologne is a two-layer cosmetic, and the powder layer was placed in the upper layer.

Example 17: Sarasara Cleansing Lotion Ethanol 35.0% by mass
Alkyl glucoside 1.0
PEG400 5.0
POE (20) sorbitan monolaurate 1.0
Hollow resin powder 0.5
(Microsphere 461 DE 20 d70 made by Expandance)
Silicone resin coated silicone rubber powder 0.6
(KSP100 manufactured by Shin-Etsu Chemical Co., Ltd.)
Water residue The cleansing lotion was a two-layer cosmetic, and the powder layer was placed in the upper layer.

Example 18: Deodorant spray exclusively for shoes Perfume 1.00% by mass
Ethanol 35.00
Brown tea extract 3.00
Malic acid 0.03
Sodium malate 0.02
POE (40) hydrogenated castor oil 0.01
Blue No. 1 0.001
Hollow resin powder 1.50
(Matsumoto Microsphere MFL-50SCA manufactured by Matsumoto Yushi Co., Ltd.)
Silicone resin-coated silicone rubber powder 2.50
(KSP100 manufactured by Shin-Etsu Chemical Co., Ltd.)
Water residue

Example 19: Fragrance spray for toilet fragrance 2.00% by mass
Ethanol 30.00
POE (40) hydrogenated castor oil 0.10
Isopropylmethylphenol 0.20
Hollow resin powder 1.50
(Gantz Pearl GMH-0850 manufactured by Gantz Kasei)
Silicone resin-coated silicone rubber powder 2.50
(KSP100 manufactured by Shin-Etsu Chemical Co., Ltd.)
Water residue

Claims (4)

A multilayer composition comprising an aqueous phase comprising two or more layers, the uppermost layer of the aqueous phase comprising a powder dispersion layer,
The powder dispersion layer contains at least (a) a hollow resin powder having a true specific gravity of 0.01 to 0.9 in a dry state and (b) a polymethylsilsesquioxane-coated crosslinked silicone elastomer powder. A multilayer composition.   Furthermore, a lower alcohol is mix | blended, The multilayer type composition of Claim 1 characterized by the above-mentioned.   2. The multilayer composition according to claim 1, wherein the total amount of the component (a) and the component (b) is 0.1 to 15.0% by mass with respect to the total amount of the multilayer composition. object. 2. The multilayer composition according to claim 1, wherein a blending amount of the component (a) and the component (b) is (a) :( b) = 1: 9 to 9: 1 in mass ratio. object.