U.S. patent application number 09/365235 was filed with the patent office on 2001-07-12 for external-use composition.
This patent application is currently assigned to SHISEIDO CO., LTD. Invention is credited to MIURA, YOSHIMASA, SUZUKI, FUKUJI, TAKAHASHI, KAZUO, TAKATA, SADAKI.
Application Number | 20010007672 09/365235 |
Document ID | / |
Family ID | 16900601 |
Filed Date | 2001-07-12 |
United States Patent
Application |
20010007672 |
Kind Code |
A1 |
MIURA, YOSHIMASA ; et
al. |
July 12, 2001 |
EXTERNAL-USE COMPOSITION
Abstract
The invention provides an external-use composition imparting no
sticky sensation in use, particularly an external-use composition
for a cosmetic composition exhibiting excellent retention during
use, by finding a gelling agent for an oily ingredient,
particularly for silicone oil. The external-use composition
contains a spherical powder (mean particle size: 0.1-200 .mu.m) of
organopolysiloxane elastomer having a JIS A hardness of 1.0-30.
Inventors: |
MIURA, YOSHIMASA; (KANAGAWA,
JP) ; TAKATA, SADAKI; (KANAGAWA, JP) ;
TAKAHASHI, KAZUO; (KANAGAWA, JP) ; SUZUKI,
FUKUJI; (KANAGAWA, JP) |
Correspondence
Address: |
TOWNSEND & BANTA
SUITE 500
1225 EYE STREET NW
WASHINGTON
DC
20005
|
Assignee: |
SHISEIDO CO., LTD
|
Family ID: |
16900601 |
Appl. No.: |
09/365235 |
Filed: |
July 30, 1999 |
Current U.S.
Class: |
424/400 |
Current CPC
Class: |
A61K 2800/412 20130101;
A61Q 19/00 20130101; A61K 8/025 20130101; A61Q 1/02 20130101; A61K
2800/43 20130101; A61Q 17/04 20130101; A61K 8/891 20130101; A61K
8/895 20130101; A61K 2800/56 20130101; A61Q 1/12 20130101 |
Class at
Publication: |
424/400 |
International
Class: |
A61K 009/00 |
Foreign Application Data
Date |
Code |
Application Number |
Jul 31, 1998 |
JP |
10-229972 |
Claims
What is claimed is:
1. An external-use composition containing a spherical powder of
organopolysiloxane elastomer having a JIS A hardness of 1.0-30,
wherein the powder has a mean particle size of 0.1-200 .mu.m.
2. An external-use composition according to claim 1, comprising the
spherical powder of organopolysiloxane elastomer and an oily
ingredient.
3. An external-use composition according to claim 1, wherein the
spherical powder of organopolysiloxane elastomer is contained in an
amount of 0.1-50.0 wt. % based on the entirety of the
composition.
4. An external-use composition according to claim 2, wherein the
spherical powder of organopolysiloxane elastomer is contained in an
amount of 0.1-50.0 wt. % and the oily ingredient is contained in an
amount of 10.0-95.0 wt. % based on the entirety of the
composition.
5. An external-use composition according to claim 2, wherein the
oily ingredient is silicon oil.
6. An external-use composition according to claim 1, which is a
cosmetic composition.
7. An external-use composition according to claim 2, which is a
cosmetic composition.
Description
BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates to a composition for external
use (hereinafter referred to as an external-use composition), and
more particularly, to an external-use composition useful as a
cosmetic composition.
[0003] 2. Background Art
[0004] Conventionally, a spherical powder of an organopolysiloxane
elastomer, having characteristic elasticity, has been developed as
a powder for cosmetic compositions and has been incorporated into a
variety of products. Such a powder exhibits favorable properties
when incorporated into cosmetic compositions, i.e., the cosmetic
composition containing such a powder exhibits good skin fittability
and spreadability on the skin; imparts a light and smooth sensation
when applied by rubbing; has a soft-touch sensation; and imparts no
strange sensation or irritation to the skin (Japanese Patent
Application Laid-Open (kokai) No. 2-243612 and Japanese Patent
Publication (kokoku) Nos. 4-17162 and 4-66446).
[0005] Meanwhile, a gelling agent for an oily ingredient is used in
order to thicken an oily ingredient in an external-use composition.
Conventionally, gelling agents such as metallic soap,
organic-compound-modified clay minerals, and oil-soluble polymers
have been known to gel hydrocarbon oils and ester oils. However,
hydrocarbon oils and ester oils per se are sticky and oily, and
such drawbacks limit use thereof in an external-use composition,
even though gelling agents therefor are available.
[0006] In contrast, silicone oils, having favorable characteristics
such as a light sensation for use and an non-sticky touch to the
skin, has been widely used in external-use compositions in recent
years. However, few gelling agents for gelling silicone oil are
known; an example of which is a certain type of polyether-modified
silicone disclosed in Japanese Patent Application Laid-Open (kokai)
No. 7-215817. In addition, a gel-type composition in which silicone
oil is gelled by use of the polyether-modified silicone exhibits
slight stickiness which is characteristic to polymers.
SUMMARY OF THE INVENTION
[0007] In view of the foregoing, an object of the present invention
is to provide an external-use composition imparting no sticky
sensation in use, particularly an external-use composition for
cosmetic compositions exhibiting excellent retention on the skin
during use (hereinafter called "cosmetic retention"), by finding a
gelling agent for an oily ingredient, particularly for silicone
oil.
[0008] In order to overcome the drawbacks, the present inventors
have conducted earnest studies on a spherical powder of
organopolysiloxane elastomer, and have found that a spherical
powder of organopolysiloxane elastomer having a JIS A hardness as
low as 1.0-30 has excellent oil-absorbability and serves as a
gelling agent for an oily ingredient, particularly silicone oil, as
compared with a conventionally used spherical powder of
organopolysiloxane elastomer having a JIS A hardness of 35-80.
[0009] The inventors have also found that an external-use
composition containing such a spherical powder of
organopolysiloxane elastomer having excellent oil-absorbability
imparts no sticky sensation in use and exhibits further improved
skin fittability and spreadability on the skin; and imparts a
further improved light and smooth sensation when applied by rubbing
(hereinafter referred to as light and smooth application
sensation), as compared with a conventionally used spherical powder
of organopolysiloxane elastomer having a JIS A hardness of 35-80,
and has excellent stability with the passage of time. Particularly,
when the composition serves as a cosmetic composition, the cosmetic
composition exhibits excellent cosmetic retention. The present
invention has been accomplished based on this finding.
[0010] Accordingly, in one aspect of the present invention, there
is provided an external-use composition containing a spherical
powder of organopolysiloxane elastomer having a JIS A hardness of
1.0-30 that has a mean particle size of 0.1-200 .mu.m.
[0011] Preferably, the external-use composition contains the
spherical powder of organopolysiloxane elastomer in an amount of
0.1-50.0 wt. % based on the entirety of the composition.
[0012] Particularly, the external-use composition is suitable for
cosmetic compositions.
[0013] As used herein, the term "mean particle size" refers to a
value which is obtained by measuring the diameters in a specific
direction of particles under an optical microscope and dividing the
sum of respective diameters of particles by the number of measured
particles.
[0014] The term "JIS A hardness" refers to a hardness measured
according to JIS K 6301 by use of the JIS A hardness meter.
[0015] The present invention provides an external-use composition
having excellent spreadability on the skin, good light and smooth
application sensation and skin fittability, and non-sticky
sensation in use. Particularly, the present invention provides a
cosmetic composition having greatly improved cosmetic
retention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0016] Modes for carrying out the present invention will next be
described.
[0017] The spherical powder of organopolysiloxane elastomer which
is incorporated into the external-use composition of the present
invention is composed of an organopolysiloxane elastomer having a
JIS A hardness of 1.0-30, preferably 1.0-10. When the JIS A
hardness is less than 1.0, the external-use composition containing
the powder disadvantageously imparts a sticky sensation in use,
whereas when the hardness is in excess of 30, gelling property of
the powder is unfavorably markedly deteriorated.
[0018] The spherical powder of organopolysiloxane elastomer that is
incorporated into the external-use composition of the present
invention has a mean particle size of 0.1-200 .mu.m, preferably
0.5-20.0. When the particle size is less than 0.1 .mu.m, a smooth
application sensation disadvantageously disappears, whereas when
the particle size is in excess of 200 .mu.m, the powder causes an
unfavorable rough sensation when applied by rubbing.
[0019] The spherical powder of organopolysiloxane elastomer which
is incorporated into the external-use composition of the present
invention may be a perfectly spherical powder or an oblate
spherical powder. However, a perfect spherical powder is more
preferable in that the composition containing the powder imparts a
more favorable smoother application sensation.
[0020] No particular limitation is imposed on the method for
producing the spherical powder (having a mean particle size of
0.1-200 .mu.m) of organopolysiloxane elastomer having a JIS A
hardness of 1.0-30, and the powder can generally be produced by use
of a curable organopolysiloxane composition as a raw material.
Examples of the curable organopolysiloxane composition include:
[0021] an addition-curable organopolysiloxane composition which is
cured through addition reaction between a diorganopolysiloxane
having a silicon-bonded hydrogen atom and an organopolysiloxane
having a silicon-bonded lower alkenyl group such as a vinyl group
conducted in the presence of a platinum catalyst;
[0022] a condensation-curable organopolysiloxane composition which
is cured through dehyrogenation reaction between a
diorganopolysiloxane having hydroxyl groups at both molecule ends
and a diorganopolysiloxane having a silicon-bonded hydrogen atom
conducted in the presence of an organotin compound;
[0023] a condensation-curable organopolysiloxane composition which
is cured through condensation reaction, such as dehydration or
removal of alcohol, oxime, amine, amide, carboxylic acid, ketone,
etc., between a diorganopolysiloxane having hydroxyl groups at both
molecule ends and hydrolyzable organosilanes conducted in the
presence of an organotin compound or titanate;
[0024] a peroxide-curable organopolysiloxane composition which is
cured by the application of heat in the presence of an organic
peroxide catalyst; and
[0025] a high-energy-ray-curable organopolysiloxane composition
which is cured through radiation of .gamma.-rays, UV-rays, or an
electron beam.
[0026] Among these curable organopolysiloxane compositions, an
addition-curable organopolysiloxane composition is preferred, in
view of a high curing rate and homogeneity in curing. A
particularly preferable composition comprises (A) a
diorganopolysiloxane having at least two silicon-bonded hydrogen
atoms in the molecule; (B) an organopolysiloxane having at least
two lower alkenyl groups in the molecule; and (C) a platinum
catalyst.
[0027] An organic group other than a lower alkenyl group may also
bond to a silicon atom in an organopolysiloxane or a
diorganopolysiloxane serving as a predominant component of the
above-mentioned curable organopolysiloxane composition, and
examples of such an organic group include an alkyl group such as
methyl, ethyl, propyl, butyl, or octyl; a substituted alkyl group
such as 2-phenylethyl, 2-phenylpropyl, 3,3,3-trifluoropropyl; an
aryl group such as phenyl, tolyl, or xylyl; and a monovalent
hydrocarbyl group having a substituent such as an epoxy,
carboxylate, or mercapto group.
[0028] Several methods may be employed for producing the spherical
powder (having a mean particle size of 0.1-200 .mu.m) of
organopolysiloxane elastomer having a JIS A hardness of 1.0-30 from
the above-mentioned curable organopolysiloxane composition.
Examples of the methods include the following (1) to (4):
[0029] (1) a method which involves mixing an addition-curable,
condensation-curable, or peroxide-curable organopolysiloxane
composition with water in the presence of a surfactant such as a
nonionic, anionic, cationic, or amphoteric surfactant; forming a
homogeneous aqueous dispersion by use of an apparatus such as a
homogenization mixer, a colloid mill, a homogenizer, or a propeller
mixer; releasing the dispersion into hot water at 50.degree. C. or
higher to thereby perform curing; and drying,
[0030] (2) a method which involves spraying an addition-curable,
condensation-curable, or peroxide-curable organopolysiloxane
composition directly into hot air-flow to thereby perform
curing,
[0031] (3) a method which involves spraying a
high-energy-ray-curable organopolysiloxane composition under
exposure to high-energy rays to thereby perform curing, and
[0032] (4) a method which involves curing an addition-curable,
condensation-curable, peroxide-curable, or high-energy-ray-curable
organopolysiloxane composition and crushing the cured product by
use of a known crushing apparatus such as a ball mill, an atomizer,
a kneader, or a roll mill.
[0033] Of these, the method (1) is preferred in that a powder
having a more spherical particle shape and a small variation in
particle size can be produced.
[0034] A spherical powder of organopolysiloxane elastomer is
described in detail in Japanese Patent Application Laid-Open
(kokai) No. 2-243612 and Japanese Patent Publication (kokoku) Nos.
4-17162 and 4-66446.
[0035] The external-use composition according to the present
invention contains the above-described spherical powder of
organopolysiloxane elastomer in an amount of preferably 0.1-50.0
wt. % based on the entirety of the composition, particularly
preferably 1.0-20.0 wt. %. When the content is less than 0.1 wt. %,
an intended effect on improvement in use-related characteristics
provided by the present invention, such as imparting no sticky
sensation in use and a light and smooth application sensation, is
poor, whereas when the content is in excess of 50.0 wt. %, the
resultant external-use composition disadvantageously exhibits
sluggish spreadability on the skin and imparts a rough
sensation.
[0036] In addition to the above-described spherical powder of
organopolysiloxane elastomer, a pigment powder may be incorporated
into the external-use composition according to the present
invention. No particular limitation is imposed on the pigment
powder so long as it is one that is typically incorporated into an
external-use composition, and any pigment powder such as an
inorganic pigment powder or an organic pigment powder may be
incorporated.
[0037] Example of the inorganic pigments include talc, kaolin,
calcium carbonate, zinc flower, titanium dioxide, red iron oxide,
yellow iron oxide, black iron oxide, ultramarine, titanium-coated
mica, bismuth oxychloride, a binderg pigment, ultramarine pink,
hydrated chromium oxide, titanated mica, chromium oxide, cobalt
aluminum oxide, iron blue, carbon black, silicic anhydride,
magnesium silicate, bentonite, mica, sericite, zirconium oxide,
magnesium oxide, zinc oxide, titanium oxide, precipitated calcium
carbonate, heavy calcium carbonate, light magnesium carbonate,
heavy magnesium carbonate, and calamine.
[0038] Examples of the organic pigments include polyester,
polymethylmethacrylate, cellulose, Nylon-12, Nylon-6,
styrene.acrylic acid copolymers, polypropylene, poly(vinyl
chloride), nylon powder, polyethylene powder, benzoguanamine
powder, tetrafluoroethylene powder, boron nitride, fish scale
flake, lake tar pigments, lake natural pigments, and
inorganic-organic hybrid pigments.
[0039] Preferably, the pigment powder is hydrophobicized. No
particular limitation is imposed on the hydrophobicized pigment
powder so long as the powder has a hydrophobic surface. Examples of
such powders include a pigment powder surface-treated with
high-viscosity silicone; a pigment powder coated with a silicone
resin which has been preliminary reacted with alkyl hydrogen
polysiloxane; silicone-coated powder further treated with alkene; a
pigment powder treated with one or more surfactants selected from a
cationic surfactant, an anionic surfactant, and a nonionic
surfactant; a wax-coated pigment powder; a pigment powder treated
with dextrinized fatty acid; and a pigment powder treated with a
fluorine compound containing a perfluoroalkyl group.
[0040] The external-use composition according to the present
invention contains powders including the above-described spherical
powder of organopolysiloxane elastomer in an amount of 0.1-60.0 wt.
% based on the entirety of the composition, particularly preferably
1.0-40.0 wt. %.
[0041] The external-use composition according to the present
invention may be used as a cosmetic composition, a drug
composition, a quasi-drug composition, etc. When the external-use
composition according to the present invention is used as a make-up
cosmetic composition such as a foundation, advantages of the
present invention are particularly notable, as the above-described
spherical powder of organopolysiloxane elastomer absorbs sebum to
thereby provide a cosmetic composition exhibiting excellent
cosmetic retention.
[0042] The form of the external-use composition according to the
present invention is not particularly limited, and the composition
may be used in the forms of liquid, milky-lotion, ointment, cream,
gel, etc., so long as the composition is applicable to the
skin.
[0043] In addition to powders including the above-described
spherical powder of organopolysiloxane elastomer, one or more
ingredients which are typically added to an external-use
composition, such as an oily ingredient or water, may be
incorporated into the external-use composition according to the
present invention without impairing the effects of the present
invention and in accordance with the form.
[0044] Examples of the oily ingredient which is incorporated into
the external-use composition according to the present invention
include:
[0045] silicone oils such as dimethylpolysiloxane,
dimethylcyclopolysiloxa- ne, methylphenyl polysiloxane, methyl
hydrogen polysiloxane, higher fatty acid-modified
organopolysiloxane, higher alcohol-modified organopolysiloxane,
trimethylsiloxysilicate, and decamethylcyclopentanesi- loxane;
[0046] hydrocarbon oils such as liquid paraffin, squalane,
vaseline, polyisobutylene, and microcrystalline wax;
[0047] ester oils such as isopropyl myristate, myristyl
octyldodecanol, and di(2-ethylhexyl) succinate;
[0048] glycerides such as neopentyl glycol diisooctanoate, glyceryl
monostearate, triglyceryl monoisostearate, and triglyceryl
cocoate;
[0049] oils and fats such as castor oil and olive oil;
[0050] lower alcohols such as ethanol;
[0051] higher alcohols such as octyldodecanol, hexadecyl alcohol,
cetyl alcohol, oleyl alcohol, stearyl alcohol, and polyethylene
glycol;
[0052] higher fatty acids such as lauric acid, palmitic acid, oleic
acid, stearic acid, and isostearic acid;
[0053] waxes such as lanolin and beeswax; and
[0054] fluorocarbon oils.
[0055] Such oily ingredients are preferably incorporated in an
amount of 10.0-95.0 wt. % based on the entirety of the
composition.
[0056] When the external-use composition according to the present
invention is emulsified, the water content of the composition is
typically 1.0-80.0 wt. % based on the entirety of the
composition.
[0057] Other additives may also be incorporated into the
external-use composition according to the present invention, so
long as the effects of the present invention are not impaired.
[0058] Examples of such additives include
[0059] humectants such as polyhydric alcohol (e.g., glycerin),
mucopolysaccharides (e.g., sodium hyaluronate), and organic acids
and salts thereof (e.g., amino acids, amino acid salts, and hydroxy
acid salts);
[0060] surfactants such as cationic surfactants, anionic
surfactants, and nonionic surfactants;
[0061] pharmaceuticals such as vitamin E and vitamin E acetate;
[0062] astringents; antioxidants; preservatives; perfume; pH
regulators such as sodium secondary phosphate; clay minerals;
thickeners; and ultraviolet absorbents.
[0063] Of these, a humectant is preferably incorporated into the
composition in order to prevent evaporation of water from the
external-use composition per se.
[0064] Specific formulations of the external-use composition of the
present invention are described below.
EXAMPLES
[0065] The present invention is described in more detail by way of
examples, which should not be construed as limiting the invention
thereto.
[0066] Throughout the examples, unless otherwise stated, the amount
of an incorporated ingredient represents weight % with respect to
the entirety of the composition containing the ingredient.
[0067] JIS A hardness of an organopolysiloxane elastomer and the
mean particle size of a spherical powder of organopolysiloxane
elastomer were measured by the following methods. In addition, a
sensory test of the cosmetic composition containing the powder was
performed as described below.
[0068] <JIS A Hardness of Organopolysiloxane Elastomer>
[0069] An organopolysiloxane composition serving as a raw material
was heated in a convection oven at 150.degree. C. for one hour, to
thereby prepare an organopolysiloxane elastomer. After the
elastomer was cooled to room temperature, JIS A hardness of the
elastomer was measured by use of a JIS A hardness meter specified
by JIS K 6301.
[0070] <Mean Particle Size of Spherical Powder of
Organopolysiloxane Elastomer>
[0071] Particles were observed under an optical microscope in order
to measure the sizes thereof, and a mean value was calculated.
<Sensory Test>
[0072] A sensory test of the cosmetic composition was performed by
a panel of 10 cosmetic experts in terms of the following five
items: (1) spreadability, (2) light application sensation, (3) skin
fittablility, (4) non-stickiness, and (5) cosmetic retention.
Regarding each item, in the case where 8 or more panelists
evaluated the item as "good," a rating AA was given; in the case
where 6-7 panelists evaluated the item as "good," a rating BB was
given; in the case where 4-5 panelists evaluated the item as
"good," a rating CC was given; and in the case where 3 or fewer
panelists evaluated the item as "good," a rating DD was given.
[0073] Cosmetic retention of the cosmetic composition was evaluated
by observation of the degree of make-up deterioration after a
practical test during which subjects walked for two hours. "Good
cosmetic retention" refers to the case where little or no
deterioration of the makeup was visually observed by the panelist
and the makeup remained mostly intact on the skin.
Examples 1 to 4 and Comparative Examples 1 to 4
[0074] A gel foundation containing the following ingredients was
prepared in accordance with a method as described below. The
foundation was subjected to a sensory test, and the results are
shown in Table 1 along with the type of powder (6) employed. In
Comparative Example 1, silicone-treated talc was incorporated in an
amount of 8.0 wt. % in place of powder (6).
[0075] A method for producing the spherical powders of
organopolysiloxane elastomer (A to F) shown in Table 1 is described
later. Polymethylsilsesquioxane powder G is commercially available
Tospearl (product of Toshiba Silicone Co., Ltd.). Each powder was
subjected to measurement of JIS A hardness, mean particle size, oil
absorption with respect to decamethylcyclopentasiloxane, and
viscosity when dispersed in decamethylcyclopentasiloxane. Results
are shown in Table 2.
1 Ingredient Amount (wt. %) (1) silicone-treated talc 10.0 (2)
silicone-treated sericite 3.0 (3) silicone-treated mica 3.0 (4)
silicone-treated titanium dioxide 6.0 (5) silicone-treated color
pigment 3.0 (6) powder 8.0 (7) decamethylcyclopentasiloxane 50.0
(8) polyether-modified silicone 4.0 (9) diglyceryl diisostearate
1.0 (10) ethyl alcohol 6.0 (11) purified water 6.0
<Method of Production>
[0076] Ingredient (6) was dispersed in ingredient (7), and powders
of ingredients (1) to (5) were further dispersed in the resultant
dispersion. Subsequently, ingredients (8) and (9) were dissolved
into the resultant dispersion, to thereby obtain an oil phase. An
aqueous phase, a mixture of ingredients (10) and (11), was added to
the oil phase with stirring. The resultant mixture was deaerated
and charged into a container, to thereby obtain a gel
foundation.
2 TABLE 1 Example Comparative Example 1 2 3 4 1 2 3 4 Powder used
as A B C D None E F G ingredient (6) Sensory test (1) Spreadability
AA AA AA BB DD CC CC DD (2) Light AA BB BB BB DD CC CC DD
application sensation (3) Skin AA BB BB BB DD CC CC DD fittability
(4) Non- AA AA AA BB CC CC CC DD stickiness (5) Cosmetic AA AA AA
BB DD CC CC DD retention State of gel Gel Gel gel liquid gel gel
gel composition Hardness of 24 18 12 8 not 6 5 1 composition
measur- (30.degree. C.)*.sup.1 able *.sup.1:Hardness was measured
by use of a curd tension meter with a load of 200 g and a
pressure-sensitive shaft of 8.phi..
[0077] As is apparent from Table 1, foundations containing a
spherical powder of organopolysiloxane elastomer having a JIS A
hardness of more than 30 exhibit rating "CC" with respect to all
evaluation items (1) to (5) in the above-described sensory test. As
is also apparent from Table 1, foundations containing a spherical
powder of organopolysiloxane elastomer having a JIS A hardness of
1.0-30 exhibit rating "AA" or "BB" with respect to all evaluation
items (1) to (5) in the above-described sensory test. Thus, these
foundations were confirmed to have excellent properties in terms of
skin fittatibility, light application sensation, spreadability,
non-stickiness, and cosmetic retention.
[0078] Method for Producing Spherical Powder of Organopolysiloxane
Elastomer (Powder A)
[0079] Polydimethylsiloxane having dimethylvinylsiloxy groups at
both ends of the molecular chain (vinyl equivalent=5000) (100 parts
by weight), dimethylsiloxane.methylhydrogensiloxane copolymer
having trimethylsiloxy groups at both ends of the molecular chain
(4.5 parts by weight), dimethylpolysiloxane having trimethylsiloxy
groups at both ends of the molecular chain (viscosity: 100 cSt) (50
parts by weight), and an isopropanol solution containing platinic
chloride (an amount as reduced to 50 ppm of platinum with respect
to the entirety of the resultant composition) were homogeneously
blended at 5.degree. C., to thereby prepare a liquid
organopolysiloxane composition.
[0080] This liquid organopolysiloxane composition was quickly mixed
into an aqueous solution (300 parts by weight) containing pure
water (electric conductivity: 0.2 .mu.S/cm) and 2 wt. % of
polyoxyethylene (9 mol-added) lauryl ether at 25.degree. C.
Subsequently, the resultant mixture was treated by use of a
homogenizer (300 kgf/cm.sup.2), to thereby prepare an aqueous
dispersion in which a liquid organopolysiloxane composition was
homogeneously dispersed.
[0081] The resultant aqueous dispersion was allowed to stand at
30.degree. C. for 6 hours, and then heated at 80.degree. C. for 1
hour, to thereby cure the composition. Subsequently, the aqueous
dispersion was dried by use of a spray dryer, to thereby obtain a
spherical powder of organopolysiloxane elastomer (powder A).
[0082] Method for Producing Spherical Powder of Organopolysiloxane
Elastomer (Powder B)
[0083] Polydimethylsiloxane having dimethylvinylsiloxy groups at
both ends of the molecular chain (vinyl equivalent=5000) (100 parts
by weight), dimethylsiloxane.methylhydrogensiloxane copolymer
having trimethylsiloxy groups at both ends of the molecular chain
(4.5 parts by weight), dimethylpolysiloxane having trimethylsiloxy
groups at both ends of the molecular chain (viscosity: 100 cSt) (50
parts by weight), and an isopropanol solution containing platinic
chloride (an amount as reduced to 50 ppm of platinum with respect
to the entirety of the resultant composition) were homogeneously
blended at 5.degree. C., to thereby prepare a liquid
organopolysiloxane composition.
[0084] This liquid organopolysiloxane composition was quickly mixed
into an aqueous solution (300 parts by weight) containing pure
water (electric conductivity: 0.2 .mu.S/cm) and 2 wt. % of
polyoxyethylene (9 mol-added) lauryl ether at 25.degree. C.
Subsequently, the resultant mixture was treated by use of a
homogenizer (200 kgf/cm.sup.2), to thereby prepare an aqueous
dispersion in which a liquid organopolysiloxane composition was
homogeneously dispered.
[0085] The resultant aqueous dispersion was allowed to stand at
30.degree. C. for 6 hours, and then was heated at 80.degree. C. for
1 hour, to thereby cure the composition. Subsequently, the aqueous
dispersion was dried by use of a spray dryer, to thereby obtain a
spherical powder of organopolysiloxane elastomer (powder B).
[0086] Method for Producing Spherical Powder of Organopolysiloxane
Elastomer (Powder C)
[0087] Polydimethylsiloxane having dimethylvinylsiloxy groups at
both ends of the molecular chain (vinyl equivalent=2500) (100 parts
by weight), polymethylhydrogensiloxane having trimethylsiloxy
groups at both ends of the molecular chain (viscosity: 20 mPa.s)
(5.2 parts by weight), and an isopropanol solution containing
platinic chloride (an amount as reduced to 50 ppm of platinum with
respect to the entirety of the resultant composition) were
homogeneously blended at 5.degree. C., to thereby prepare a liquid
organopolysiloxane composition.
[0088] This liquid organopolysiloxane composition was heated in a
convection oven at 150.degree. C. for one hour, to thereby cure the
composition and obtain an organopolysiloxane elastomer.
Subsequently, the organopolysiloxane elastomer was pulverized by
use of a pulverizer for 3 hours, and passed through a 100-mesh
sieve, to thereby to obtain a spherical powder of
organopolysiloxane elastomer (powder C).
Method for Producing Spherical Powder of Organopolysiloxane
Elastomer (Powder D)
[0089] Polydimethylsiloxane having dimethylvinylsiloxy groups at
both ends of the molecular chain (vinyl equivalent=5000) (100 parts
by weight), dimethylsiloxane.methylhydrogensiloxane copolymer
having trimethylsiloxy groups at both ends of the molecular chain
(4.5 parts by weight), and an isopropanol solution containing
platinic chloride (an amount as reduced to 50 ppm of platinum with
respect to the entirety of the resultant composition) were
homogeneously blended at 5.degree. C., to thereby prepare a liquid
organopolysiloxane composition.
[0090] This liquid organopolysiloxane composition was quickly mixed
into an aqueous solution (300 parts by weight) containing pure
water (electric conductivity: 0.2 .mu.S/cm) and 2 wt. % of
polyoxyethylene (9 mol-added) lauryl ether at 25.degree. C.
Subsequently, the resultant mixture was treated by use of a
homogenizer (300 kgf/cm.sup.2), to thereby prepare an aqueous
dispersion in which a liquid organopolysiloxane composition was
homogeneously dispersed.
[0091] The resultant aqueous dispersion was allowed to stand at
30.degree. C. for 6 hours, and then heated at 80.degree. C. for 1
hour, to thereby cure the composition. Subsequently, the aqueous
dispersion was dried by use of a spray dryer, to thereby obtain a
spherical powder of organopolysiloxane elastomer (powder D).
[0092] Method for Producing Spherical Powder of Organopolysiloxane
Elastomer (Powder E)
[0093] Polydimethylsiloxane having dimethylvinylsiloxy groups at
both ends of the molecular chain (vinyl equivalent=2500) (100 parts
by weight), polymethylhydrogensiloxane having trimethylsiloxy
groups at both ends of the molecular chain (viscosity: 20 mPa.s)
(5.2 parts by weight), and an isopropanol solution containing
platinic chloride (an amount as reduced to 50 ppm of platinum with
respect to the entirety of the resultant composition) were
homogeneously blended at 5.degree. C., to thereby prepare a liquid
organopolysiloxane composition.
[0094] This liquid organopolysiloxane composition was quickly mixed
into an aqueous solution (300 parts by weight) containing pure
water (electric conductivity: 0.2 .mu.S/cm) and 2 wt. % of
polyoxyethylene (9 mol-added) lauryl ether at 25.degree. C.
Subsequently, the resultant mixture was treated by use of a
homogenizer (300 kgf/cm.sup.2), to thereby prepare an aqueous
dispersion in which a liquid organopolysiloxane composition was
homogeneously dispered.
[0095] The resultant aqueous dispersion was allowed to stand at
30.degree. C. for 6 hours, and then heated at 80.degree. C. for 1
hour, to thereby cure the composition. Subsequently, the aqueous
dispersion was dried by use of a spray dryer, to thereby obtain a
spherical powder of organopolysiloxane elastomer (powder E).
[0096] Method for Producing Spherical Powder of Organopolysiloxane
Elastomer (Powder F)
[0097] Polydimethylsiloxane having dimethylvinylsiloxy groups at
both ends of the molecular chain (vinyl equivalent=2500) (100 parts
by weight), polymethylhydrogensiloxane having trimethylsiloxy
groups at both ends of the molecular chain (viscosity: 20 mPa.s)
(5.2 parts by weight), and an isopropanol solution containing
platinic chloride (an amount as reduced to 50 ppm of platinum with
respect to the entirety of the resultant composition) were
homogeneously blended at 5.degree. C., to thereby prepare a liquid
organopolysiloxane composition.
[0098] This liquid organopolysiloxane composition was quickly mixed
into an aqueous solution (300 parts by weight) containing pure
water (electric conductivity: 0.2 .mu.S/cm) and 2 wt. % of
polyoxyethylene (9 mol-added) lauryl ether at 25.degree. C.
Subsequently, the resultant mixture was treated by use of a
homogenizer (200 kgf/cm.sup.2), to thereby prepare an aqueous
dispersion in which a liquid organopolysiloxane composition was
homogeneously dispered.
[0099] The resultant aqueous dispersion was allowed to stand at
30.degree. C. for 6 hours, and then heated at 80.degree. C. for 1
hour, to thereby cure the composition. Subsequently, the aqueous
dispersion was dried by use of a spray dryer, to thereby obtain a
spherical powder of organopolysiloxane elastomer (powder F).
3TABLE 2 Powder A B C D E F G Mean particle size 1 10 50 4 1 10 3
(.mu.m) JIS A hardness 7 7 7 30 50 50 .gtoreq.90 Oil absorption
with 450 408 382 365 200 150 48 respect to decametylcyclopenta-
siloxane (g/100 g) Viscosity at 30.degree. C. 200 163 120 45 20 15
5 (mPa .multidot. s)*.sup.2 *.sup.2:Viscosity was measured by
dispersing a powder (10 wt. %) in decamethylcyclopentasiloxane (90
wt. %) by use of a dispersion mixer and measuring the viscosity of
the resultant dispersion by use of a B-type viscometer.
[0100] As is apparent from Table 2, oil absorption of a spherical
powder of organopolysiloxane elastomer increases with a reduction
of JIS A hardness and with a reduction of the mean particle
size.
[0101] As is apparent from Tables 1 and 2, a foundation has high
hardness when it contains a spherical powder of organopolysiloxane
elastomer having high oil absorption, and also, a spherical powder
of organopolysiloxane elastomer having higher oil absorption has
more excellent property of gelling an oily ingredient.
[0102] Further examples of the external-use composition of the
present invention--Examples 5 to 14 and Comparative Examples 5 to
15--are described below. Each external-use composition was
subjected to the above-described sensory test (items (1)-(5)). The
results are shown in Table 3, along with the results of the sensory
test in Example 1.
Example 5
Emollient Cream
[0103]
4 Ingredient Amount (wt. %) (1) ion-exchange water balance (2)
glycerin 10.0 (3) methylparaben 0.2 (4) squalane 20.0 (5) cetyl
octanoate 8.5 (6) microcrystalline wax 1.0 (7) polyoxyethylene
glyceryl triisostearate 0.2 (8) perfume suitable amount (9) organic
compound-modified clay mineral 1.3 (10) spherical powder of 10.0
organopolysiloxane elastomer (powder A)
<Method of Production>
[0104] Ingredients (3) to (9) were mixed and dissolved while being
heated to 70.degree. C., to thereby prepare an oil phase, and
ingredient (10) was homogeneously dispersed in the oil phase.
Ingredient (2) was added to ingredient (1), and the resultant
mixture was heated to 70.degree. C. to thereby prepare an aqueous
phase. The aqueous phase was added to the oil phase containing
ingredient (10) in a dispersed state, with sufficient stirring. The
resultant mixture was homogenized by use of a homogenization mixer
and cooled to 30.degree. C. to thereby obtain an emollient
cream.
Example 6
[0105]
5 Milky lotion Ingredient Amount (wt. %) (1) ion-exchange water
balance (2) 1,3-butylene glycol 5.0 (3) liquid paraffin 20.0 (4)
squalane 10.0 (5) beeswax 2.0 (6) sorbitan sesquioleate 4.0 (7) POE
(20) sorbitan monooleate 1.0 (8) perfume suitable amount (9)
spherical powder of 0.1 organopolysiloxane elastomer (powder A)
<Method of Production>
[0106] Ingredients (1) and (2) were mixed and heated to 70.degree.
C. to thereby prepare an aqueous phase. Subsequently, ingredients
(3) to (8) were mixed while being heated to 70.degree. C.
Ingredient (9) was dispersed in the mixture, and the aqueous phase
was slowly added to the resultant mixture, to carry out preliminary
emulsification. The resultant mixture was homogenized by use of a
homogenization mixer, followed by deaeration, filtration, and
cooling, to thereby obtain a milky lotion.
Example 7
[0107]
6 Water-in-oil emulsion-type foundation Ingredient Amount (wt. %)
(1) ion-exchange water balance (2) 1,3-butylene glycol 3.0 (3)
dimethylpolysiloxane 15.0 (viscosity at 25.degree. C.: 6 mPa
.multidot. s) (4) methylparaben 0.1 (5) polyoxyalkylene-modified
5.0 organopolysiloxane
[0108] (6) decamethylcyclopentasiloxane 20.0
[0109] (7) perfume suitable amount
[0110] (8) hydrophobicized (silicone-treated) powder 20.0
[0111] (9) spherical powder of organopolysiloxane elastomer (powder
B) 3.0
<Method of Production>
[0112] Ingredients (3) to (7) were mixed and dissolved at
40.degree. C. to thereby prepare an oil phase. Ingredients (8) and
(9) were homogeneously dispersed in the oil phase, and ingredients
(1) and (2) were added to the resultant mixture with sufficient
stirring. The resultant mixture was homogenized by use of a
homogenization mixer, to thereby obtain a water-in-oil
emulsion-type foundation.
Example 8
[0113]
7 Water-in-oil emulsion-type solid foundation Ingredient Amount
(wt. %) (1) ion-exchange water balance (2) glycerin 5.0 (3)
methylparaben 0.1 (4) polyoxyalkylene-modified 5.0
organopolysiloxane (5) decamethylcyclopentasiloxane 20.0 (6)
dimethylpolysiloxane (viscosity at 25.degree. C.: 6 mPas) 5.0 (7)
paraffin wax 10.0 (8) hydrophobicized (silicone-treated) powder
30.0 (9) spherical powder of 7.0 organopolysiloxane elastomer
(powder D)
<Method of Production>
[0114] Ingredients (3) to (7) were mixed and dissolved while being
heated to 80.degree. C. to prepare an oil phase, and ingredients
(8) and (9) were homogeneously dispersed in the oil phase.
Ingredients (1) and (2) were mixed and heated to 80.degree. C. to
prepare an aqueous phase. Subsequently, the aqueous phase was added
to the oil phase with sufficient stirring. The resultant mixture
was homogenized by use of a homogenization mixer, poured into an
inner dish, and cooled to 30.degree. C., to thereby obtain a
water-in-oil emulsion-type solid foundation.
Example 9
[0115]
8 Gel-type makeup base Ingredient Amount (wt. %) (1) ion-exchange
water balance (2) 1,3-butylene glycol 3.0 (3) methylparaben 0.15
(4) polyoxyalkylene-modified 3.0 organopolysiloxane (5)
decamethylcyclopentasiloxane 25.0 (6) octyl methoxycinnamate 5.0
(7) dimethylpolysiloxane 10.0 (8) spherical powder of 30.0
organopolysiloxane elastomer (powder A)
<Method of Production>
[0116] Ingredients (3) to (7) were mixed and dissolved at
40.degree. C. to obtain a solution, and ingredient (8) was
homogeneously dispersed in the solution, to thereby prepare an oil
phase. Ingredients (1) and (2) were added to the oil phase with
sufficient stirring. The resultant mixture was homogenized by use
of a homogenization mixer, deaerated, and filtered to thereby
obtain a makeup base.
Example 10
[0117]
9 Water-in-oil emulsion-type foundation Ingredient Amount (wt. %)
(1) ion-exchange water balance (2) 95% ethyl alcohol 15.0 (3)
1,3-butylene glycol 3.0 (4) methylparaben 0.1 (5)
polyoxyalkylene-modified 5.0 organopolysiloxane (6)
decamethylcyclopentasiloxane 20.0 (7) perfume suitable amount (8)
hydrophobicized (fluorine-treated) powder 20.0 (9) spherical powder
of 10.0 organopolysiloxane elastomer (powder D)
<Method of Production>
[0118] Ingredients (4) to (7) were mixed and dissolved at
40.degree. C. to prepare an oil phase. Ingredients (8) and (9) were
homogeneously dispersed in the oil phase, and ingredients (1) to
(3) were further added to the oil phase with sufficient stirring.
The resultant mixture was homogenized by use of a homogenization
mixer, to thereby obtain a water-in-oil emulsion-type
foundation.
Example 11
[0119]
10 Gel-type sunscreen Ingredient Amount (wt. %) (1)
dimethylpolysiloxane (6 cs) 19.8 (2) octamethylcyclotetrasiloxane
30.0 (3) spherical powder of 12.0 organopolysiloxane elastomer
(powder B) (4) polyether-modified silicone 20.0 (5) octyl
methoxycinnamate 8.0 (6) purified water 8.0 (7) ethyl alcohol 2.0
(8) methylparaben 0.2
<Method of Production>
[0120] Ingredients (1), (2), (4), and (5) were mixed with stirring,
and powder of (3) was dispersed in the resultant mixture, to
thereby prepare an oil phase. Ingredients (7) and (8) were
dissolved in ingredient (6), to prepare an aqueous phase. The
aqueous phase was added to the oil phase with stirring. After
deaeration, the resultant mixture was charged into a container, to
thereby obtain a gel-type sunscreen.
Example 12
[0121]
11 Pressed powder Ingredient Amount (wt. %) (1) talc balance (2)
sericite 10.0 (3) kaolin 5.0 (4) titanium dioxide 5.0 (5) zinc
myristate 5.0 (6) color pigment 3.0 (7) spherical powder of 10.0
organopolysiloxane elastomer (powder A) (8) porous spherical silica
5.0 (mean particle size: 3 .mu.m) (9) squalane 3.0 (10) glyceryl
triisooctanoate 2.0 (11) preservative suitable amount (12) perfume
suitable amount
<Method of Production>
[0122] Ingredients (1) and (6) were sufficiently mixed by use of a
blender. Ingredients (2) to (5), (7), and (8) were added to the
mixture, and the resultant mixture was further mixed sufficiently.
Ingredients (9) to (11) were added to the resultant mixture. After
the color of the mixture was adjusted, ingredient (12) was sprayed
thereto and the resultant mixture was homogenized. Subsequently,
the mixture was crushed by use of a crusher, passed through a
sieve, and compression-molded into an inner dish, to thereby obtain
a pressed powder.
Example 13
[0123]
12 Powdery foundation Ingredient Amount (wt. %) (1) talc balance
(2) sericite 15.0 (3) mica 20.0 (4) titanium dioxide 10.0 (5) color
pigment 5.0 (6) spherical powder of 10.0 organopolysiloxane
elastomer (powder A) (7) porous spherical resin powder 10.0
("Microsponge," product of Dow Corning Toray Co., Ltd.; mean
particle size: 7 .mu.m) (8) squalane 6.0 (9) dimethylpolysiloxane
3.0 (10) octyl myristate 3.0 (11) sorbitan monooleate 1.0 (12)
preservative, antioxidant suitable amount (13) perfume suitable
amount
<Method of Production>
[0124] The ingredients were mixed in the same manner as described
in Example 9, to thereby obtain a powdery foundation.
Example 14
[0125]
13 Two-way foundation Ingredient Amount (wt. %) (1)
silicone-treated talc balance (2) silicone-treated sericite 15.0
(3) silicone-treated mica 30.0 (4) silicone-treated titanium
dioxide 10.0 (5) silicone-treated color pigment 5.0 (6) spherical
powder of 5.0 organopolysiloxane elastomer (powder B) (7) squalane
3.0 (8) solid paraffin 1.0 (9) dimethylpolysiloxane 4.0 (10) octyl
methoxycinnamate 1.0 (11) preservative, antioxidant suitable amount
(12) perfume suitable amount
<Method of Production>
[0126] The ingredients were mixed in the same manner as described
in Example 9, to thereby obtain a two-way (i.e., usable with or
without water) foundation.
Comparative Example 5
[0127] The procedure of Example 1 was repeated except that the
spherical powder of organopolysiloxane elastomer was replaced by
the same amount of ion-exchange water, to thereby obtain a gel-type
foundation.
Comparative Example 6
[0128] The procedure of Example 5 was repeated except that the
spherical powder of organopolysiloxane elastomer was replaced by
the same amount of ion-exchange water, to thereby obtain an
emollient cream.
Comparative Example 7
[0129] The procedure of Example 6 was repeated except that the
spherical powder of organopolysiloxane elastomer was replaced by
the same amount of ion-exchange water, to thereby obtain a milky
lotion.
Comparative Example 8
[0130] The procedure of Example 7 was repeated except that the
spherical powder of organopolysiloxane elastomer was replaced by
the same amount of ion-exchange water, to thereby obtain a
water-in-oil emulsion-type foundation.
Comparative Example 9
[0131] The procedure of Example 8 was repeated except that the
spherical powder of organopolysiloxane elastomer was replaced by
the same amount of ion-exchange water, to thereby obtain a
water-in-oil emulsion-type solid foundation.
Comparative Example 10
[0132] The procedure of Example 9 was repeated except that the
spherical powder of organopolysiloxane elastomer was replaced by
the same amount of ion-exchange water, to thereby obtain a gel-type
makeup base.
Comparative Example 11
[0133] The procedure of Example 10 was repeated except that the
spherical powder of organopolysiloxane elastomer was replaced by
the same amount of ion-exchange water, to thereby obtain a
water-in-oil emulsion-type foundation.
Comparative Example 12
[0134] The procedure of Example 11 was repeated except that the
spherical powder of organopolysiloxane elastomer was replaced by
the same amount of ion-exchange water, to thereby obtain a gel-type
sunscreen.
Comparative Example 13
[0135] The procedure of Example 12 was repeated except that the
spherical powder of organopolysiloxane elastomer was replaced by
the same amount of ion-exchange water, to thereby obtain a pressed
powder.
Comparative Example 14
[0136] The procedure of Example 13 was repeated except that the
spherical powder of organopolysiloxane elastomer was replaced by
the same amount of ion-exchange water, to thereby obtain a powdery
foundation.
Comparative Example 15
[0137] The procedure of Example 14 was repeated except that the
spherical powder of organopolysiloxane elastomer was replaced by
the same amount of ion-exchange water, to thereby obtain a two-way
foundation.
14 TABLE 3 Light Spread- application Skin Non- Cosmetic ability
sensation fittability stickiness retention Example 1 AA AA AA AA AA
Example 5 AA BB BB BB AA Example 6 AA BB AA AA BB Example 7 AA AA
AA AA Example 8 BB BB AA AA AA Example 9 BB BB AA BB AA Example 10
AA AA AA AA AA Example 11 AA AA AA AA AA Example 12 AA AA AA AA AA
Example 13 AA AA BB AA AA Example 14 AA AA BB AA AA Comp. CC DD CC
CC DD Example 5 Comp. CC CC CC CC CC Example 6 Comp. BB CC CC CC CC
Example 7 Comp. BB BB CC BB DD Example 8 Comp. CC CC CC CC DD
Example 9 Comp. BB CC CC DD DD Example 10 Comp. BB CC CC CC CC
Example 11 Comp. CC CC DD DD CC Example 12 Comp. BB BB BB BB DD
Example 13 Comp. BB BB BB BB DD Example 14 Comp. BB BB BB BB DD
Example 15
[0138] As is clear from Table 3, the external-use compositions of
Example 1 and Examples 5-14 are superior to compositions of
Comparative Examples 5-15 in terms of skin fittability, light
application sensation, spreadability, non-stickiness, and cosmetic
retention.
* * * * *